技术领域technical field
本发明属于材料领域，具体涉及一种尼龙阀体材料及其制备方法。The invention belongs to the field of materials, and in particular relates to a nylon valve body material and a preparation method thereof.
背景技术Background technique
阀门是流体输送系统中的控制部件，具有截止、调节、导流、防止逆流、稳压、分流或溢流泄压等功能。用于流体控制系统的阀门，从最简单的截止阀到极为复杂的自控系统中所用的各种阀门，其品种和规格相当繁多。阀门可用于控制空气、水、蒸汽、各种腐蚀性介质、泥浆、油品、液态金属和放射性介质等各种类型流体的流动。阀门根据材质还分为铸铁阀门，铸钢阀门，不锈钢阀门，铬钼钢阀门，铬钼钒钢阀门，双相钢阀门，塑料阀门，非标订制阀门等；The valve is a control component in the fluid conveying system, which has the functions of cut-off, regulation, diversion, prevention of backflow, voltage stabilization, diversion or overflow and pressure relief. Valves used in fluid control systems, from the simplest shut-off valve to various valves used in extremely complex automatic control systems, have a wide variety and specifications. Valves can be used to control the flow of various types of fluids such as air, water, steam, various corrosive media, mud, oil, liquid metal and radioactive media. Valves are also divided into cast iron valves, cast steel valves, stainless steel valves, chrome molybdenum steel valves, chrome molybdenum vanadium steel valves, duplex steel valves, plastic valves, non-standard customized valves, etc.
尼龙作为工程塑料中最大最重要的品种，具有很强的生命力，主要在于它改性后实现高性能化，其次是汽车、电器、通讯、电子、机械等产业自身对产品高性能的要求越来越强烈，相关产业的飞速发展，促进了工程塑料高性能化的进程，改性尼龙未来发展趋势如下：①高强度高刚性尼龙的市场需求量越来越大，新的增强材料如无机晶须增强、碳纤维增强PA将成为重要的品种，主要是用于汽车发动机部件，机械部件以及航空设备部件。②尼龙合金化将成为改性工程塑料发展的主流。尼龙合金化是实现尼龙高性能的重要途径，也是制造尼龙、尼龙专用料、提高尼龙性能的主要手段。通过掺混其他高聚物，来改善尼龙的吸水性，提高制品的尺寸稳定性，以及低温脆性、耐热性和耐磨性。从而，适用车种不同要求的用途。③纳米尼龙的制造技术与应用将得到迅速发展。纳米尼龙的优点在于其热性能、力学性能、阻燃性、阻隔性比纯尼龙高，而制造成本与普通尼龙相当。因而，具有很大的竞争力。④用于电子、电气、电器的阻燃尼龙与日俱增，绿色化阻燃尼龙越来越受到市场的重视。⑤抗静电、导电尼龙以及磁性尼龙将成为电子设备、矿山机械、纺织机械的首选材料。⑥加工助剂的研究与应用，将推动改性尼龙的功能化、高性能化的进程。⑦综合技术的应用，产品的精细化是推动其产业发展的动力；As the largest and most important variety of engineering plastics, nylon has a strong vitality, mainly because it can achieve high performance after modification, followed by the automobile, electrical appliances, communications, electronics, machinery and other industries themselves have more and more high-performance requirements for products. The more intense, the rapid development of related industries has promoted the process of high-performance engineering plastics. The future development trend of modified nylon is as follows: ① The market demand for high-strength and high-rigidity nylon is increasing, and new reinforcing materials such as inorganic whiskers Reinforced, carbon fiber reinforced PA will become an important variety, mainly used for automotive engine parts, mechanical parts and aviation equipment parts. ②Nylon alloying will become the mainstream of the development of modified engineering plastics. Nylon alloying is an important way to achieve high performance of nylon, and it is also the main means to manufacture nylon and nylon special materials and improve the performance of nylon. By blending other polymers, it can improve the water absorption of nylon, improve the dimensional stability of the product, as well as low temperature brittleness, heat resistance and wear resistance. Therefore, it is suitable for the applications required by different types of vehicles. ③ The manufacturing technology and application of nano-nylon will be developed rapidly. The advantages of nano-nylon are that its thermal properties, mechanical properties, flame retardancy and barrier properties are higher than those of pure nylon, and the manufacturing cost is comparable to that of ordinary nylon. Therefore, it has great competitiveness. ④ The flame retardant nylon used in electronics, electrical appliances and electrical appliances is increasing day by day, and the green flame retardant nylon has received more and more attention from the market. ⑤Antistatic, conductive nylon and magnetic nylon will become the preferred materials for electronic equipment, mining machinery and textile machinery. ⑥ The research and application of processing aids will promote the process of functionalization and high performance of modified nylon. ⑦ The application of comprehensive technology and the refinement of products are the driving force for the development of its industry;
目前，作为阀体材料的非金属类材料有聚四氟乙烯、聚丙烯、聚乙烯、聚氯乙烯等，尼龙却很少被用于作为阀体材料，因此，本发明的目的就是提供一种高性能的尼龙材料，以满足其在阀体材料的应用。At present, the non-metallic materials used as valve body materials include polytetrafluoroethylene, polypropylene, polyethylene, polyvinyl chloride, etc., but nylon is rarely used as valve body material. Therefore, the purpose of the present invention is to provide a High performance nylon material to meet its application in valve body material.
发明内容SUMMARY OF THE INVENTION
本发明的目的是提供一种尼龙阀体材料及其制备方法。The purpose of the present invention is to provide a nylon valve body material and a preparation method thereof.
为实现上述目的，本发明采用以下技术方案：To achieve the above object, the present invention adopts the following technical solutions:
一种尼龙阀体材料，包括下述重量份的各原料：A nylon valve body material, comprising the following raw materials in parts by weight:
亚磷酸双酚A 酯4-7、己内酰胺160-200、引发剂5-7、苯酚36-40、37%的甲醛20-30、氢氧化钠1-2、碳化硅纤维3-4、钛酸四丁酯20-30、二硫代水杨酸1-2、聚酰胺蜡微粉4-6、硅烷偶联剂kh550 2-3、甲基丙烯酸缩水甘油酯4-7。Bisphenol A phosphite 4-7, caprolactam 160-200, initiator 5-7, phenol 36-40, 37% formaldehyde 20-30, sodium hydroxide 1-2, silicon carbide fiber 3-4, titanic acid Tetrabutyl ester 20-30, dithiosalicylic acid 1-2, polyamide wax micropowder 4-6, silane coupling agent kh550 2-3, glycidyl methacrylate 4-7.
所述的引发剂为过氧化二异丙苯。The initiator is dicumyl peroxide.
一种尼龙阀体材料的制备方法，包括以下步骤：A preparation method of nylon valve body material, comprising the following steps:
（1）取引发剂，加入到其重量20-30倍的无水乙醇中，搅拌均匀，得引发剂溶液；(1) Take the initiator, add it to 20-30 times its weight in absolute ethanol, stir evenly, and obtain the initiator solution;
（2）取钛酸四丁酯、二硫代水杨酸混合，加入到混合料重量51-60倍的去离子水中，搅拌反应3-5小时，得溶胶分散液；(2) Mix tetrabutyl titanate and dithiosalicylic acid, add them into deionized water with a weight of 51-60 times the weight of the mixture, and stir and react for 3-5 hours to obtain a sol dispersion;
（3）取聚酰胺蜡微粉、硅烷偶联剂kh550混合，加入到混合料重量7-9倍的无水乙醇中，在60-65℃下保温搅拌1-2小时，蒸馏除去乙醇，得氨基蜡微粉；(3) Mix the polyamide wax micropowder and silane coupling agent kh550, add it into absolute ethanol 7-9 times the weight of the mixture, keep stirring at 60-65°C for 1-2 hours, remove the ethanol by distillation, and obtain the amino group Wax micropowder;
（4）取上述氨基蜡微粉，加入到溶胶分散液中，送入到70-75℃的恒温水浴中，保温搅拌100-130分钟，得水分散液；(4) Take the above-mentioned amino wax micropowder, add it to the sol dispersion, put it into a constant temperature water bath at 70-75°C, keep stirring for 100-130 minutes to obtain a water dispersion;
（5）取苯酚、37%的甲醛混合，搅拌均匀，送入到85-90℃的水浴中，加入氢氧化钠，保温搅拌3-4小时，加入甲基丙烯酸缩水甘油酯，降低温度为50-55℃，保温搅拌1-2小时，减压脱水，得改性填料；(5) Mix phenol and 37% formaldehyde, stir evenly, put it into a water bath at 85-90°C, add sodium hydroxide, keep stirring for 3-4 hours, add glycidyl methacrylate, reduce the temperature to 50 -55°C, keep stirring for 1-2 hours, decompress and dehydrate to obtain modified filler;
（6）取己内酰胺，加入到上述水分散液中，搅拌均匀，送入到反应釜中，通入氮气，调节反应釜温度为65-70℃，加入上述引发剂溶液，保温搅拌3-5小时，出料，得聚合物溶液；(6) Take caprolactam, add it to the above water dispersion, stir evenly, put it into the reaction kettle, feed nitrogen, adjust the temperature of the reaction kettle to 65-70°C, add the above initiator solution, keep stirring for 3-5 hours , discharging to obtain polymer solution;
（7）取上述改性填料，加入到聚合物溶液中，升高温度为150-160℃，保温搅拌80-100分钟，抽滤，将滤饼水洗，干燥，得预混料；(7) Take the above modified filler, add it to the polymer solution, raise the temperature to 150-160°C, keep stirring for 80-100 minutes, suction filter, wash the filter cake with water, and dry to obtain a premix;
（8）取上述预混料，与亚磷酸双酚A 酯、碳化硅纤维混合，搅拌均匀，送入到挤出机中，熔融挤出，冷却，即得。(8) Take the above premix, mix it with bisphenol A phosphite and silicon carbide fiber, stir evenly, send it into an extruder, melt extrude, and cool it.
步骤（7）所述的干燥温度为80-90℃，干燥时间为40-50分钟。The drying temperature in step (7) is 80-90° C., and the drying time is 40-50 minutes.
本发明的优点：Advantages of the present invention:
本发明首先以钛酸四丁酯为前驱体，二硫代水杨酸为促进剂，在水中水解，得到溶胶分散液，之后将聚酰胺蜡微粉采用硅烷偶联剂kh550处理，得到氨基蜡微粉，再与酸掺杂的氨基蜡微粉共混，进行酰胺化反应，得水分散液，再以苯酚、37%的甲醛为原料，进行环氧改性，得改性填料，然后以己内酰胺为单体，以水分散液为溶剂，进行聚合反应，将得到的聚合物溶液与环氧改性的填料共混反应，促进环氧交联，从而得到成品尼龙材料，本发明的材料具有很好的力学强度稳定性，且通过亚磷酸双酚A 酯、硬脂酸盐等共混，起到了很好的协同提高耐热稳定性的效果，本发明的材料，力学强度高，特别适合作为阀体材料，综合性能优异。In the present invention, tetrabutyl titanate is used as a precursor and dithiosalicylic acid is used as an accelerator, and hydrolyzed in water to obtain a sol dispersion, and then the polyamide wax micropowder is treated with a silane coupling agent kh550 to obtain amino wax micropowder , and then blended with acid-doped amino wax micropowder to carry out amidation reaction to obtain aqueous dispersion, and then use phenol and 37% formaldehyde as raw materials to carry out epoxy modification to obtain modified filler, and then use caprolactam as monolayer body, using the aqueous dispersion as a solvent to carry out a polymerization reaction, and the obtained polymer solution is mixed with an epoxy-modified filler to promote epoxy cross-linking, thereby obtaining a finished nylon material. The material of the present invention has good Mechanical strength stability, and through the blending of bisphenol A phosphite, stearate, etc., it has a good effect of synergistically improving heat resistance stability. The material of the present invention has high mechanical strength and is especially suitable as a valve body. material with excellent overall performance.
具体实施方式Detailed ways
实施例1Example 1
一种尼龙阀体材料，包括下述重量份的各原料：A nylon valve body material, comprising the following raw materials in parts by weight:
亚磷酸双酚A 酯4、己内酰胺160、引发剂5、苯酚36、37%的甲醛20、氢氧化钠1、碳化硅纤维3、钛酸四丁酯20、二硫代水杨酸1、聚酰胺蜡微粉4、硅烷偶联剂kh550 2、甲基丙烯酸缩水甘油酯4。Bisphenol A Phosphite 4, Caprolactam 160, Initiator 5, Phenol 36, 37% Formaldehyde 20, Sodium Hydroxide 1, Silicon Carbide Fiber 3, Tetrabutyl Titanate 20, Dithiosalicylic Acid 1, Poly Amide wax powder 4, silane coupling agent kh550 2, glycidyl methacrylate 4.
所述的引发剂为过氧化二异丙苯。The initiator is dicumyl peroxide.
一种尼龙阀体材料的制备方法，包括以下步骤：A preparation method of nylon valve body material, comprising the following steps:
（1）取引发剂，加入到其重量20倍的无水乙醇中，搅拌均匀，得引发剂溶液；(1) Take the initiator, add it to 20 times its weight in absolute ethanol, stir evenly, and obtain the initiator solution;
（2）取钛酸四丁酯、二硫代水杨酸混合，加入到混合料重量51倍的去离子水中，搅拌反应3小时，得溶胶分散液；(2) Mix tetrabutyl titanate and dithiosalicylic acid, add them to deionized water 51 times the weight of the mixture, and stir and react for 3 hours to obtain a sol dispersion;
（3）取聚酰胺蜡微粉、硅烷偶联剂kh550混合，加入到混合料重量7倍的无水乙醇中，在60℃下保温搅拌1小时，蒸馏除去乙醇，得氨基蜡微粉；(3) Mix the polyamide wax micropowder and the silane coupling agent kh550, add it into absolute ethanol with a weight of 7 times the mixture, keep stirring at 60°C for 1 hour, and remove the ethanol by distillation to obtain the amino wax micropowder;
（4）取上述氨基蜡微粉，加入到溶胶分散液中，送入到70℃的恒温水浴中，保温搅拌100分钟，得水分散液；(4) Take the above-mentioned amino wax micropowder, add it to the sol dispersion, put it into a constant temperature water bath at 70°C, keep stirring for 100 minutes to obtain a water dispersion;
（5）取苯酚、37%的甲醛混合，搅拌均匀，送入到85℃的水浴中，加入氢氧化钠，保温搅拌3小时，加入甲基丙烯酸缩水甘油酯，降低温度为50℃，保温搅拌1小时，减压脱水，得改性填料；(5) Mix phenol and 37% formaldehyde, stir evenly, put it into a water bath at 85°C, add sodium hydroxide, keep stirring for 3 hours, add glycidyl methacrylate, lower the temperature to 50°C, keep stirring 1 hour, decompression and dehydration to obtain modified filler;
（6）取己内酰胺，加入到上述水分散液中，搅拌均匀，送入到反应釜中，通入氮气，调节反应釜温度为65℃，加入上述引发剂溶液，保温搅拌3小时，出料，得聚合物溶液；(6) Take caprolactam, add it into the above-mentioned aqueous dispersion, stir evenly, put it into the reaction kettle, feed nitrogen, adjust the temperature of the reaction kettle to 65°C, add the above-mentioned initiator solution, keep stirring for 3 hours, and discharge, to obtain a polymer solution;
（7）取上述改性填料，加入到聚合物溶液中，升高温度为150℃，保温搅拌80分钟，抽滤，将滤饼水洗，干燥，得预混料；(7) Take the above modified filler, add it to the polymer solution, raise the temperature to 150°C, keep stirring for 80 minutes, suction filter, wash the filter cake with water, and dry to obtain a premix;
（8）取上述预混料，与亚磷酸双酚A 酯、碳化硅纤维混合，搅拌均匀，送入到挤出机中，熔融挤出，冷却，即得。(8) Take the above premix, mix it with bisphenol A phosphite and silicon carbide fiber, stir evenly, send it into an extruder, melt extrude, and cool it.
步骤（7）所述的干燥温度为80℃，干燥时间为40分钟。The drying temperature in step (7) is 80°C, and the drying time is 40 minutes.
实施例2Example 2
一种尼龙阀体材料，包括下述重量份的各原料：A nylon valve body material, comprising the following raw materials in parts by weight:
亚磷酸双酚A 酯7、己内酰胺200、引发剂7、苯酚40、37%的甲醛30、氢氧化钠2、碳化硅纤维4、钛酸四丁酯30、二硫代水杨酸2、聚酰胺蜡微粉6、硅烷偶联剂kh550 3、甲基丙烯酸缩水甘油酯7。Bisphenol A Phosphite 7, Caprolactam 200, Initiator 7, Phenol 40, 37% Formaldehyde 30, Sodium Hydroxide 2, Silicon Carbide Fiber 4, Tetrabutyl Titanate 30, Dithiosalicylic Acid 2, Polyurethane Amide wax powder 6, silane coupling agent kh550 3, glycidyl methacrylate 7.
所述的引发剂为过氧化二异丙苯。The initiator is dicumyl peroxide.
一种尼龙阀体材料的制备方法，包括以下步骤：A preparation method of nylon valve body material, comprising the following steps:
（1）取引发剂，加入到其重量30倍的无水乙醇中，搅拌均匀，得引发剂溶液；(1) Take the initiator, add it to 30 times its weight in absolute ethanol, stir evenly, and obtain the initiator solution;
（2）取钛酸四丁酯、二硫代水杨酸混合，加入到混合料重量60倍的去离子水中，搅拌反应5小时，得溶胶分散液；(2) Mixing tetrabutyl titanate and dithiosalicylic acid, adding them to deionized water 60 times the weight of the mixture, stirring and reacting for 5 hours to obtain a sol dispersion;
（3）取聚酰胺蜡微粉、硅烷偶联剂kh550混合，加入到混合料重量9倍的无水乙醇中，在65℃下保温搅拌2小时，蒸馏除去乙醇，得氨基蜡微粉；(3) Mix the polyamide wax micropowder and the silane coupling agent kh550, add it to anhydrous ethanol that is 9 times the weight of the mixture, keep stirring at 65°C for 2 hours, and remove the ethanol by distillation to obtain the amino wax micropowder;
（4）取上述氨基蜡微粉，加入到溶胶分散液中，送入到75℃的恒温水浴中，保温搅拌130分钟，得水分散液；(4) Take the above-mentioned amino wax micropowder, add it to the sol dispersion, put it into a constant temperature water bath at 75°C, keep stirring for 130 minutes to obtain a water dispersion;
（5）取苯酚、37%的甲醛混合，搅拌均匀，送入到85-90℃的水浴中，加入氢氧化钠，保温搅拌4小时，加入甲基丙烯酸缩水甘油酯，降低温度为55℃，保温搅拌2小时，减压脱水，得改性填料；(5) Mix phenol and 37% formaldehyde, stir evenly, put it into a water bath at 85-90°C, add sodium hydroxide, keep stirring for 4 hours, add glycidyl methacrylate, lower the temperature to 55°C, Insulation and stirring for 2 hours, decompression and dehydration to obtain modified filler;
（6）取己内酰胺，加入到上述水分散液中，搅拌均匀，送入到反应釜中，通入氮气，调节反应釜温度为70℃，加入上述引发剂溶液，保温搅拌5小时，出料，得聚合物溶液；(6) Take caprolactam, add it into the above-mentioned aqueous dispersion, stir evenly, put it into the reaction kettle, feed nitrogen, adjust the temperature of the reaction kettle to 70°C, add the above-mentioned initiator solution, keep stirring for 5 hours, and discharge, to obtain a polymer solution;
（7）取上述改性填料，加入到聚合物溶液中，升高温度为160℃，保温搅拌100分钟，抽滤，将滤饼水洗，干燥，得预混料；(7) Take the above modified filler, add it to the polymer solution, raise the temperature to 160°C, keep stirring for 100 minutes, suction filter, wash the filter cake with water, and dry to obtain a premix;
（8）取上述预混料，与亚磷酸双酚A 酯、碳化硅纤维混合，搅拌均匀，送入到挤出机中，熔融挤出，冷却，即得。(8) Take the above premix, mix it with bisphenol A phosphite and silicon carbide fiber, stir evenly, send it into an extruder, melt extrude, and cool it.
步骤（7）所述的干燥温度为90℃，干燥时间为50分钟。The drying temperature in step (7) is 90°C, and the drying time is 50 minutes.
性能测试：Performance Testing:
本发明实施例1的尼龙阀体材料：The nylon valve body material of Embodiment 1 of the present invention:
拉伸性能：按 ISO527-2 进行测试，拉伸速度为 5mm/min，测试温度为 23℃，测得；Tensile properties: tested according to ISO527-2, the tensile speed is 5mm/min, and the test temperature is 23℃;
本发明实施例1的尼龙阀体材料的拉伸强度为183.6Mpa；The tensile strength of the nylon valve body material of Example 1 of the present invention is 183.6Mpa;
本发明实施例2的尼龙阀体材料的拉伸强度为189.4Mpa。The tensile strength of the nylon valve body material of Example 2 of the present invention is 189.4Mpa.
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| CN201910679431.8ACN110305472A (en) | 2019-07-26 | 2019-07-26 | A kind of nylon valve body material and preparation method thereof |
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| CN201910679431.8ACN110305472A (en) | 2019-07-26 | 2019-07-26 | A kind of nylon valve body material and preparation method thereof |
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|---|---|---|---|---|
| CN112094619A (en)* | 2019-12-13 | 2020-12-18 | 上海铂淳胶粘技术有限公司 | Fiber composite hot melt adhesive and preparation method thereof |
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102732012A (en)* | 2012-06-15 | 2012-10-17 | 苏州宇度医疗器械有限责任公司 | Silicon carbide reinforced nylon composite material |
| CN102732016A (en)* | 2012-06-15 | 2012-10-17 | 苏州宇度医疗器械有限责任公司 | Preparation method for silicon carbide reinforced nylon composite |
| CN108517115A (en)* | 2018-03-20 | 2018-09-11 | 繁昌县聚恒智能装备有限公司 | A kind of anti-oxidant nylon material and preparation method thereof |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732012A (en)* | 2012-06-15 | 2012-10-17 | 苏州宇度医疗器械有限责任公司 | Silicon carbide reinforced nylon composite material |
| CN102732016A (en)* | 2012-06-15 | 2012-10-17 | 苏州宇度医疗器械有限责任公司 | Preparation method for silicon carbide reinforced nylon composite |
| CN108517115A (en)* | 2018-03-20 | 2018-09-11 | 繁昌县聚恒智能装备有限公司 | A kind of anti-oxidant nylon material and preparation method thereof |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112094619A (en)* | 2019-12-13 | 2020-12-18 | 上海铂淳胶粘技术有限公司 | Fiber composite hot melt adhesive and preparation method thereof |
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| RJ01 | Rejection of invention patent application after publication | Application publication date:20191008 | |
| RJ01 | Rejection of invention patent application after publication |