技术领域technical field
本发明涉及造纸制浆领域，特别涉及一种水解制浆的方法及其装置。The invention relates to the field of paper pulping, in particular to a hydrolysis pulping method and a device thereof.
背景技术Background technique
纸和纸板是以纸浆为主造成的，而制浆方法可分为：化学法和机械法以及处于两者之间的化学机械法、半化学法。全世界纸浆产量中，化学浆占72.4％，机械浆占16.6％，其余约占11.0％。化学法制浆分为碱法和酸法，碱法包含石灰法和烧碱法。化学法制浆的主要目的是，尽可能多地脱除植物纤维原料中使纤维粘合在一起的胞间木素使之成为纸浆，制浆过程主要包含蒸煮、洗涤和漂白等工序。蒸煮工序是植物原料在烧碱或硫酸盐或亚硫酸盐存在下高温蒸煮，从而使植物纤维细胞壁中的木质素降解。植物纤维原料经蒸煮后得到大约50％的纸浆，另外50％左右的物质溶解在蒸煮液中而形成大量高浓度废液，对碱法制浆，这种废液叫黑液；对酸法制浆，这种废液称为红液。中国目前大部分造纸厂采用碱法制浆，其所排放的黑液是制浆过程中污染物浓度最高，色度最深的废水，其中含有大量的木质素和半纤维素等降解产物、色素、戊糖类、残碱和其它溶出物，大约每生产1吨纸浆要排放10吨黑液，不仅造成植物资源的浪费还导致严重的环境污染问题，是造纸工业最棘手的难题和研究热点。Paper and cardboard are mainly made of pulp, and the pulping methods can be divided into: chemical method and mechanical method, as well as chemical mechanical method and semi-chemical method in between. Among the world's pulp production, chemical pulp accounts for 72.4%, mechanical pulp accounts for 16.6%, and the rest accounts for about 11.0%. Chemical pulping is divided into alkali method and acid method, and the alkali method includes lime method and caustic soda method. The main purpose of chemical pulping is to remove as much intercellular lignin as possible from the plant fiber raw materials that binds the fibers together to make pulp. The pulping process mainly includes cooking, washing and bleaching processes. The cooking process is high-temperature cooking of plant raw materials in the presence of caustic soda or sulfate or sulfite, thereby degrading the lignin in the plant fiber cell wall. About 50% of the pulp is obtained after the plant fiber raw material is cooked, and about 50% of the material is dissolved in the cooking liquid to form a large amount of high-concentration waste liquid. For alkaline pulping, this waste liquid is called black liquor; for acid pulping pulp, this waste liquid is called red liquor. At present, most paper mills in China use alkaline pulping, and the black liquor discharged is the wastewater with the highest concentration of pollutants and the deepest color in the pulping process, which contains a large amount of degradation products such as lignin and hemicellulose, pigments, Pentose sugars, residual alkalis and other extractables, about 10 tons of black liquor are discharged for every ton of pulp produced, which not only causes waste of plant resources but also causes serious environmental pollution problems. It is the most difficult problem and research hotspot in the paper industry.
公开于该背景技术部分的信息仅仅旨在增加对本发明的总体背景的理解，而不应当被视为承认或以任何形式暗示该信息构成已为本领域一般技术人员所公知的现有技术。The information disclosed in this Background section is only for enhancing the understanding of the general background of the present invention and should not be taken as an acknowledgment or any form of suggestion that the information constitutes the prior art that is already known to those skilled in the art.
发明内容Contents of the invention
本发明的目的在于提供一种水解制浆的方法，以超/亚临界CO2溶解于水中作为质子酸替代烧碱或硫酸盐或亚硫酸盐进行化学法制浆，减少了重污染废水的排放。The purpose of the present invention is to provide a method of hydrolysis pulping, with super/subcriticalCO Dissolved in water as protonic acid instead of caustic soda or sulfate or sulfite for chemical pulping, reducing the discharge of heavily polluted wastewater.
本发明的另一目的在于提供一种水解制浆的装置。Another object of the present invention is to provide a hydrolysis pulping device.
为实现上述目的，本发明提供了一种水解制浆的方法，包括以下步骤：To achieve the above object, the invention provides a method for hydrolysis pulping, comprising the following steps:
(1)准备原料，将水与木片或草片按质量比2:1～200:1相互混合，然后预热；(1) Prepare raw materials, mix water and wood chips or grass chips in a mass ratio of 2:1 to 200:1, and then preheat;
(2)水解反应，将步骤(1)制得的混合物放入反应器内，往反应器内充入CO2，反应器内的温度为80～500℃，压力为0.5～50MPa；应器内的温度为80～500℃，反应压力为0.5～50.0MPa，使通入的CO2气体处于超临界状态或亚临界状态；(2) Hydrolysis reaction, put the mixture prepared in step (1) into the reactor, fill the reactor with CO2 , the temperature in the reactor is 80-500°C, and the pressure is 0.5-50MPa; The temperature is 80-500°C, and the reaction pressure is 0.5-50.0MPa, so that the CO2 gas introduced is in a supercritical or subcritical state;
(3)取出反应器中反应后的混合气体；(3) take out the mixed gas after reaction in the reactor;
(4)反应1～6h后，经减压后物料从反应器中放出反应制得的浆料和还原糖。(4) After reacting for 1-6 hours, the slurry and reducing sugar prepared by the reaction are released from the reactor after decompression.
优选地，上述技术方案中，所述步骤(3)混合气体中含有CO2、水蒸汽、糠醛和乙酸，从反应器中取出混合气体的流量为0～12000m3/h，将气体通过膨胀机，经膨胀机膨胀降压为0～1.0MPa，降温为5℃～80℃，膨胀机与透平压缩机连接，往透平压缩机内补充CO2气体，再将混合气体通入反应器内。气体流量为0时，没有气体流出。Preferably, in the above technical solution, the mixed gas in the step (3) contains CO2 , water vapor, furfural and acetic acid, the flow rate of the mixed gas taken out from the reactor is 0-12000m3 /h, and the gas is passed through the expander , the expander expands and depressurizes to 0-1.0MPa, and the temperature drops to 5°C-80°C. The expander is connected to the turbine compressor, and CO2 gas is added to the turbine compressor, and then the mixed gas is passed into the reactor. . When the gas flow rate is 0, no gas flows out.
优选地，上述技术方案中，所述步骤(3)中流出的气体经过膨胀机后，进入气液分离器进行分离，剩下的气体为CO2，将CO2再通入透平压缩机。Preferably, in the above technical solution, the gas flowing out of the step (3) enters the gas-liquid separator for separation after passing through the expander, the remaining gas is CO2 , and the CO2 is then fed into the turbo compressor.
优选地，上述技术方案中，气液分离器的温度为5～40℃，压力为0.0～1.0MPa，气液分离器液体流量为0～100m3/h，气体流量为0～10000m3/h。当液体流出量和气体流出量为0时，即没有液体或气体流出。Preferably, in the above technical solution, the temperature of the gas-liquid separator is 5-40°C, the pressure is 0.0-1.0 MPa, the liquid flow rate of the gas-liquid separator is 0-100m3 /h, and the gas flow rate is 0-10000m3 /h . When the liquid outflow and gas outflow are 0, there is no liquid or gas outflow.
优选地，上述技术方案中，所述步骤(2)往反应器内分1～10个阶段充入CO2。Preferably, in the above technical solution, in the step (2), CO2 is charged into the reactor in 1 to 10 stages.
优选地，上述技术方案中，所述的木片或草片为甘蔗渣、单竹、稻草或马尾松中的一种。Preferably, in the above technical solution, the wood chips or grass chips are one of bagasse, single bamboo, straw or masson pine.
一种用于水解制浆的装置，包括：反应器，其包括：多个加热管，设于反应器内部；以及气体分布器，其包括进气口和多个用于排气的喷头；膨胀机，其与所述反应器连接；以及透平压缩机，其与所述膨胀机连接，并通过所述膨胀机驱动所述透平压缩机工作，所述透平压缩机的出气口与所述反应器连接。A device for hydrolysis pulping, comprising: a reactor, which includes: a plurality of heating pipes, arranged inside the reactor; and a gas distributor, which includes an air inlet and a plurality of nozzles for exhaust; expansion machine, which is connected with the reactor; and a turbocompressor, which is connected with the expander, and drives the turbocompressor to work through the expander, and the gas outlet of the turbocompressor is connected with the The reactor is connected.
优选地，上述技术方案中，所述气体分布器呈“L”型，其底端为圆环管状，在该圆环管上均匀设有多个用于排气的喷头，所述喷头倾斜设置。Preferably, in the above technical solution, the gas distributor is in an "L" shape, and its bottom end is in the shape of a ring tube, and a plurality of nozzles for exhaust are uniformly arranged on the ring tube, and the nozzles are arranged obliquely .
优选地，上述技术方案中，所述加热管为多个，呈平行均布在所述反应器内部；所述气体分布器有多个，所述多个气体分布器相互连通，所述每个气体分布器设在所述加热管之间。Preferably, in the above technical solution, there are multiple heating pipes, which are distributed in parallel and evenly inside the reactor; there are multiple gas distributors, and the multiple gas distributors communicate with each other, and each of the A gas distributor is provided between the heating tubes.
优选地，上述技术方案中，所述用于水解制浆的装置，还包括：预处理器，其与所述反应器连接，用于生产所需的原料进行预处理；气液分离器，其与所述膨胀机连接；以及喷放器，其于所述反应器连接，用于喷放出浆料和还原糖。Preferably, in the above technical solution, the device for hydrolysis pulping also includes: a preprocessor, which is connected to the reactor, and is used to produce the required raw materials for pretreatment; a gas-liquid separator, which It is connected with the expander; and a blower, which is connected with the reactor, is used for blowing out slurry and reducing sugar.
上述反应的机理如下：The mechanism of the above reaction is as follows:
往反应器内充入CO2混合气体，CO2气体在反应器内不断地循环和鼓泡流动，在高温高压条件下，CO2处于超临界或亚临界状态。利用超/亚临界CO2溶解于水中形成质子酸对植物纤维中的木质素、戊糖类和半纤维等进行水解降解生成还原糖、糠醛和乙酸等，而且生成的糠醛与乙酸等挥发性产物、水蒸气被循环CO2夹带不断地从反应器流出并使膨胀机做功驱动透平压缩机4，以达到膨胀—压缩自循环。Fill the reactor with CO2 mixed gas, and the CO2 gas circulates and bubbles continuously in the reactor. Under high temperature and high pressure conditions, CO2 is in a supercritical or subcritical state. Use super/subcriticalCO2 dissolved in water to form protonic acid to hydrolyze and degrade lignin, pentose sugars and hemifibres in plant fibers to produce reducing sugars, furfural and acetic acid, etc., and the generated volatile products such as furfural and acetic acid , The water vapor is entrained by the circulating CO2 and continuously flows out of the reactor and makes the expander do work to drive the turbo compressor 4 to achieve expansion-compression self-circulation.
从反应器中采取出的气相通过膨胀机，流出的混合气体包括糠醛、乙酸、水蒸气和CO2。膨胀机与透平压缩机链接，由于反应器内的CO2处于超临界或亚临界状态，当气相被采取出进入膨胀机后，CO2从超临界状态或亚临界状态跃迁为低温低压常态，从超/亚临界状态跃迁为低温低压常态即称为跨临界状态。混合气体气体膨胀推动膨胀机做功，膨胀机与透平压缩机连接，膨胀机驱动压缩机工作。气相物料从膨胀机流经气液分离器进行冷凝和气液分离，所得液体为糠醛与乙酸的水溶液；气体主要是作为循环使用的CO2，该循环CO2与新补充的CO2经透平压缩机加压后流回反应器。由于从反应器流出的气相含有CO2、水蒸汽、糠醛和乙酸等，而加压循环的气体仅为不凝气体CO2，这是因为经膨胀机降压降温后，水、糠醛和乙酸蒸汽冷凝为液体从气液分离器分离出来，而用于循环的气体仅剩下不凝气体CO2的缘故，可见驱动膨胀机的气体流量大于透平压缩机加压循环气体的流量，亦即是说膨胀机做出的功大于透平压缩机所需的功，系统所需增加的能量是由反应器内加热盘管供给水的蒸发热能，因而本系统可实现膨胀-压缩自循环。The gas phase taken from the reactor passes through the expander, and the outflowing mixed gas includes furfural, acetic acid, water vapor and CO2 . The expander is linked with the turbo compressor. Since theCO2 in the reactor is in a supercritical or subcritical state, when the gas phase is taken out and enters the expander, theCO2 transitions from a supercritical or subcritical state to a low-temperature and low-pressure normal state. The transition from super/subcritical state to low temperature and low pressure normal state is called transcritical state. The expansion of the mixed gas pushes the expander to do work, the expander is connected with the turbo compressor, and the expander drives the compressor to work. The gas phase material flows from the expander through the gas-liquid separator for condensation and gas-liquid separation, and the obtained liquid is an aqueous solution of furfural and acetic acid; the gas is mainly used as recycled CO2 , and the recycled CO2 and newly supplemented CO2 are compressed by a turbine After being pressurized, it flows back into the reactor. Since the gas phase flowing out of the reactor contains CO2 , water vapor, furfural and acetic acid, etc., the gas in the pressurized cycle is only non-condensable gas CO2 The condensed liquid is separated from the gas-liquid separator, and the gas used for circulation is only the non-condensable gas CO2 , it can be seen that the gas flow rate driving the expander is greater than the flow rate of the pressurized cycle gas of the turbine compressor, that is, It is said that the work done by the expander is greater than the work required by the turbo compressor, and the increased energy required by the system is the evaporation heat energy of the water supplied by the heating coil in the reactor, so the system can realize expansion-compression self-circulation.
由于植物纤维水解生成的糠醛和乙酸不断地流离反应器，从而消除了产物累积而引起的反馈抑制作用，打破了植物纤维中木质素、戊糖和半纤维素水解降解的化学平衡，使反应不断地朝着水解降解的方向进行，从而提高了水解降解反应速度和平衡转化率，实现水解降解反应-分离的耦合。又由于CO2在反应器中不断地循环流动，强化了植物纤维物料的鼓泡搅拌和热质传递，而且CO2还产生“超空泡”效应，最大限度地减少了物料、水和气之间的流动阻力，大大地提高了反应器的传热传质效果。况且，CO2还可以产生“同分子”效应，抑制浆料纤维素降解生成CO2的副反应，提高了木片或草片制浆的纸浆得率。Since the furfural and acetic acid produced by the hydrolysis of plant fibers continuously flow out of the reactor, the feedback inhibition caused by product accumulation is eliminated, and the chemical balance of the hydrolysis degradation of lignin, pentose and hemicellulose in plant fibers is broken, so that the reaction continues. Towards the direction of hydrolytic degradation, thereby increasing the hydrolytic degradation reaction speed and equilibrium conversion rate, and realizing the coupling of hydrolytic degradation reaction-separation. And because CO2 continuously circulates in the reactor, the bubbling stirring and heat mass transfer of plant fiber materials are strengthened, and CO2 also produces a "supercavitation" effect, which minimizes the gap between materials, water and air. The flow resistance greatly improves the heat and mass transfer effect of the reactor. Moreover, CO2 can also produce a "same molecule" effect, inhibit the side reaction of pulp cellulose degradation to generate CO2 , and increase the pulp yield of wood chips or grass chips pulping.
与现有技术相比，本发明具有如下有益效果：Compared with the prior art, the present invention has the following beneficial effects:
(1)以超/亚临界CO2溶解于水中作为质子酸替代烧碱或硫酸盐或亚硫酸盐进行化学法制浆，减少了重污染废水的排放，特别是中国大部分造纸厂是采用碱法制浆，每生产1吨纸浆要排放10吨黑液，而本发明的制浆方法无黑液也无废气排放，是一种绿色环保的制浆方法。(1) Dissolve super/subcriticalCO2 in water as protonic acid instead of caustic soda or sulfate or sulfite for chemical pulping, which reduces the discharge of heavily polluted wastewater, especially most paper mills in China use the alkali method Pulping requires the discharge of 10 tons of black liquor for every ton of pulp produced, but the pulping method of the present invention has no black liquor and no waste gas discharge, and is a green and environmentally friendly pulping method.
(2)本发明水解制浆的方法，采用跨临界CO2水解降解反应-分离耦合进行制浆，不仅生产纸浆还同时副产了糠醛、乙酸和还原糖，充分利用了木片或草片原料中含有的木质素、戊糖类和半纤维等资源制造出大宗有价值的化工产品，吃干榨尽可再生资源的有效成分，实现了“原子经济”的零排放目标，大大地提高了生物质资源的利用率。(2) The method for hydrolysis pulping of the present invention adopts transcritical COHydrolysis degradation reaction-separation coupling is carried out pulping, not only produces paper pulp but also produces furfural, acetic acid and reducing sugar by-product simultaneously, fully utilizes in the raw material of wood chip or grass chip The resources contained in lignin, pentose and hemi-fiber produce a large number of valuable chemical products, eat dry and extract the effective components of renewable resources, realize the zero emission goal of "atomic economy", and greatly increase the biomass resource utilization.
(3)本发明水解制浆的装置，采用跨临界CO2膨胀-压缩自循环的方式，使从跨临界反应器流出的高压CO2和水蒸汽经膨胀机膨胀直接推动透平压缩机加压不凝气体CO2循环回系统，减少了热功转换过程：热能→机械能→电能→机械能的有效能损失，提高了热能转换的热功效率，实现了节能减排和零排放的目标。(3) The hydrolysis pulping device of the present invention adopts the transcriticalCO2 expansion-compression self-circulation mode, so that the high-pressureCO2 and water vapor flowing out from the transcritical reactor directly push the turbocompressor to pressurize through the expansion of the expander The non-condensable gasCO2 circulates back to the system, which reduces the effective energy loss in the thermal power conversion process: thermal energy→mechanical energy→electrical energy→mechanical energy, improves the thermal power efficiency of thermal energy conversion, and achieves the goal of energy saving, emission reduction and zero emission.
(4)利用循环回系统的CO2从带有多喷头的气体分布管中喷出，推动跨临界反应器内的木片或草片物料定向旋转搅拌和产生“超空泡”效应，强化了反应器内的传热传质。由于跨临界反应器内不需要机械搅拌装置，更有利于高压设备的制造、操作、维修与防漏。(4) Utilize the CO2 recycled to the system to spray out from the gas distribution pipe with multi-nozzles, promote the directional rotation and stirring of the wood chips or grass chips in the transcritical reactor and generate the "supercavitation" effect, which strengthens the reaction Heat and mass transfer in the vessel. Since no mechanical stirring device is required in the transcritical reactor, it is more conducive to the manufacture, operation, maintenance and leakage prevention of high-pressure equipment.
(5)以超/亚临界CO2溶解于水产生的质子酸替代烧碱或硫酸盐或亚硫酸盐进行化学法制浆，具有成本低、没有易燃易爆和强腐蚀性物质，安全性能好。(5) Protonic acid produced by dissolving super/subcriticalCO2 in water instead of caustic soda or sulfate or sulfite for chemical pulping has low cost, no flammable, explosive and strong corrosive substances, and good safety performance .
(6)跨临界CO2水解降解制浆方法比传统制浆方法的纸浆总得率高5％～10％，而且硬度低、强度好、白度高、可漂性好。(6) The total pulp yield of transcriticalCO2 hydrolytic degradation pulping method is 5%-10% higher than that of traditional pulping method, and it has low hardness, good strength, high whiteness and good bleachability.
附图说明Description of drawings
图1是根据本发明的水解制浆的工艺流程图。Figure 1 is a process flow diagram of hydrolytic pulping according to the present invention.
图2是根据本发明反应器的结构示意图。Fig. 2 is a schematic structural view of a reactor according to the present invention.
图3是根据本发明反应器中单个气体分布器的结构示意图。Fig. 3 is a schematic structural view of a single gas distributor in a reactor according to the present invention.
图4是根据本发明反应器中单个气体分布器的俯视图。Figure 4 is a top view of a single gas distributor in a reactor according to the invention.
具体实施方式Detailed ways
下面结合附图，对本发明的具体实施方式进行详细描述，但应当理解本发明的保护范围并不受具体实施方式的限制。The specific embodiments of the present invention will be described in detail below in conjunction with the accompanying drawings, but it should be understood that the protection scope of the present invention is not limited by the specific embodiments.
除非另有其它明确表示，否则在整个说明书和权利要求书中，术语“包括”或其变换如“包含”或“包括有”等等将被理解为包括所陈述的元件或组成部分，而并未排除其它元件或其它组成部分。Unless expressly stated otherwise, throughout the specification and claims, the term "comprise" or variations thereof such as "includes" or "includes" and the like will be understood to include the stated elements or constituents, and not Other elements or other components are not excluded.
实施例1Example 1
如图1至图4所示，用于水解制浆的装置，包括：预处理器1、反应器2、膨胀机3、透平压缩机4、气液分离器5、喷放器6。As shown in FIGS. 1 to 4 , the device for hydrolysis pulping includes: a preprocessor 1 , a reactor 2 , an expander 3 , a turbocompressor 4 , a gas-liquid separator 5 , and a blower 6 .
预处理器1的出料口与所述反应器2的进料口连接，预处理器1用于对生产所需的原料进行加热预处理。反应器2，呈圆柱形，反应器的上部设有进料口21、出气口22，底部设有出料口23，反应器2包括加热管24，为加热盘管，其设于反应器内部；气体分布器25，其包括进气口251和多个用于排气的喷头252；膨胀机3与所述反应器2的出气口连接。透平压缩机4与所述膨胀机3连接，并通过所述膨胀机3驱动所述透平压缩机4工作，所述透平压缩机4的出气口与所述反应器2连接。气液分离器4与所述膨胀机3连接，用于分离反应后产生的混合气体，分离出气体和液体。喷放器6与反应器2连接，用于喷放出反应器2内的浆料和还原糖。The discharge port of the preprocessor 1 is connected with the feed port of the reactor 2, and the preprocessor 1 is used for heating and pretreating the raw materials required for production. The reactor 2 is cylindrical. The upper part of the reactor is provided with a feed inlet 21 and a gas outlet 22, and the bottom is provided with a feed outlet 23. The reactor 2 includes a heating pipe 24, which is a heating coil, which is located inside the reactor. a gas distributor 25, which includes an air inlet 251 and a plurality of nozzles 252 for exhaust; the expander 3 is connected to the gas outlet of the reactor 2. The turbocompressor 4 is connected to the expander 3 , and the turbocompressor 4 is driven to work by the expander 3 , and the gas outlet of the turbocompressor 4 is connected to the reactor 2 . The gas-liquid separator 4 is connected with the expander 3, and is used for separating the mixed gas generated after the reaction, and separating gas and liquid. The ejector 6 is connected with the reactor 2, and is used for ejecting the slurry and reducing sugar in the reactor 2.
优选地，所述气体分布器25呈“L”型，其底端为圆环管状，在该圆环管上均匀设有多个用于排气的喷头252，所述喷头为“L”型，成同一方向倾斜设置。在呈环状的管上均布有多个排气喷头，使气体排放更为均匀，使得至于反应器内的物料与气体充分接触，加快反应速率。呈倾斜设置的喷头喷出的气体往同一方向倾斜喷出气体，使气泡呈旋转状在反应器2内运动，使得反应的物料与气体充分接触，加快反应速度。Preferably, the gas distributor 25 is in an "L" shape, and its bottom end is in the shape of a circular tube, and a plurality of nozzles 252 for exhaust are uniformly arranged on the circular tube, and the nozzles are in an "L" shape , inclined in the same direction. There are multiple exhaust nozzles evenly distributed on the ring-shaped tube to make the gas discharge more uniform, so that the materials in the reactor can fully contact with the gas and speed up the reaction rate. The gas ejected from the oblique nozzles is obliquely ejected in the same direction, so that the bubbles move in the reactor 2 in a rotating shape, so that the reacting materials can fully contact with the gas, and the reaction speed is accelerated.
优选地，所述加热管24为多个，呈平行均布在所述反应器2内部；所述气体分布器25有多个，所述多个气体分布器25相互连通，所述每个气体分布器25的圆环管设在所述加热管24之间。Preferably, there are multiple heating pipes 24, which are uniformly distributed inside the reactor 2 in parallel; there are multiple gas distributors 25, and the multiple gas distributors 25 communicate with each other, and each gas distributor 25 The circular tubes of the distributor 25 are arranged between the heating tubes 24 .
利用上述的装置作为反应装置，一种水解制浆的方法，包括以下步骤：Utilize above-mentioned device as reaction device, a kind of method for hydrolysis pulping, comprises the following steps:
(1)准备原料，将水与甘蔗渣按质量比50:1相互混合，然后预热。(1) Prepare raw materials, mix water and bagasse in a mass ratio of 50:1, and then preheat.
(2)水解反应，将步骤(1)制得的混合物放入反应器内，加热升温至160℃后，往反应器内充入CO2，保持反应器内的温度为160℃，压力为8MPa。(2) Hydrolysis reaction, put the mixture prepared in step (1) into the reactor, heat up to 160°C, fill the reactor with CO2 , keep the temperature in the reactor at 160°C, and the pressure at 8MPa .
(3)取出反应器中反应后的混合气体，混合气体中含有CO2、水蒸汽、糠醛和乙酸，从反应器中取出混合气体的流量为0～10000m3/h，气体流量为0时，没有气体流出。将气体通过膨胀机，经膨胀机膨胀降压为0～1.0MPa，降温为20℃～30℃，进入气液分离器进行分离，气液分离器的温度为10～20℃，压力为0.0～1.0MPa，气液分离器液体流量为0～50m3/h，气体流量为0～8000m3/h，当液体流出量和气体流出量为0时，即没有液体或气体流出。剩下的气体为CO2，将CO2再通入透平压缩机，其与新补充的CO2经透平压缩机加压后通入反应器内。(3) Take out the reacted mixed gas in the reactor. The mixed gas contains CO2 , water vapor, furfural and acetic acid. The flow rate of the mixed gas taken out from the reactor is 0-10000m3 /h. When the gas flow rate is 0, No gas comes out. Pass the gas through the expander, expand and reduce the pressure to 0~1.0MPa, cool down to 20℃~30℃, enter the gas-liquid separator for separation, the temperature of the gas-liquid separator is 10~20℃, and the pressure is 0.0~ 1.0MPa, the liquid flow rate of the gas-liquid separator is 0~50m3 /h, and the gas flow rate is 0~8000m3 /h. When the liquid outflow and gas outflow are 0, there is no liquid or gas outflow. The remaining gas is CO2 , and the CO2 is passed into the turbo compressor again, and the newly supplemented CO2 is pressurized by the turbo compressor and then passed into the reactor.
(4)反应2h后，反应器减压至1.0MPa，从反应器中放出反应制得的浆料和还原糖从反应器中放入喷放器，采用直接全压喷料方法快速放料。蔗渣产浆总得率为62.5％。(4) After reacting for 2 hours, the reactor was decompressed to 1.0MPa, and the slurry and reducing sugar prepared by the reaction were released from the reactor and put into the blower from the reactor, and the direct full-pressure spraying method was used for rapid discharge. The total yield of bagasse pulp is 62.5%.
实施例2Example 2
使用的反应装置与实施例1相同，一种水解制浆的方法，包括以下步骤：The reaction unit that uses is identical with embodiment 1, a kind of method for hydrolysis pulping, comprises the following steps:
(1)准备原料，将水与甘蔗渣按质量比200:1相互混合，然后预热；(1) Prepare the raw materials, mix water and bagasse in a mass ratio of 200:1, and then preheat;
(2)水解反应，将步骤(1)制得的混合物放入反应器内，加热升温至300℃后，往反应器内充入CO2，反应器内的温度为300℃，压力为15MPa；(2) Hydrolysis reaction, put the mixture prepared in step (1) into the reactor, heat up to 300°C, then fill the reactor with CO2 , the temperature in the reactor is 300°C, and the pressure is 15MPa;
(3)取出反应器中反应后的混合气体，混合气体中含有CO2、水蒸汽、糠醛和乙酸，从反应器中取出混合气体的流量为0～10000m3/h，气体流量为0时，没有气体流出。将气体通过膨胀机，经膨胀机膨胀降压为0～1.0MPa，降温为20℃～30℃，进入气液分离器进行分离，气液分离器的温度为10～20℃，压力为0.0～1.0MPa，气液分离器液体流量为0～50m3/h，气体流量为0～8000m3/h，当液体流出量和气体流出量为0时，即没有液体或气体流出。剩下的气体为CO2，将CO2再通入透平压缩机，其与新补充的CO2经透平压缩机加压后通入反应器内；(3) Take out the reacted mixed gas in the reactor. The mixed gas contains CO2 , water vapor, furfural and acetic acid. The flow rate of the mixed gas taken out from the reactor is 0-10000m3 /h. When the gas flow rate is 0, No gas comes out. Pass the gas through the expander, expand and reduce the pressure to 0~1.0MPa, cool down to 20℃~30℃, enter the gas-liquid separator for separation, the temperature of the gas-liquid separator is 10~20℃, and the pressure is 0.0~ 1.0MPa, the liquid flow rate of the gas-liquid separator is 0~50m3 /h, and the gas flow rate is 0~8000m3 /h. When the liquid outflow and gas outflow are 0, there is no liquid or gas outflow. The remaining gas is CO2 , and the CO2 is passed into the turbo compressor again, and the newly supplemented CO2 is pressurized by the turbo compressor and then passed into the reactor;
(4)反应2h后，反应器减压至1.0MPa，从反应器中放出反应制得的浆料和还原糖从反应器中放入喷放器，采用直接全压喷料方法快速放料。蔗渣产浆总得率为61.07％。(4) After reacting for 2 hours, the reactor was decompressed to 1.0MPa, and the slurry and reducing sugar prepared by the reaction were released from the reactor and put into the blower from the reactor, and the direct full-pressure spraying method was used for rapid discharge. The total yield of bagasse pulp was 61.07%.
实施例3Example 3
使用的反应装置与实施例1相同，一种水解制浆的方法，包括以下步骤：The reaction unit that uses is identical with embodiment 1, a kind of method for hydrolysis pulping, comprises the following steps:
(1)准备原料，将水与甘蔗渣按质量比70:1相互混合，然后预热；(1) Prepare the raw materials, mix water and bagasse in a mass ratio of 70:1, and then preheat;
(2)水解反应，将步骤(1)制得的混合物放入反应器内，加热升温至500℃后，往反应器内充入CO2，反应器内的温度为500℃，压力为30MPa；(2) Hydrolysis reaction, put the mixture prepared in step (1) into the reactor, heat up to 500°C, then fill the reactor with CO2 , the temperature in the reactor is 500°C, and the pressure is 30MPa;
(3)取出反应器中反应后的混合气体，混合气体中含有CO2、水蒸汽、糠醛和乙酸，从反应器中取出混合气体的流量为0～10000m3/h，气体流量为0时，没有气体流出。将气体通过膨胀机，经膨胀机膨胀降压为0～1.0MPa，降温为20℃～30℃，进入气液分离器进行分离，气液分离器的温度为10～20℃，压力为0.0～1.0MPa，气液分离器液体流量为0～50m3/h，气体流量为0～8000m3/h，当液体流出量和气体流出量为0时，即没有液体或气体流出。剩下的气体为CO2，将CO2再通入透平压缩机，其与新补充的CO2经透平压缩机加压后通入反应器内；(3) Take out the reacted mixed gas in the reactor. The mixed gas contains CO2 , water vapor, furfural and acetic acid. The flow rate of the mixed gas taken out from the reactor is 0-10000m3 /h. When the gas flow rate is 0, No gas comes out. Pass the gas through the expander, expand and reduce the pressure to 0~1.0MPa, cool down to 20℃~30℃, enter the gas-liquid separator for separation, the temperature of the gas-liquid separator is 10~20℃, and the pressure is 0.0~ 1.0MPa, the liquid flow rate of the gas-liquid separator is 0~50m3 /h, and the gas flow rate is 0~8000m3 /h. When the liquid outflow and gas outflow are 0, there is no liquid or gas outflow. The remaining gas is CO2 , and the CO2 is passed into the turbo compressor again, and the newly supplemented CO2 is pressurized by the turbo compressor and then passed into the reactor;
(4)反应3h后，反应器减压至1.0MPa，从反应器中放出反应制得的浆料和还原糖从反应器中放入喷放器，采用直接全压喷料方法快速放料。蔗渣产浆总得率为55.10％。(4) After reacting for 3 hours, the reactor was decompressed to 1.0MPa, and the slurry and reducing sugar prepared by the reaction were released from the reactor and put into the blower from the reactor, and the direct full-pressure spraying method was used for rapid discharge. The total yield of bagasse pulp is 55.10%.
实施例4Example 4
使用的反应装置与实施例1相同，一种水解制浆的方法，包括以下步骤：The reaction unit that uses is identical with embodiment 1, a kind of method for hydrolysis pulping, comprises the following steps:
(1)准备原料，将水与单竹按质量比50:1相互混合，然后预热；(1) Prepare raw materials, mix water and single bamboo in a mass ratio of 50:1, and then preheat;
(2)水解反应，将步骤(1)制得的混合物放入反应器内，加热升温至150℃后，往反应器内充入CO2，反应器内的温度为150℃，压力为8MPa；(2) Hydrolysis reaction, put the mixture prepared in step (1) into the reactor, heat up to 150°C, then fill the reactor with CO2 , the temperature in the reactor is 150°C, and the pressure is 8MPa;
(3)取出反应器中反应后的混合气体，混合气体中含有CO2、水蒸汽、糠醛和乙酸，从反应器中取出混合气体的流量为0～10000m3/h，气体流量为0时，没有气体流出。将气体通过膨胀机，经膨胀机膨胀降压为0～1.0MPa，降温为20℃～30℃，进入气液分离器进行分离，气液分离器的温度为10～20℃，压力为0.0～1.0MPa，气液分离器液体流量为0～50m3/h，气体流量为0～8000m3/h，当液体流出量和气体流出量为0时，即没有液体或气体流出。剩下的气体为CO2，将CO2再通入透平压缩机，其与新补充的CO2经透平压缩机加压后通入反应器内；(3) Take out the reacted mixed gas in the reactor. The mixed gas contains CO2 , water vapor, furfural and acetic acid. The flow rate of the mixed gas taken out from the reactor is 0-10000m3 /h. When the gas flow rate is 0, No gas comes out. Pass the gas through the expander, expand and reduce the pressure to 0~1.0MPa, cool down to 20℃~30℃, enter the gas-liquid separator for separation, the temperature of the gas-liquid separator is 10~20℃, and the pressure is 0.0~ 1.0MPa, the liquid flow rate of the gas-liquid separator is 0~50m3 /h, and the gas flow rate is 0~8000m3 /h. When the liquid outflow and gas outflow are 0, there is no liquid or gas outflow. The remaining gas is CO2 , and the CO2 is passed into the turbo compressor again, and the newly supplemented CO2 is pressurized by the turbo compressor and then passed into the reactor;
(4)反应3h后，反应器减压至1.0MPa，从反应器中放出反应制得的浆料和还原糖从反应器中放入喷放器，采用直接全压喷料方法快速放料。单竹产浆总得率为52.40％。(4) After reacting for 3 hours, the reactor was decompressed to 1.0MPa, and the slurry and reducing sugar prepared by the reaction were released from the reactor and put into the blower from the reactor, and the direct full-pressure spraying method was used for rapid discharge. The total pulp yield of single bamboo is 52.40%.
实施例5Example 5
使用的反应装置与实施例1相同，一种水解制浆的方法，包括以下步骤：The reaction unit that uses is identical with embodiment 1, a kind of method for hydrolysis pulping, comprises the following steps:
(1)准备原料，将水与单竹按质量比200:1相互混合，然后预热；(1) Prepare raw materials, mix water and single bamboo in a mass ratio of 200:1, and then preheat;
(2)水解反应，将步骤(1)制得的混合物放入反应器内，加热升温至300℃后，往反应器内充入CO2，反应器内的温度为300℃，压力为3MPa；(2) Hydrolysis reaction, put the mixture prepared in step (1) into the reactor, heat up to 300°C, then fill the reactor with CO2 , the temperature in the reactor is 300°C, and the pressure is 3MPa;
(3)取出反应器中反应后的混合气体，混合气体中含有CO2、水蒸汽、糠醛和乙酸，从反应器中取出混合气体的流量为0～10000m3/h，气体流量为0时，没有气体流出。将气体通过膨胀机，经膨胀机膨胀降压为0～1.0MPa，降温为20℃～30℃，进入气液分离器进行分离，气液分离器的温度为10～20℃，压力为0.0～1.0MPa，气液分离器液体流量为0～50m3/h，气体流量为0～8000m3/h，当液体流出量和气体流出量为0时，即没有液体或气体流出。剩下的气体为CO2，将CO2再通入透平压缩机，其与新补充的CO2经透平压缩机加压后通入反应器内；(3) Take out the reacted mixed gas in the reactor. The mixed gas contains CO2 , water vapor, furfural and acetic acid. The flow rate of the mixed gas taken out from the reactor is 0-10000m3 /h. When the gas flow rate is 0, No gas comes out. Pass the gas through the expander, expand and reduce the pressure to 0~1.0MPa, cool down to 20℃~30℃, enter the gas-liquid separator for separation, the temperature of the gas-liquid separator is 10~20℃, and the pressure is 0.0~ 1.0MPa, the liquid flow rate of the gas-liquid separator is 0~50m3 /h, and the gas flow rate is 0~8000m3 /h. When the liquid outflow and gas outflow are 0, there is no liquid or gas outflow. The remaining gas is CO2 , and the CO2 is passed into the turbo compressor again, and the newly supplemented CO2 is pressurized by the turbo compressor and then passed into the reactor;
(4)反应3h后，反应器减压至1.0MPa，从反应器中放出反应制得的浆料和还原糖从反应器中放入喷放器，采用直接全压喷料方法快速放料。单竹产浆总得率为48.70％。(4) After reacting for 3 hours, the reactor was decompressed to 1.0MPa, and the slurry and reducing sugar prepared by the reaction were released from the reactor and put into the blower from the reactor, and the direct full-pressure spraying method was used for rapid discharge. The total pulp yield of single bamboo was 48.70%.
实施例6Example 6
使用的反应装置与实施例1相同，一种水解制浆的方法，包括以下步骤：The reaction unit that uses is identical with embodiment 1, a kind of method for hydrolysis pulping, comprises the following steps:
(1)准备原料，将水与稻草按质量比2:1相互混合，然后预热；(1) Prepare raw materials, mix water and rice straw with each other in a mass ratio of 2:1, and then preheat;
(2)水解反应，将步骤(1)制得的混合物放入反应器内，加热升温至150℃后，往反应器内充入CO2，保持反应器内的温度为150℃，压力为8MPa；(2) Hydrolysis reaction, put the mixture prepared in step (1) into the reactor, heat up to 150°C, fill the reactor with CO2 , keep the temperature in the reactor at 150°C, and the pressure at 8MPa ;
(3)取出反应器中反应后的混合气体，混合气体中含有CO2、水蒸汽、糠醛和乙酸，从反应器中取出混合气体的流量为0～10000m3/h，气体流量为0时，没有气体流出。将气体通过膨胀机，经膨胀机膨胀降压为0～1.0MPa，降温为20℃～30℃，进入气液分离器进行分离，气液分离器的温度为10～20℃，压力为0.0～1.0MPa，气液分离器液体流量为0～50m3/h，气体流量为0～8000m3/h，当液体流出量和气体流出量为0时，即没有液体或气体流出。剩下的气体为CO2，将CO2再通入透平压缩机，其与新补充的CO2经透平压缩机加压后通入反应器内；(3) Take out the reacted mixed gas in the reactor. The mixed gas contains CO2 , water vapor, furfural and acetic acid. The flow rate of the mixed gas taken out from the reactor is 0-10000m3 /h. When the gas flow rate is 0, No gas comes out. Pass the gas through the expander, expand and reduce the pressure to 0~1.0MPa, cool down to 20℃~30℃, enter the gas-liquid separator for separation, the temperature of the gas-liquid separator is 10~20℃, and the pressure is 0.0~ 1.0MPa, the liquid flow rate of the gas-liquid separator is 0~50m3 /h, and the gas flow rate is 0~8000m3 /h. When the liquid outflow and gas outflow are 0, there is no liquid or gas outflow. The remaining gas is CO2 , and the CO2 is passed into the turbo compressor again, and the newly supplemented CO2 is pressurized by the turbo compressor and then passed into the reactor;
(4)反应4h后，反应器减压至1.0MPa，从反应器中放出反应制得的浆料和还原糖从反应器中放入喷放器，采用直接全压喷料方法快速放料。稻草产浆总得率为56.60％。(4) After reacting for 4 hours, the reactor was decompressed to 1.0MPa, and the slurry and reducing sugar produced by the reaction were released from the reactor and put into the blower from the reactor, and the direct full-pressure spraying method was used for rapid discharge. The total yield of rice straw pulp was 56.60%.
实施例7Example 7
使用的反应装置与实施例1相同，一种水解制浆的方法，包括以下步骤：The reaction unit that uses is identical with embodiment 1, a kind of method for hydrolysis pulping, comprises the following steps:
(1)准备原料，将水与稻草按质量比200:1相互混合，然后预热；(1) Prepare raw materials, mix water and rice straw with each other at a mass ratio of 200:1, and then preheat;
(2)水解反应，将步骤(1)制得的混合物放入反应器内，加热升温至300℃后，往反应器内充入CO2，保持反应器内的温度为300℃，压力为15MPa；(2) Hydrolysis reaction, put the mixture prepared in step (1) into the reactor, heat up to 300°C, fill the reactor with CO2 , keep the temperature in the reactor at 300°C, and the pressure at 15MPa ;
(3)取出反应器中反应后的混合气体，混合气体中含有CO2、水蒸汽、糠醛和乙酸，从反应器中取出混合气体的流量为0～10000m3/h，气体流量为0时，没有气体流出。将气体通过膨胀机，经膨胀机膨胀降压为0～1.0MPa，降温为20℃～30℃，进入气液分离器进行分离，气液分离器的温度为10～20℃，压力为0.0～1.0MPa，气液分离器液体流量为0～50m3/h，气体流量为0～8000m3/h，当液体流出量和气体流出量为0时，即没有液体或气体流出。剩下的气体为CO2，将CO2再通入透平压缩机，其与新补充的CO2经透平压缩机加压后通入反应器内；(3) Take out the reacted mixed gas in the reactor. The mixed gas contains CO2 , water vapor, furfural and acetic acid. The flow rate of the mixed gas taken out from the reactor is 0-10000m3 /h. When the gas flow rate is 0, No gas comes out. Pass the gas through the expander, expand and reduce the pressure to 0~1.0MPa, cool down to 20℃~30℃, enter the gas-liquid separator for separation, the temperature of the gas-liquid separator is 10~20℃, and the pressure is 0.0~ 1.0MPa, the liquid flow rate of the gas-liquid separator is 0~50m3 /h, and the gas flow rate is 0~8000m3 /h. When the liquid outflow and gas outflow are 0, there is no liquid or gas outflow. The remaining gas is CO2 , and the CO2 is passed into the turbo compressor again, and the newly supplemented CO2 is pressurized by the turbo compressor and then passed into the reactor;
(4)反应1h后，反应器减压至1.0MPa，从反应器中放出反应制得的浆料和还原糖从反应器中放入喷放器，采用直接全压喷料方法快速放料。稻草产浆总得率为55.42％。(4) After reacting for 1 hour, the reactor was decompressed to 1.0MPa, and the slurry and reducing sugar prepared by the reaction were released from the reactor and put into the blower from the reactor, and the direct full-pressure spraying method was used for rapid discharge. The total yield of rice straw pulp was 55.42%.
实施例8Example 8
使用的反应装置与实施例1相同，一种水解制浆的方法，包括以下步骤：The reaction unit that uses is identical with embodiment 1, a kind of method for hydrolysis pulping, comprises the following steps:
(1)准备原料，将水与马尾松按质量比20:1相互混合，然后预热；(1) Prepare raw materials, mix water and masson pine with each other in a mass ratio of 20:1, and then preheat;
(2)水解反应，将步骤(1)制得的混合物放入反应器内，加热升温至300℃后，往反应器内充入CO2，保持反应器内的温度为300℃，压力为15MPa；(2) Hydrolysis reaction, put the mixture prepared in step (1) into the reactor, heat up to 300°C, fill the reactor with CO2 , keep the temperature in the reactor at 300°C, and the pressure at 15MPa ;
(3)取出反应器中反应后的混合气体，混合气体中含有CO2、水蒸汽、糠醛和乙酸，从反应器中取出混合气体的流量为0～10000m3/h，气体流量为0时，没有气体流出。将气体通过膨胀机，经膨胀机膨胀降压为0～1.0MPa，降温为20℃～30℃，进入气液分离器进行分离，气液分离器的温度为10～20℃，压力为0.0～1.0MPa，气液分离器液体流量为0～50m3/h，气体流量为0～8000m3/h，当液体流出量和气体流出量为0时，即没有液体或气体流出。剩下的气体为CO2，将CO2再通入透平压缩机，其与新补充的CO2经透平压缩机加压后通入反应器内；(3) Take out the reacted mixed gas in the reactor. The mixed gas contains CO2 , water vapor, furfural and acetic acid. The flow rate of the mixed gas taken out from the reactor is 0-10000m3 /h. When the gas flow rate is 0, No gas comes out. Pass the gas through the expander, expand and reduce the pressure to 0~1.0MPa, cool down to 20℃~30℃, enter the gas-liquid separator for separation, the temperature of the gas-liquid separator is 10~20℃, and the pressure is 0.0~ 1.0MPa, the liquid flow rate of the gas-liquid separator is 0~50m3 /h, and the gas flow rate is 0~8000m3 /h. When the liquid outflow and gas outflow are 0, there is no liquid or gas outflow. The remaining gas is CO2 , and the CO2 is passed into the turbo compressor again, and the newly supplemented CO2 is pressurized by the turbo compressor and then passed into the reactor;
(4)反应5h后，反应器减压至1.0MPa，从反应器中放出反应制得的浆料和还原糖从反应器中放入喷放器，采用直接全压喷料方法快速放料，马尾松产浆总得率为61.20％。(4) After reacting for 5h, the reactor was decompressed to 1.0MPa, and the slurry prepared by the reaction and reducing sugar were released from the reactor and put into the blower from the reactor, and the direct full-pressure spraying method was used to discharge quickly, The total yield of masson pine pulp was 61.20%.
实施例9Example 9
使用的反应装置与实施例1相同，一种水解制浆的方法，包括以下步骤：The reaction unit that uses is identical with embodiment 1, a kind of method for hydrolysis pulping, comprises the following steps:
(1)准备原料，将水与马尾松按质量比50:1相互混合，然后预热；(1) Prepare raw materials, mix water and masson pine with each other in a mass ratio of 50:1, and then preheat;
(2)水解反应，将步骤(1)制得的混合物放入反应器内，加热升温至400℃后，往反应器内充入CO2，保持反应器内的温度为400℃，压力为15MPa；(2) Hydrolysis reaction, put the mixture prepared in step (1) into the reactor, heat up to 400°C, fill the reactor with CO2 , keep the temperature in the reactor at 400°C, and the pressure at 15MPa ;
(3)取出反应器中反应后的混合气体，混合气体中含有CO2、水蒸汽、糠醛和乙酸，从反应器中取出混合气体的流量为0～12000m3/h，气体流量为0时，没有气体流出。将气体通过膨胀机，经膨胀机膨胀降压为0～1.0MPa，降温为60℃～70℃，进入气液分离器进行分离，气液分离器的温度为20～30℃，压力为0.0～1.0MPa，气液分离器液体流量为0～70m3/h，气体流量为0～9000m3/h，当液体流出量和气体流出量为0时，即没有液体或气体流出。剩下的气体为CO2，将CO2再通入透平压缩机，其与新补充的CO2经透平压缩机加压后通入反应器内；(3) Take out the reacted mixed gas in the reactor. The mixed gas contains CO2 , water vapor, furfural and acetic acid. The flow rate of the mixed gas taken out from the reactor is 0～12000m3 /h. When the gas flow rate is 0, No gas comes out. Pass the gas through the expander, expand and reduce the pressure to 0~1.0MPa, cool down to 60℃~70℃, and enter the gas-liquid separator for separation. The temperature of the gas-liquid separator is 20~30℃, and the pressure is 0.0~ 1.0MPa, the liquid flow rate of the gas-liquid separator is 0-70m3 /h, and the gas flow rate is 0-9000m3 /h. When the liquid outflow and gas outflow are 0, there is no liquid or gas outflow. The remaining gas is CO2 , and the CO2 is passed into the turbo compressor again, and the newly supplemented CO2 is pressurized by the turbo compressor and then passed into the reactor;
(4)反应5h后，反应器减压至1.0MPa，从反应器中放出反应制得的浆料和还原糖从反应器中放入喷放器，采用直接全压喷料方法快速放料。马尾松产浆总得率为60.70％。(4) After reacting for 5 hours, the reactor was decompressed to 1.0MPa, and the slurry and reducing sugar produced by the reaction were released from the reactor and put into the blower from the reactor, and the direct full-pressure spraying method was used for rapid discharge. The total yield of masson pine pulp was 60.70%.
实施例10Example 10
使用的反应装置与实施例1相同，一种水解制浆的方法，包括以下步骤：The reaction unit that uses is identical with embodiment 1, a kind of method for hydrolysis pulping, comprises the following steps:
(1)准备原料，将水与稻草按质量比100:1相互混合，然后预热；(1) Prepare raw materials, mix water and rice straw with each other in a mass ratio of 100:1, and then preheat;
(2)水解反应，将步骤(1)制得的混合物放入反应器内，加热升温至200℃后，往反应器内充入CO2，保持反应器内的温度为200℃，压力为8MPa；(2) Hydrolysis reaction, put the mixture prepared in step (1) into the reactor, heat up to 200°C, fill the reactor with CO2 , keep the temperature in the reactor at 200°C, and the pressure at 8MPa ;
(3)取出反应器中反应后的混合气体，混合气体中含有CO2、水蒸汽、糠醛和乙酸，从反应器中取出混合气体的流量为0～10000m3/h，气体流量为0时，没有气体流出。将气体通过膨胀机，经膨胀机膨胀降压为0～1.0MPa，降温为30℃～40℃，进入气液分离器进行分离，气液分离器的温度为20～30℃，压力为0.0～1.0MPa，气液分离器液体流量为0～20m3/h，气体流量为0～5000m3/h，当液体流出量和气体流出量为0时，即没有液体或气体流出。剩下的气体为CO2，将CO2再通入透平压缩机，其与新补充的CO2经透平压缩机加压后通入反应器内；(3) Take out the reacted mixed gas in the reactor. The mixed gas contains CO2 , water vapor, furfural and acetic acid. The flow rate of the mixed gas taken out from the reactor is 0-10000m3 /h. When the gas flow rate is 0, No gas comes out. Pass the gas through the expander, expand and reduce the pressure to 0~1.0MPa, drop the temperature to 30℃~40℃, enter the gas-liquid separator for separation, the temperature of the gas-liquid separator is 20~30℃, and the pressure is 0.0~ 1.0MPa, the liquid flow rate of the gas-liquid separator is 0~20m3 /h, and the gas flow rate is 0~5000m3 /h. When the liquid outflow and gas outflow are 0, there is no liquid or gas outflow. The remaining gas is CO2 , and the CO2 is passed into the turbo compressor again, and the newly supplemented CO2 is pressurized by the turbo compressor and then passed into the reactor;
(4)反应2h后，反应器减压至1.0MPa，从反应器中放出反应制得的浆料和还原糖从反应器中放入喷放器，采用直接全压喷料方法快速放料。稻草产浆总得率为61.70％。(4) After reacting for 2 hours, the reactor was decompressed to 1.0MPa, and the slurry and reducing sugar prepared by the reaction were released from the reactor and put into the blower from the reactor, and the direct full-pressure spraying method was used for rapid discharge. The total yield of rice straw pulp was 61.70%.
实施例11Example 11
使用的反应装置与实施例1相同，一种水解制浆的方法，包括以下步骤：The reaction unit that uses is identical with embodiment 1, a kind of method for hydrolysis pulping, comprises the following steps:
(1)准备原料，将水与稻草按质量比150:1相互混合，然后预热；(1) Prepare raw materials, mix water and rice straw with each other at a mass ratio of 150:1, and then preheat;
(2)水解反应，将步骤(1)制得的混合物放入反应器内，加热升温至250℃后，往反应器内充入CO2，保持反应器内的温度为250℃，压力为8MPa；(2) Hydrolysis reaction, put the mixture prepared in step (1) into the reactor, heat up to 250°C, fill the reactor with CO2 , keep the temperature in the reactor at 250°C, and the pressure at 8MPa ;
(3)取出反应器中反应后的混合气体，混合气体中含有CO2、水蒸汽、糠醛和乙酸，从反应器中取出混合气体的流量为0～10000m3/h，气体流量为0时，没有气体流出。将气体通过膨胀机，经膨胀机膨胀降压为0～1.0MPa，降温为70℃～80℃，进入气液分离器进行分离，气液分离器的温度为30～40℃，压力为0.0～1.0MPa，气液分离器液体流量为0～70m3/h，气体流量为0～8000m3/h，当液体流出量和气体流出量为0时，即没有液体和气体流出。剩下的气体为CO2，将CO2再通入透平压缩机，其与新补充的CO2经透平压缩机加压后通入反应器内；(3) Take out the reacted mixed gas in the reactor. The mixed gas contains CO2 , water vapor, furfural and acetic acid. The flow rate of the mixed gas taken out from the reactor is 0-10000m3 /h. When the gas flow rate is 0, No gas comes out. Pass the gas through the expander, expand and reduce the pressure to 0~1.0MPa, cool down to 70℃~80℃, enter the gas-liquid separator for separation, the temperature of the gas-liquid separator is 30~40℃, and the pressure is 0.0~ 1.0MPa, the liquid flow rate of the gas-liquid separator is 0-70m3 /h, and the gas flow rate is 0-8000m3 /h. When the liquid outflow and gas outflow are 0, there is no liquid and gas outflow. The remaining gas is CO2 , and the CO2 is passed into the turbo compressor again, and the newly supplemented CO2 is pressurized by the turbo compressor and then passed into the reactor;
(4)反应2h后，反应器减压至1.0MPa，从反应器中放出反应制得的浆料和还原糖从反应器中放入喷放器，采用直接全压喷料方法快速放料。稻草产浆总得率为56.10％。(4) After reacting for 2 hours, the reactor was decompressed to 1.0MPa, and the slurry and reducing sugar prepared by the reaction were released from the reactor and put into the blower from the reactor, and the direct full-pressure spraying method was used for rapid discharge. The total yield of rice straw pulp was 56.10%.
实施例12Example 12
使用的反应装置与实施例1相同，一种水解制浆的方法，包括以下步骤：The reaction unit that uses is identical with embodiment 1, a kind of method for hydrolysis pulping, comprises the following steps:
(1)准备原料，将水与马尾松按质量比10:1相互混合，然后预热；(1) Prepare the raw materials, mix water and masson pine with each other in a mass ratio of 10:1, and then preheat;
(2)水解反应，将步骤(1)制得的混合物放入反应器内，加热升温至350℃后，往反应器内充入CO2，保持反应器内的温度为350℃，压力为8MPa；(2) Hydrolysis reaction, put the mixture prepared in step (1) into the reactor, heat up to 350°C, fill the reactor with CO2 , keep the temperature in the reactor at 350°C, and the pressure at 8MPa ;
(3)取出反应器中反应后的混合气体，混合气体中含有CO2、水蒸汽、糠醛和乙酸，从反应器中取出混合气体的流量为0～8000m3/h，气体流量为0时，没有气体流出。将气体通过膨胀机，经膨胀机膨胀降压为0～1.0MPa，降温为20℃～30℃，进入气液分离器进行分离，气液分离器的温度为5～15℃，压力为0.0～1.0MPa，气液分离器液体流量为0～100m3/h，气体流量为0～7000m3/h，当液体流出量和气体流出量为0时，即没有液体和气体流出。剩下的气体为CO2，将CO2再通入透平压缩机，其与新补充的CO2经透平压缩机加压后通入反应器内；(3) Take out the reacted mixed gas in the reactor. The mixed gas contains CO2 , water vapor, furfural and acetic acid. The flow rate of the mixed gas taken out from the reactor is 0-8000m3 /h. When the gas flow rate is 0, No gas comes out. Pass the gas through the expander, expand and reduce the pressure to 0~1.0MPa, cool down to 20℃~30℃, enter the gas-liquid separator for separation, the temperature of the gas-liquid separator is 5~15℃, and the pressure is 0.0~ 1.0MPa, the liquid flow rate of the gas-liquid separator is 0-100m3 /h, and the gas flow rate is 0-7000m3 /h. When the liquid outflow and gas outflow are 0, there is no liquid and gas outflow. The remaining gas is CO2 , and the CO2 is passed into the turbo compressor again, and the newly supplemented CO2 is pressurized by the turbo compressor and then passed into the reactor;
(4)反应2h后，反应器减压至1.0MPa，从反应器中放出反应制得的浆料和还原糖从反应器中放入喷放器，采用直接全压喷料方法快速放料。马尾松产浆总得率为60.20％。(4) After reacting for 2 hours, the reactor was decompressed to 1.0MPa, and the slurry and reducing sugar prepared by the reaction were released from the reactor and put into the blower from the reactor, and the direct full-pressure spraying method was used for rapid discharge. The total yield of masson pine pulp was 60.20%.
前述对本发明的具体示例性实施方案的描述是为了说明和例证的目的。这些描述并非想将本发明限定为所公开的精确形式，并且很显然，根据上述教导，可以进行很多改变和变化。对示例性实施例进行选择和描述的目的在于解释本发明的特定原理及其实际应用，从而使得本领域的技术人员能够实现并利用本发明的各种不同的示例性实施方案以及各种不同的选择和改变。本发明的范围意在由权利要求书及其等同形式所限定。The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. These descriptions are not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application, thereby enabling others skilled in the art to make and use various exemplary embodiments of the invention, as well as various Choose and change. It is intended that the scope of the invention be defined by the claims and their equivalents.
| Application Number | Priority Date | Filing Date | Title |
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| CN201510082886.3ACN104674585B (en) | 2015-02-15 | 2015-02-15 | Transcritical CO_2 response system hydrolyzes the method and device of slurrying |
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| CN201510082886.3ACN104674585B (en) | 2015-02-15 | 2015-02-15 | Transcritical CO_2 response system hydrolyzes the method and device of slurrying |
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| CN201510082886.3AActiveCN104674585B (en) | 2015-02-15 | 2015-02-15 | Transcritical CO_2 response system hydrolyzes the method and device of slurrying |
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| CN105200834A (en)* | 2015-09-30 | 2015-12-30 | 广西大学 | Method of producing pulp by instant vaporization expansion-infiltration in straw sheets |
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| CN101591362A (en)* | 2009-06-25 | 2009-12-02 | 河南科技大学 | Supercritical CO 2-water system hydrolytic inulin prepares the method for fructose |
| WO2011091044A1 (en)* | 2010-01-19 | 2011-07-28 | Sriya Innovations, Inc. | Production of fermentable sugars and lignin from biomass using supercritical fluids |
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| CN101591362A (en)* | 2009-06-25 | 2009-12-02 | 河南科技大学 | Supercritical CO 2-water system hydrolytic inulin prepares the method for fructose |
| WO2011091044A1 (en)* | 2010-01-19 | 2011-07-28 | Sriya Innovations, Inc. | Production of fermentable sugars and lignin from biomass using supercritical fluids |
| CN103097539A (en)* | 2010-03-30 | 2013-05-08 | 康奈尔大学 | Biphasic supercritical carbon dioxide-water pretreatment of lignocellulosic biomass |
| CN103502257A (en)* | 2011-05-04 | 2014-01-08 | 瑞恩麦特克斯股份有限公司 | Multistage cellulose hydrolysis and quench with or without acid |
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| CN105200834A (en)* | 2015-09-30 | 2015-12-30 | 广西大学 | Method of producing pulp by instant vaporization expansion-infiltration in straw sheets |
| CN105200834B (en)* | 2015-09-30 | 2017-12-22 | 广西大学 | Pulping process expand-is permeated in instant vaporization inside blade |
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