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CN113277491A - By using CO2Method for preparing yak dung-based hydrothermal charcoal - Google Patents

By using CO2Method for preparing yak dung-based hydrothermal charcoal
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CN113277491A
CN113277491ACN202110549988.7ACN202110549988ACN113277491ACN 113277491 ACN113277491 ACN 113277491ACN 202110549988 ACN202110549988 ACN 202110549988ACN 113277491 ACN113277491 ACN 113277491A
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yak
dung
hydrothermal
yak dung
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陈冠益
田静楠
钟磊
宋英今
李金磊
陈红云
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Tianjin University
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Abstract

The invention discloses a method for utilizing CO2The method for preparing the yak-dung-based hydrothermal charcoal comprises the following steps: providing dried and crushed yak dung; placing yak dung and water in CO2Carrying out hydrothermal reaction at a preset temperature in a hydrothermal reaction kettle under the atmosphere to obtain a solid product; and washing and drying the solid product to obtain the yak dung-based hydrothermal carbon. The invention also provides the yak excrement-based hydrothermal carbon obtained by the method and application of the yak excrement-based hydrothermal carbon in soil improvement.

Description

By using CO2Method for preparing yak dung-based hydrothermal charcoal
Technical Field
The invention relates to the technical field of fertilizer preparation, in particular to a method for utilizing CO2A method for preparing yak dung-based hydrothermal charcoal.
Background
Yak dung is one of the most abundant biomass in Tibet, and the annual output is as high as 1 thousand and ten thousand tons. Yak dung is selected as fuel by herdsmen in Qinghai-Tibet plateau areas. However, smoke generated in the combustion process of yak dung can cause serious indoor air pollution, the generated particulate matters (PM 2.5) can cause adverse effects such as cardiovascular diseases, respiratory system diseases and cancers on a human body, and in addition, the particulate matters released by combustion also have serious effects on the atmospheric environment. Therefore, the problem of resource utilization of yak dung needs to be solved urgently.
Yak dung is a substance rich in carbon and nitrogen, and contains a large amount of trace elements such as Zn, Fe and the like required by plants. More importantly, the heavy metal content of the yak excrement hydrothermal carbon is lower than that of the hydrothermal carbon prepared from other materials. Therefore, yak excrement is a promising high-quality raw material for agricultural hydrothermal carbon production, and yak excrement biomass carbonization treatment is gradually accepted and favored by people as a novel environment-friendly treatment mode.
After entering the soil, the hydrothermal carbon has a remarkable improvement effect on the basic physicochemical properties of the soil, can supplement nutrients in the soil, and can effectively preserve nutrients and water so as to improve the fertility of the soil. However, the hydrothermal carbon has a relatively undeveloped pore structure due to a relatively low specific surface area, and after the hydrothermal carbon is applied to soil as a fertilizer, a large amount of nitrogen is easily released in the initial stage, so that a large amount of nitrogen is lost, which limits the application of the hydrothermal carbon in soil fertilizers and agricultural fields, and the slow release effect can be achieved by further modification treatment.
Therefore, the improvement of the specific surface area and the stability of the hydrothermal carbon has positive significance for the application of the hydrothermal carbon in the fields of soil fertilizers and agriculture.
Disclosure of Invention
In view of the above, the present invention provides a method for improving the specific surface area and stability of hydrothermal carbon by using CO2A method for preparing yak dung-based hydrothermal charcoal.
The invention provides a method for utilizing CO2The method for preparing the yak-dung-based hydrothermal charcoal comprises the following steps: lifting deviceProviding dried and crushed yak dung; placing yak dung and water in CO2Carrying out hydrothermal reaction at a preset temperature in a hydrothermal reaction kettle under the atmosphere to obtain a solid product; and washing and drying the solid product to obtain the yak dung-based hydrothermal carbon.
In some embodiments, the mass ratio of the yak dung to the water is 1 (3-10).
In some embodiments, the mass ratio of yak dung to water is 1: 5.
In some embodiments, the hydrothermal reaction is carried out at a temperature of 200-300 ℃ for 1-2 h.
In some embodiments, the hydrothermal reaction is carried out at a reaction temperature of 250 ℃ for a reaction time of 2 h.
In some embodiments, the hydrothermal reaction is carried out under stirring of a stirring shaft, and the rotation speed of the stirring shaft is 50-100 r.min-1
In some embodiments, providing the air dried, comminuted yak dung comprises: naturally air drying yak dung, drying in oven, pulverizing, and sieving.
In some embodiments, washing and drying the solid product comprises: washing the solid product with absolute ethyl alcohol and water for 2-3 times respectively; and (3) drying the washed solid product in an oven at 90-105 ℃.
The invention also provides the yak excrement-based hydrothermal charcoal obtained by the method.
The invention also provides an application of the yak dung-based hydrothermal carbon in soil improvement.
The invention utilizes CO2Carrying out hydrothermal carbonization treatment on yak excrement to obtain yak excrement-based hydrothermal carbon. The yak excrement-based hydrothermal carbon prepared by the method has high specific surface area and stability.
The yak dung-based hydrothermal carbon prepared by the method is applied to soil improvement, can play a good role in providing soil fertility and nutrient utilization efficiency, and can realize high-efficiency utilization of yak dung.
Drawings
FIG. 1 is a schematic diagram of a method for utilizing CO according to an embodiment of the present invention2A flow chart of a method for preparing yak dung-based hydrothermal carbon;
fig. 2 is a Fourier infrared spectrum analysis of yak dung and yak dung-based hydrothermal carbon provided by the embodiment of the invention.
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
The invention provides a method for utilizing CO2The method for preparing the yak-dung-based hydrothermal charcoal comprises the following steps: providing dried and crushed yak dung; placing yak dung and water in CO2Carrying out hydrothermal reaction at a preset temperature in a hydrothermal reaction kettle under the atmosphere to obtain a solid product; and washing and drying the solid product to obtain the yak dung-based hydrothermal carbon.
FIG. 1 is a schematic diagram of a method for utilizing CO according to an embodiment of the present invention2A flow chart of a method for preparing yak dung-based hydrothermal charcoal. As shown in fig. 1, the method includes operations S101 to S103.
In operation S101, air-dried and pulverized yak dung is provided.
According to the embodiment of the invention, the yak dung which is air-dried and crushed comprises the following components: naturally air-drying yak dung, drying in an oven at 90-105 ℃ for 3-6 h, crushing and sieving.
According to an embodiment of the invention, the post-comminution sieving comprises: after being crushed, the mixture is sieved by a 40-80 mesh sieve, for example, a 40 mesh sieve, a 60 mesh sieve and an 80 mesh sieve.
In operation S102, yak dung and water are placed in CO2And carrying out hydrothermal reaction at a preset temperature in a hydrothermal reaction kettle under the atmosphere to obtain a solid product.
According to the embodiment of the invention, the mass ratio of the yak dung to the water is 1 (3-10), for example, the mass ratio can be 1:3, 1:5, 1:7, 1:9 and 1: 10.
According to the embodiment of the present invention, the reaction temperature of the hydrothermal reaction is 200 to 300 ℃, for example, 200 ℃, 225 ℃, 250 ℃, 275 ℃, 300 ℃; the reaction time is 1 to 2 hours, for example, 1 hour, 1.5 hours, 2 hours.
According to the embodiment of the present invention, the reaction temperature of the hydrothermal reaction may be 250 ℃, and the reaction time may be 2 hours.
According to the embodiment of the invention, practical experiments prove that when the reaction temperature of the hydrothermal reaction is 250 ℃ and the reaction time is 2 hours, the specific surface area of the prepared yak-dung-based hydrothermal carbon is larger.
According to the embodiment of the invention, the hydrothermal reaction is carried out under the stirring of the stirring shaft, and the rotating speed of the stirring shaft is 50-100 r.min-1. For example, it may be 50 r.min-1、60r·min-1、80r·min-1、90r·min-1、100r·min-1
In operation S103, the solid product is washed and dried to obtain yak-dung-based hydrothermal charcoal.
According to an embodiment of the present invention, the washing and drying of the solid product comprises: washing the solid product with absolute ethyl alcohol and water for 2-3 times respectively; and (3) drying the washed solid product in an oven at 90-105 ℃.
The invention also provides the yak excrement-based hydrothermal charcoal obtained by the method.
The invention also provides an application of the yak dung-based hydrothermal carbon in soil improvement.
To more clearly illustrate the features of the practice of the present invention, a CO-utilizing process will be incorporated2The invention is further illustrated by the examples of the process for preparing yak-dung-based hydrothermal charcoal.
Example 1
Naturally air drying yak dung, drying in oven, pulverizing, and sieving. Respectively weighing 10g of yak dung and 50mL of water in CO2In the hydrothermal reaction kettle under the atmosphere, the rotating speed of the stirring shaft is set to be 100 r.min-1The reaction temperature of the hydrothermal reaction is 200 ℃, and the reaction time is 1 h. After the reaction is finished, a solid product is obtained. And washing the obtained solid product with 250mL of anhydrous ethanol and 250mL of water for 2-3 times respectively, and drying the solid product at 105 ℃ for 24h to obtain the yak-dung-based hydrothermal charcoal (marked as C2001).
By using N2AsComparative experiment, the atmosphere of the above reaction was changed to N2Obtained in N2Preparing the obtained yak dung-based hydrothermal charcoal (marked as N2001) in the atmosphere; wherein "C" represents CO2Atmosphere "N" stands for N2Atmosphere, "200" represents the reaction temperature of the hydrothermal reaction, and "1" represents the reaction time period of the hydrothermal reaction.
Respectively in the presence of CO2Under an atmosphere and in N2And testing the specific surface area of the yak dung-based hydrothermal carbon prepared in the atmosphere. The test results show that in CO2The specific surface area of the yak-dung-based hydrothermal charcoal (C2001) prepared in the atmosphere is 15.27m2·g-1(ii) a In N2The specific surface area of the yak-dung-based hydrothermal charcoal (N2001) prepared in the atmosphere is 10.25m2·g-1
Example 2
A yak dung-based hydrothermal carbon was prepared by a method similar to that of example 1, except that the reaction temperature of the hydrothermal reaction was set to 200 ℃ and the reaction time was set to 2 hours, to obtain a yak dung-based hydrothermal carbon (labeled as C2002).
By using N2As a comparative test, the atmosphere of the above reaction was changed to N2To obtain N2The obtained yak dung-based hydrothermal charcoal (marked as N2002) is prepared under the atmosphere.
Respectively in the presence of CO2Under an atmosphere and in N2And testing the specific surface area of the yak dung-based hydrothermal carbon prepared in the atmosphere. The test results show that in CO2The specific surface area of the yak-dung-based hydrothermal charcoal (C2002) prepared in the atmosphere is 15.27m2·g-1(ii) a In N2The specific surface area of the yak-dung-based hydrothermal charcoal (N2002) prepared in the atmosphere is 10.25m2·g-1
Table 1 shows the reaction temperature of the hydrothermal reaction at 200 ℃ in CO2And N2And comparing the specific surface areas of the yak excrement-based hydrothermal carbon prepared in the atmosphere.
TABLE 1
Figure BDA0003075048580000051
Example 3
A yak dung-based hydrothermal carbon was prepared by a method similar to that of example 1, except that the reaction temperature of the hydrothermal reaction was set to 250 ℃ and the reaction time was set to 1 hour, to obtain a yak dung-based hydrothermal carbon (labeled as C2501).
By using N2As a comparative test, the atmosphere of the above reaction was changed to N2To obtain N2The obtained yak dung-based hydrothermal charcoal (marked as N2501) is prepared under the atmosphere.
Respectively in the presence of CO2Under an atmosphere and in N2And testing the specific surface area of the yak dung-based hydrothermal carbon prepared in the atmosphere. The test results show that in CO2The specific surface area of the yak dung-based hydrothermal charcoal (C2501) prepared in the atmosphere is 58.25m2·g-1(ii) a In N2The specific surface area of the yak dung-based hydrothermal charcoal (N2501) prepared in the atmosphere is 44.24m2·g-1
Example 4
A yak dung-based hydrothermal carbon was prepared by a method similar to that of example 1, except that the reaction temperature of the hydrothermal reaction was set to 250 ℃ and the reaction time was set to 2 hours, to obtain a yak dung-based hydrothermal carbon (labeled as C2502).
By using N2As a comparative test, the atmosphere of the above reaction was changed to N2To obtain N2The obtained yak dung-based hydrothermal charcoal (marked as N2502) is prepared under the atmosphere.
Respectively in the presence of CO2Under an atmosphere and in N2And testing the specific surface area of the yak dung-based hydrothermal carbon prepared in the atmosphere. The test results show that in CO2The specific surface area of the yak-dung-based hydrothermal charcoal (C2502) prepared in the atmosphere is 60.13m2·g-1(ii) a In N2The specific surface area of the yak dung-based hydrothermal charcoal (N2502) prepared in the atmosphere is 43.24m2·g-1. Compared with in N2Preparing yak dung-based hydrothermal charcoal (N2502) in CO atmosphere2The specific surface area of the yak dung-based hydrothermal charcoal (C2502) prepared in the atmosphere is increased39.06%。
Table 2 shows the reaction temperature of the hydrothermal reaction at 250 ℃ in CO2And N2And comparing the specific surface areas of the yak excrement-based hydrothermal carbon prepared in the atmosphere.
TABLE 2
Figure BDA0003075048580000061
Example 5
A yak dung-based hydrothermal carbon is prepared by a method similar to that in example 1, except that the reaction temperature of the hydrothermal reaction is set to 300 ℃, and the reaction time is set to 1h, so that the yak dung-based hydrothermal carbon (marked as C3001) is obtained.
By using N2As a comparative test, the atmosphere of the above reaction was changed to N2To obtain N2The obtained yak dung-based hydrothermal charcoal (marked as N3001) is prepared under the atmosphere.
Respectively in the presence of CO2Under an atmosphere and in N2And testing the specific surface area of the yak dung-based hydrothermal carbon prepared in the atmosphere. The test results show that in CO2The specific surface area of the yak dung-based hydrothermal carbon (C3001) prepared in the atmosphere is 3.62m2·g-1(ii) a In N2The specific surface area of the yak dung-based hydrothermal carbon (N3001) prepared in the atmosphere is 2.14m2·g-1
Example 6
A yak dung-based hydrothermal carbon is prepared by a method similar to that in example 1, except that the reaction temperature of the hydrothermal reaction is set to 300 ℃, and the reaction time is set to 2 hours, so that the yak dung-based hydrothermal carbon (marked as C3002) is obtained.
By using N2As a comparative test, the atmosphere of the above reaction was changed to N2To obtain N2Preparing the obtained yak dung-based hydrothermal charcoal (marked as N3002) in the atmosphere.
Respectively in the presence of CO2Under an atmosphere and in N2And testing the specific surface area of the yak dung-based hydrothermal carbon prepared in the atmosphere. The test results show that in CO2Under atmosphereThe specific surface area of the obtained yak-dung-based hydrothermal charcoal (C3002) is 2.54m2·g-1(ii) a In N2The specific surface area of the yak dung-based hydrothermal carbon (N3002) prepared in the atmosphere is 1.52m2·g-1
Table 3 shows the reaction temperature of the hydrothermal reaction at 300 ℃ in CO2And N2And comparing the specific surface areas of the yak excrement-based hydrothermal carbon prepared in the atmosphere.
TABLE 3
Figure BDA0003075048580000071
Fig. 2 is a Fourier infrared spectrum analysis of yak dung and yak dung-based hydrothermal carbon provided by the embodiment of the invention. As shown in FIG. 2, in CO2The infrared spectrogram of functional group of yak dung-based hydrothermal carbon prepared under atmosphere is shown at wavenumber of 865cm-1The yak excrement-based hydrothermal charcoal contains higher aromatic substances, and has higher stability.
Embodiments of the invention utilize CO2Carrying out hydrothermal carbonization treatment on yak excrement to obtain yak excrement-based hydrothermal carbon. The yak excrement-based hydrothermal carbon prepared by the embodiment of the invention has higher specific surface area and stability. When the reaction temperature of the hydrothermal reaction is 250 ℃ and the reaction time is 2 hours, the specific surface area of the prepared yak-dung-based hydrothermal carbon reaches 60.13m2·g-1Relative to in N2The specific surface area of the yak dung-based hydrothermal carbon prepared in the atmosphere is obviously improved.
The yak excrement-based hydrothermal carbon prepared by the embodiment of the invention is applied to soil improvement, can play a good role in improving soil fertility and nutrient utilization efficiency, and can realize high-efficiency utilization of yak excrement.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

Translated fromChinese
1.一种利用CO2制备牦牛粪基水热炭的方法,其特征在于,包括:1. a method of utilizing CO2 to prepare yak dung-based hydrothermal carbon, is characterized in that, comprising:提供风干、粉碎后的牦牛粪;Provide air-dried and crushed yak dung;将所述牦牛粪与水置于CO2气氛下的水热反应釜中,在预设温度下进行水热反应,得到固体产物;The yak dung and water are placed in a hydrothermal reactor underCO atmosphere, and a hydrothermal reaction is carried out at a preset temperature to obtain a solid product;将所述固体产物洗涤、干燥后,得到牦牛粪基水热炭。After washing and drying the solid product, yak dung-based hydrothermal charcoal is obtained.2.根据权利要求1所述的方法,其特征在于,所述牦牛粪与所述水的质量比为1:(3~10)。2. method according to claim 1, is characterized in that, the mass ratio of described yak dung and described water is 1:(3~10).3.根据权利要求1所述的方法,其特征在于,所述牦牛粪与所述水的质量比为1:5。3. method according to claim 1, is characterized in that, the mass ratio of described yak dung and described water is 1:5.4.根据权利要求1所述的方法,其特征在于,所述水热反应的反应温度为200~300℃,反应时长为1~2h。4 . The method according to claim 1 , wherein the reaction temperature of the hydrothermal reaction is 200-300° C., and the reaction time is 1-2 h. 5 .5.根据权利要求4所述的方法,其特征在于,所述水热反应的反应温度为250℃,反应时长为2h。5 . The method according to claim 4 , wherein the reaction temperature of the hydrothermal reaction is 250° C., and the reaction time is 2 h. 6 .6.根据权利要求1所述的方法,其特征在于,所述水热反应在搅拌轴搅拌下进行,所述搅拌轴的转速为50~100r·min-16 . The method according to claim 1 , wherein the hydrothermal reaction is carried out under stirring by a stirring shaft, and the rotational speed of the stirring shaft is 50-100 r·min−1 . 7 .7.根据权利要求1所述的方法,其特征在于,所述提供风干、粉碎后的牦牛粪包括:将所述牦牛粪在自然状态下风干后,置于烘箱干燥,粉碎后过筛。7. The method according to claim 1, wherein the providing air-dried and pulverized yak dung comprises: after the yak dung is air-dried in a natural state, placed in an oven to dry, and sieved after pulverization.8.根据权利要求1所述的方法,其特征在于,所述将所述固体产物洗涤、干燥包括:8. The method according to claim 1, wherein the washing and drying of the solid product comprises:分别用无水乙醇和水洗涤所述固体产物2~3次;Wash the solid product 2-3 times with absolute ethanol and water respectively;将洗涤后的固体产物置于90~105℃烘箱烘干。The washed solid product is placed in an oven at 90-105°C for drying.9.一种利用权利要求1~8中任一项所述的方法得到的牦牛粪基水热炭。9. A yak dung-based hydrothermal charcoal obtained by the method according to any one of claims 1 to 8.10.一种利用权利要求9所述的牦牛粪基水热炭在土壤改良中的应用。10. An application of the yak dung-based hydrothermal charcoal according to claim 9 in soil improvement.
CN202110549988.7A2021-05-202021-05-20By using CO2Method for preparing yak dung-based hydrothermal charcoalPendingCN113277491A (en)

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