CN115215332B - Preparation method of graphene synergistic sol for improving soil quality - Google Patents
Preparation method of graphene synergistic sol for improving soil quality Download PDFInfo
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- CN115215332B CN115215332B CN202210848115.0A CN202210848115A CN115215332B CN 115215332 B CN115215332 B CN 115215332B CN 202210848115 A CN202210848115 A CN 202210848115A CN 115215332 B CN115215332 B CN 115215332B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 73
- 239000002689 soil Substances 0.000 title claims abstract description 44
- 230000002195 synergetic effect Effects 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 26
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 19
- 239000010439 graphite Substances 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 239000002270 dispersing agent Substances 0.000 claims abstract description 15
- 238000009830 intercalation Methods 0.000 claims abstract description 14
- 230000002687 intercalation Effects 0.000 claims abstract description 14
- 239000006185 dispersion Substances 0.000 claims abstract description 13
- 239000000440 bentonite Substances 0.000 claims abstract description 10
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 10
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000002791 soaking Methods 0.000 claims abstract description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 18
- 239000012279 sodium borohydride Substances 0.000 claims description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- XNLICIUVMPYHGG-UHFFFAOYSA-N pentan-2-one Chemical compound CCCC(C)=O XNLICIUVMPYHGG-UHFFFAOYSA-N 0.000 claims description 12
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 10
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 8
- 239000000194 fatty acid Substances 0.000 claims description 8
- 229930195729 fatty acid Natural products 0.000 claims description 8
- 150000004665 fatty acids Chemical class 0.000 claims description 8
- 229920002401 polyacrylamide Polymers 0.000 claims description 8
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 6
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- KVXNKFYSHAUJIA-UHFFFAOYSA-N acetic acid;ethoxyethane Chemical compound CC(O)=O.CCOCC KVXNKFYSHAUJIA-UHFFFAOYSA-N 0.000 claims description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 235000015097 nutrients Nutrition 0.000 abstract description 9
- 230000007774 longterm Effects 0.000 abstract description 5
- 238000001179 sorption measurement Methods 0.000 abstract description 5
- 238000004321 preservation Methods 0.000 abstract description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 8
- 239000003337 fertilizer Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 229920000151 polyglycol Polymers 0.000 description 4
- 239000010695 polyglycol Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000020477 pH reduction Effects 0.000 description 2
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical compound CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000012217 deletion Methods 0.000 description 1
- 230000037430 deletion Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- -1 fire-run Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/02—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2101/00—Agricultural use
Abstract
A preparation method of graphene synergistic sol for improving soil quality comprises the following steps: step one, adding flake graphite into a mixed acid solution, and soaking for 3-4 hours; adding 5-8g/L of intercalation agent into the mixed acid solution, reacting for 4-6 hours at 45-55 ℃, then washing until the pH is between 4.6-5.3, dispersing for 1-2 hours by using ultrasonic wave, and drying at 100 ℃ to obtain graphene oxide; thirdly, placing graphene oxide in a reducing solution, and performing reaction treatment for 2-3 hours to obtain graphene; adding 300-400g/L graphene into the dispersion solution, adding 2-3g/L dispersing agent and 8-12g/L organic bentonite, and performing ultrasonic treatment for 30-40min to obtain graphene synergistic sol; the graphene synergistic sol prepared by limiting the preparation process of the graphene synergistic sol has strong adsorption capacity, so that the long-term preservation of nutrients by soil is greatly enhanced, and the volatilization and deep leakage loss on the ground of the nutrients are effectively controlled.
Description
Technical Field
The application belongs to the field of soil improvement preparations, and particularly relates to a preparation method of graphene synergistic sol for improving soil quality.
Background
At present, soil is barren in many places in China, so that crops cannot be planted in the land, and the land is wasted in a large area. The comprehensive characterization of the soil environment and the physical, chemical and biological property degradation of the soil shows that the content of organic matters is reduced, the nutrient elements are deficient, the soil structure is damaged, the soil is eroded, the soil layer becomes thin, the soil is hardened, and the soil is easy to be acidified, alkalized, desertified and the like. In these characterizations, the decrease in organic content can be an important indicator of soil degradation, which is associated with many properties of the soil. For example, the ph of soil is critical to plant growth, most crops thrive in neutral or slightly acidic soil, but in order to pursue yield, small deletions of conventional agricultural application of lime, fire-run, fertilizer application, etc. are accumulated chronically, causing imbalance in the soil rational structure of cultivated land. Because the planting technology of the fertilizer is excessively dependent, the long-term large-scale application of the fertilizer is one of the important reasons for the hardening and acidification of the soil, and is also a culprit for the hardening and acidification of the soil in China.
However, the existing soil restoration agent can only solve one soil impoverishment problem, and the soil impoverishment is often caused by a plurality of factors, so that the soil restoration agent in the prior art is slow in curative effect and cannot radically solve the soil impoverishment problem.
Disclosure of Invention
The application aims to overcome the defects of the prior art and provides a preparation method of graphene sol for improving soil quality
The application adopts the following technical scheme:
a preparation method of graphene synergistic sol for improving soil quality comprises the following steps:
step one, adding flake graphite into a mixed acid solution, and soaking for 3-4 hours;
adding 5-8g/L of intercalation agent into the mixed acid solution, reacting for 4-6 hours at 45-55 ℃, then washing until the pH is between 4.6-5.3, dispersing for 1-2 hours by using ultrasonic wave, and drying at 100 ℃ to obtain graphene oxide;
thirdly, placing graphene oxide in a reducing solution, and performing reaction treatment for 2-3 hours to obtain graphene;
adding 300-400g/L graphene into the dispersion solution, adding 2-3g/L dispersing agent and 8-12g/L organic bentonite, and performing ultrasonic treatment for 30-40min to obtain graphene synergistic sol;
the intercalation agent consists of phosphoric anhydride, acetic acid and sodium bicarbonate according to the mass ratio of 1:0.4-0.6:2-3;
the dispersing agent consists of fatty acid polyethylene glycol ether and polyacrylamide according to the mass ratio of 1:0.56-0.65.
Preferably, the dispersion solution consists of acetone, methyl propyl ketone and ethylene glycol diethyl ether acetate according to the volume ratio of 1:0.65-0.72:0.3-0.4.
Preferably, the reducing solution is a sodium borohydride solution.
Preferably, the sodium borohydride solution is prepared by adding sodium borohydride and water in a ratio of 2-3g to 65-70ml.
Preferably, the addition ratio of the mixed acid solution to the crystalline flake graphite is 8-10 ml/0.3-0.5 g.
Preferably, the mixed acid consists of nitric acid solution and hydrochloric acid solution according to the volume ratio of 1:12-15.
Preferably, the mass concentration of the nitric acid solution is 62-65%, and the mass concentration of the hydrochloric acid solution is 35-40%.
Preferably, the addition ratio of the reducing solution to the graphite oxide is 10-12 ml/0.2-0.3 g.
As can be seen from the above description of the present application, compared with the prior art, the present application has the following beneficial effects:
according to the preparation method, the preparation process of the graphene synergistic sol is limited, so that the prepared graphene synergistic sol has strong adsorption capacity, and the long-term preservation of nutrients by soil is greatly enhanced, so that the volatilization and deep seepage loss on the soil of the nutrients are effectively controlled, the electrochemical property of the soil can be improved, the fertilizer utilization rate is improved, and the fertilizer saving and synergy effects are realized; when the graphene is dispersed, fatty acid polyethylene glycol ether and polyacrylamide are added as dispersing agents, so that the graphene is uniformly dispersed in a dispersing solution; the organic bentonite is added, so that the graphene synergistic sol can be formed stably, and the trend of automatically condensing and enlarging the formed graphene synergistic sol can be effectively slowed down, so that the storage time of the graphene synergistic sol is prolonged;
the composition and the proportion of the intercalation agent are limited to obtain graphene oxide with less ash, high purity and large expansion capacity, so that the prepared graphene has high purity and strong adsorption capacity, the adsorption capacity of finally prepared graphene sol is further improved, the long-term preservation of soil to nutrients is greatly enhanced, and the volatilization and deep leakage loss of nutrients on the ground are effectively controlled.
Detailed Description
The application is further described below by means of specific embodiments.
A preparation method of graphene synergistic sol for improving soil quality comprises the following steps:
step one, adding flake graphite into a mixed acid solution, and soaking for 3-4 hours, wherein the adding ratio of the mixed acid solution to the flake graphite is 8-10ml, and the adding ratio is 0.3-0.5g;
adding 5-8g/L of intercalation agent into the mixed acid solution, reacting for 4-6 hours at 45-55 ℃, then washing until the pH is between 4.6-5.3, dispersing for 1-2 hours by using ultrasonic wave, and drying at 100 ℃ to obtain graphene oxide;
step three, placing graphene oxide into a reducing solution, and carrying out reaction treatment for 2-3 hours to obtain graphene, wherein the adding ratio of the reducing solution to the graphite oxide is 10-12ml, and the ratio of the reducing solution to the graphite oxide is 0.2-0.3g;
and step four, adding 300-400g/L graphene into the dispersion solution, adding 2-3g/L dispersing agent and 8-12g/L organic bentonite, and carrying out ultrasonic treatment for 30-40min to obtain the graphene synergistic sol.
Wherein the intercalation agent consists of phosphoric anhydride, acetic acid and sodium bicarbonate according to the mass ratio of 1:0.4-0.6:2-3;
the dispersing agent consists of fatty acid polyglycol ether and polyacrylamide in the mass ratio of 1 to 0.56-0.65.
The dispersion solution consists of acetone, methyl propyl ketone and glycol diethyl ether acetate according to the volume ratio of 1:0.65-0.72:0.3-0.4.
The reducing solution is sodium borohydride solution, and the adding ratio of sodium borohydride to water of the sodium borohydride solution is 2-3 g/65-70 ml.
The mixed acid consists of nitric acid solution and hydrochloric acid solution according to the volume ratio of 1:12-15, wherein the mass concentration of the nitric acid solution is 62-65%, and the mass concentration of the hydrochloric acid solution is 35-40%.
Example 1
A preparation method of graphene synergistic sol for improving soil quality comprises the following steps:
step one, adding flake graphite into a mixed acid solution, and soaking for 3 hours, wherein the adding ratio of the mixed acid solution to the flake graphite is 8ml to 0.5g;
adding 5g/L of intercalation agent into the mixed acid solution, reacting at 45 ℃ for 6 hours, washing until the pH is between 4.6 and 5.3, dispersing for 1 hour by using ultrasonic waves, and drying at 100 ℃ to obtain graphene oxide;
step three, placing graphene oxide into a reducing solution, and carrying out reaction treatment for 3 hours to obtain graphene, wherein the adding ratio of the reducing solution to the graphite oxide is 10 ml/0.2 g;
and step four, adding 300g/L graphene into the dispersion solution, adding 2g/L dispersing agent and 12g/L organic bentonite, and carrying out ultrasonic treatment for 40min to obtain the graphene synergistic sol.
Wherein the intercalation agent consists of phosphoric anhydride, acetic acid and sodium bicarbonate according to the mass ratio of 1:0.4:2;
the dispersing agent consists of fatty acid polyglycol ether and polyacrylamide in the mass ratio of 1 to 0.65.
The dispersion solution consists of acetone, methyl propyl ketone and glycol diethyl ether acetate according to the volume ratio of 1:0.65:0.4.
The reducing solution is sodium borohydride solution, and the adding ratio of sodium borohydride to water of the sodium borohydride solution is 2 g/65 ml.
The mixed acid consists of nitric acid solution and hydrochloric acid solution according to the volume ratio of 1:12, wherein the mass concentration of the nitric acid solution is 62%, and the mass concentration of the hydrochloric acid solution is 40%.
Example 2
A preparation method of graphene synergistic sol for improving soil quality comprises the following steps:
step one, adding flake graphite into a mixed acid solution, and soaking for 4 hours, wherein the adding ratio of the mixed acid solution to the flake graphite is 10ml to 0.3g;
adding 8g/L of intercalation agent into the mixed acid solution, reacting at 55 ℃ for 4 hours, washing until the pH is between 4.6 and 5.3, dispersing for 2 hours by using ultrasonic waves, and drying at 100 ℃ to obtain graphene oxide;
step three, placing graphene oxide into a reducing solution, and carrying out reaction treatment for 2 hours to obtain graphene, wherein the adding ratio of the reducing solution to the graphite oxide is 12ml to 0.3g;
and step four, adding 400g/L graphene into the dispersion solution, adding 3g/L dispersing agent and 8g/L organic bentonite, and carrying out ultrasonic treatment for 30min to obtain the graphene synergistic sol.
Wherein the intercalation agent consists of phosphoric anhydride, acetic acid and sodium bicarbonate according to the mass ratio of 1:0.6:3;
the dispersing agent consists of fatty acid polyglycol ether and polyacrylamide in the mass ratio of 1 to 0.56.
The dispersion solution consists of acetone, methyl propyl ketone and glycol diethyl ether acetate according to the volume ratio of 1:0.72:0.3.
The reducing solution is sodium borohydride solution, and the adding ratio of sodium borohydride to water of the sodium borohydride solution is 3 g/70 ml.
The mixed acid consists of nitric acid solution and hydrochloric acid solution according to the volume ratio of 1:15, wherein the mass concentration of the nitric acid solution is 65%, and the mass concentration of the hydrochloric acid solution is 35%.
Example 3
A preparation method of graphene synergistic sol for improving soil quality comprises the following steps:
step one, adding flake graphite into a mixed acid solution, and soaking for 3.5 hours, wherein the adding ratio of the mixed acid solution to the flake graphite is 9ml to 0.4g;
adding 6g/L of intercalation agent into the mixed acid solution, reacting at 50 ℃ for 5 hours, washing until the pH is between 4.6 and 5.3, dispersing by ultrasonic wave for 1.5 hours, and drying at 100 ℃ to obtain graphene oxide;
step three, placing graphene oxide into a reducing solution, and carrying out reaction treatment for 2.5 hours to obtain graphene, wherein the adding ratio of the reducing solution to the graphite oxide is 11 ml/0.25 g;
and step four, adding 350g/L graphene into the dispersion solution, adding 2.5g/L dispersing agent and 10g/L organic bentonite, and carrying out ultrasonic treatment for 35min to obtain the graphene synergistic sol.
Wherein the intercalation agent consists of phosphoric anhydride, acetic acid and sodium bicarbonate according to the mass ratio of 1:0.5:2.5;
the dispersing agent consists of fatty acid polyglycol ether and polyacrylamide in the mass ratio of 1 to 0.62.
The dispersion solution consists of acetone, methyl propyl ketone and glycol diethyl ether acetate according to the volume ratio of 1:0.69:0.35.
The reducing solution is sodium borohydride solution, and the adding ratio of sodium borohydride to water of the sodium borohydride solution is 2.5 g/67 ml.
The mixed acid consists of nitric acid solution and hydrochloric acid solution according to the volume ratio of 1:13, wherein the mass concentration of the nitric acid solution is 63%, and the mass concentration of the hydrochloric acid solution is 37%.
Comparative example 1
The raw material composition and the preparation method are basically the same as those of the example 3, and the difference is that: and in the fourth step, no organic bentonite is added.
Comparative example 2
Is a graphene sol which is commercially available and can be used for soil improvement.
The graphene synergistic sol prepared in the examples 1-3 and the graphene sol prepared in the comparative examples 1-2 were subjected to a storage time test to obtain the following data:
project | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 |
Stable shelf life of sol | >180 days | >187 days | >190 days | <120 days | <90 days |
According to the table, the storage time of the graphene synergistic sol prepared by the method is more than 180 days, and the product quality and stability are good.
According to the preparation method, the preparation process of the graphene synergistic sol is limited, so that the prepared graphene synergistic sol has strong adsorption capacity, and the long-term preservation of nutrients by soil is greatly enhanced, so that the volatilization and deep seepage loss on the soil of the nutrients are effectively controlled, the electrochemical property of the soil can be improved, the fertilizer utilization rate is improved, and the fertilizer saving and synergy effects are realized; when the graphene is dispersed, fatty acid polyethylene glycol ether and polyacrylamide are added as dispersing agents, so that the graphene is uniformly dispersed in a dispersing solution; the addition of the organic bentonite can enable the graphene synergistic sol to be formed stably, and can effectively slow down the trend of the formed graphene synergistic sol that the automatic coagulation becomes large so as to prolong the storage time of the graphene synergistic sol.
The foregoing description is only illustrative of the preferred embodiments of the present application and is not to be construed as limiting the scope of the application, i.e., the application is not to be limited to the details of the claims and the description, but rather is to cover all modifications which are within the scope of the application.
Claims (4)
1. A preparation method of graphene synergistic sol for improving soil quality is characterized by comprising the following steps: the method comprises the following steps:
step one, adding flake graphite into a mixed acid solution, and soaking for 3-4 hours;
adding 5-8g/L of intercalation agent into the mixed acid solution, reacting for 4-6 hours at 45-55 ℃, then washing until the pH is between 4.6-5.3, dispersing for 1-2 hours by using ultrasonic wave, and drying at 100 ℃ to obtain graphene oxide;
thirdly, placing graphene oxide in a reducing solution, and performing reaction treatment for 2-3 hours to obtain graphene;
adding 300-400g/L graphene into the dispersion solution, adding 2-3g/L dispersing agent and 8-12g/L organic bentonite, and performing ultrasonic treatment for 30-40min to obtain graphene synergistic sol;
the intercalation agent consists of phosphoric anhydride, acetic acid and sodium bicarbonate according to the mass ratio of 1:0.4-0.6:2-3;
the dispersing agent consists of fatty acid polyethylene glycol ether and polyacrylamide according to the mass ratio of 1:0.56-0.65;
the dispersion solution consists of acetone, methyl propyl ketone and glycol diethyl ether acetate according to the volume ratio of 1:0.65-0.72:0.3-0.4;
the addition ratio of the mixed acid solution to the crystalline flake graphite is 8-10mL, 0.3-0.5g;
the mixed acid consists of nitric acid solution and hydrochloric acid solution according to the volume ratio of 1:12-15;
the mass concentration of the nitric acid solution is 62-65%, and the mass concentration of the hydrochloric acid solution is 35-40%.
2. The method for preparing the graphene synergistic sol for improving soil quality according to claim 1, which is characterized by comprising the following steps: the reducing solution is sodium borohydride solution.
3. The method for preparing the graphene synergistic sol for improving soil quality according to claim 2, which is characterized by comprising the following steps: the adding ratio of sodium borohydride to water in the sodium borohydride solution is 2-3 g/65-70 mL.
4. The method for preparing the graphene synergistic sol for improving soil quality according to claim 1, which is characterized by comprising the following steps: the addition ratio of the reducing solution to the graphene oxide is 10-12mL, and 0.2-0.3g.
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CN105293476A (en) * | 2015-11-16 | 2016-02-03 | 复旦大学 | Preparation method of large-size graphene oxide or graphene |
CN106146886A (en) * | 2016-06-30 | 2016-11-23 | 常州第六元素材料科技股份有限公司 | A kind of composite of Graphene intercalation silicate and preparation method thereof |
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