CN115636896A - Preparation method of copper-graphene-acrylic acid composite gel - Google Patents
Preparation method of copper-graphene-acrylic acid composite gel Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 25
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- QYCVHILLJSYYBD-UHFFFAOYSA-L copper;oxalate Chemical compound [Cu+2].[O-]C(=O)C([O-])=O QYCVHILLJSYYBD-UHFFFAOYSA-L 0.000 claims abstract description 13
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 41
- 239000011259 mixed solution Substances 0.000 claims description 26
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000003999 initiator Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000003431 cross linking reagent Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000009826 distribution Methods 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 5
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000000498 cooling water Substances 0.000 claims description 2
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 2
- 239000000017 hydrogel Substances 0.000 abstract description 31
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 abstract description 25
- 239000000499 gel Substances 0.000 abstract description 12
- 238000006116 polymerization reaction Methods 0.000 abstract description 8
- 230000008929 regeneration Effects 0.000 abstract description 3
- 238000011069 regeneration method Methods 0.000 abstract description 3
- 238000010557 suspension polymerization reaction Methods 0.000 abstract description 3
- 241000238557 Decapoda Species 0.000 description 6
- 238000009360 aquaculture Methods 0.000 description 5
- 244000144974 aquaculture Species 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000007059 acute toxicity Effects 0.000 description 3
- 231100000403 acute toxicity Toxicity 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- 241000238553 Litopenaeus vannamei Species 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 241000238552 Penaeus monodon Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- -1 ammonium ions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000000366 juvenile effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/80—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in fisheries management
- Y02A40/81—Aquaculture, e.g. of fish
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention relates to a preparation method of copper-graphene-acrylic acid composite gel, which adopts program temperature control and ultrasonic wave to control the polymerization reaction process, obtains polymerization hydrogel with uniform and consistent structure through suspension polymerization reaction, adopts a power-adjustable ultrasonic reactor in the reaction, carries out ultrasonic treatment on copper oxalate, acrylic acid and graphene oxide solutions with different densities to form a solution with uniform texture, and then controls the ultrasonic power and temperature to slowly and uniformly complete the polymerization reaction, thereby obtaining a hydrogel product with uniform and consistent structure. The composite hydrogel prepared by the invention shows special stability and reliability in removing ammonia nitrogen with the concentration of less than 5 mg/L. The ammonia nitrogen adsorbed on the surface of the composite hydrogel prepared by the invention can be desorbed by more than 98 percent, so that the effective regeneration of the hydrogel is realized.
Description
Technical Field
The invention relates to the field of polymerization reaction, and particularly relates to a preparation method of copper-graphene-acrylic acid composite gel.
Background
In an aquaculture base, feed is required to be added into water for feeding fishes and shrimps, the temperature change fluctuation is large all the year round, the residual feed in the water is not eaten by the fishes and shrimps in time, and the excrement of the fishes and shrimps is released into a water body, so that the ammonia nitrogen concentration in the water body is increased, and the increase of the ammonia nitrogen concentration in the water body has strong acute toxicity to the fishes and shrimps in aquaculture.
The research in the last five years shows that the ammonia nitrogen has acute toxicity to the Penaeus monodon, penaeus vannamei Boone, litopenaeus vannamei Boone, and other juvenile shrimps. The method selects ammonia nitrogen with acute toxicity to fishes and shrimps as a target substance, copper ions are introduced into a hydrogel framework while acrylic acid and graphene hydrogel are synthesized, the existing acrylic acid-graphene oxide hydrogel is improved, the ion exchange effect of carboxylic acid and ammonium ions is fully exerted, the removal efficiency of the ammonia nitrogen in the aquaculture tail water is greatly improved by means of the strong coordination effect of the copper ions and the ammonia, and the cost for removing the ammonia nitrogen can be effectively reduced. Realizes organic unification of improving the removal rate of ammonia nitrogen in the tail water of aquaculture and reducing the cost.
In the prior art, copper oxalate, graphene oxide solution and acrylic acid have different densities, so that homogeneous solutions are difficult to obtain under ordinary mechanical stirring or magnetic stirring. Therefore, the composite hydrogel prepared by the traditional stirring and mixing method has the defects of nonuniform dispersion and inconsistent reaction speed.
Disclosure of Invention
The invention aims to provide a preparation method of copper-graphene-acrylic acid composite gel aiming at the technical problems, which can overcome the problems of uniformity and consistency of polymerization reaction caused by non-uniformity among different substances with certain difference in density and inaccuracy in temperature control, and prepare and obtain copper-graphene-acrylic acid composite gel with more uniform texture and structure, and the composite gel can play a better desorption effect on ammonia nitrogen.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a preparation method of copper-graphene-acrylic acid composite gel is characterized by comprising the following steps: the method comprises the following steps:
step (1): weighing graphite oxide powder, adding deionized water, and performing ultrasonic water bath treatment with the power of 600W and the frequency of 40kHz to obtain a graphene oxide GO solution;
step (2): measuring an acrylic acid solution, adding a copper oxalate solution, and putting the solution into a water bath of ultrasonic waves with the power of 600W and the frequency of 40kHz to fully dissolve the solution to obtain a mixed solution B;
and (3): measuring an acrylic acid solution, sequentially adding an initiator, a cross-linking agent and a pore-forming agent, and magnetically stirring for a period of time to obtain a mixed solution C;
and (4): mixing the mixed solution B and the mixed solution C, and adding the graphene oxide GO solution subjected to ultrasonic treatment to obtain a mixed solution D;
and (5): putting the mixed solution D into a reaction container provided with a condenser, and introducing cooling water into the condenser to move the reaction container into an ultrasonic reactor containing water;
and (6): two-stage temperature programming is adopted, and the ultrasonic power is adjusted: the first stage, ultrasonic power is 200W, frequency is 40KHz, heating ultrasonic from initial water temperature 40 deg.C, raising temperature from 40 deg.C to 50 deg.C within 5 min, and maintaining for 5 min; in the second stage, the ultrasonic power is 400 watts, the frequency is 40KHz, the temperature is increased from 50 ℃ to 60 ℃ within 5 minutes, and the duration is 15 minutes; and finally obtaining the copper-graphene-acrylic acid composite gel H-Cu-AA-GO with uniform texture distribution.
In the step (1), the concentration of the graphene oxide is 4mg/ml; in the step (1), ultrasonic treatment is adopted for 12 hours.
The amount of acrylic acid used in step (2) and the amount of acrylic acid used in step (3) are each half of the total amount of acrylic acid used in the reaction.
In the step (2), the adding ratio of the acrylic acid to the copper oxalate is 30.2-1.6 mL/g.
And (3) performing ultrasonic treatment for 20-30min in the step (2) to fully dissolve the copper oxalate.
The volume ratio of the total amount of acrylic acid used in the reaction to the amount of the graphene oxide GO solution added in the step (4) is 3.
And (3) adding an initiator, a cross-linking agent and a pore-forming agent in the step (3), and magnetically stirring for 30min at 36 ℃.
In the step (3), benzoyl peroxide is adopted as the initiator, N' -methylene-bisacrylamide is adopted as the cross-linking agent, and hexadecyl trimethyl ammonium bromide is adopted as the pore-forming agent.
And (4) adding the graphene oxide GO solution subjected to ultrasonic treatment, continuing stirring for 15-20min, and fully mixing to obtain a mixed solution D.
In the step (5), a single-mouth round-bottom flask is adopted as a reaction container, a condenser is connected to the upper mouth of the single-mouth round-bottom flask, condensed water is connected to the condenser, and the condenser is placed into a water bath of the ultrasonic reactor; the ultrasonic reactor adopts an ultrasonic reactor with adjustable power and adjustable temperature.
Compared with the prior art, the invention has the beneficial effects that:
the method adopts program temperature control and ultrasonic wave to control the polymerization reaction process, and obtains the polymerized hydrogel with uniform and consistent structure through suspension polymerization reaction. In the reaction, an ultrasonic reactor with adjustable power is adopted, copper oxalate, acrylic acid and graphene oxide solutions with different densities are subjected to ultrasonic treatment to form a solution with uniform texture, and then the polymerization reaction is slowly and uniformly completed by controlling the ultrasonic power and temperature, so that a hydrogel product with uniform and consistent structure is obtained.
The method ensures that the copper oxalate is fully dissolved in the reaction and can be uniformly distributed on the hydrogel framework in the subsequent reaction. As the densities of acrylic acid, copper oxalate, graphene oxide and other additives such as an initiator, a pore-forming agent and the like are not completely the same, a slight layering phenomenon can occur in the suspension polymerization reaction, in order to overcome the phenomenon, the temperature needs to be quickly raised, the mixture is heated and polymerized in a solution as soon as possible, and the fastest temperature is reached between 55 and 60 ℃ in the polymerization reaction process. The composite hydrogel prepared by the method of the invention does not delaminate, and can obtain the copper-graphene-acrylic acid composite gel with uniform texture distribution.
The composite hydrogel prepared by the invention shows special stability and reliability in removing ammonia nitrogen with the concentration of less than 5 mg/L. The ammonia nitrogen adsorbed on the surface of the composite hydrogel prepared by the invention can be desorbed by more than 98 percent, so that the effective regeneration of the hydrogel is realized, and a set of economic and feasible scheme can be provided for removing low-concentration ammonia nitrogen in water in the aquaculture industry.
Drawings
FIG. 1: the invention adopts a structural schematic diagram of a device.
Detailed Description
The above-mentioned contents of the present invention are further described in detail by way of examples below, but it should not be understood that the scope of the above-mentioned subject matter of the present invention is limited to the following examples, and any technique realized based on the above-mentioned contents of the present invention falls within the scope of the present invention.
The experimental procedures used in the following examples are conventional procedures unless otherwise specified, and reagents, methods and equipment used therein are conventional in the art unless otherwise specified.
Example 1:
weighing 400mg of graphite oxide powder, adding 100.00mL of deionized water, placing the graphite oxide powder into a water bath with ultrasonic waves with the power of 600W/frequency of 40kHz, and treating for 12 hours to obtain a graphene oxide solution with the concentration of 4mg/mL, wherein the graphene oxide solution is marked as a graphene oxide GO solution.
Accurately transferring 30mL of acrylic acid solution, adding 1.6g of copper oxalate solution, placing the solution into a water bath with ultrasonic waves with the power of 600W/frequency of 40kHz, and treating for 20min to obtain a transparent mixed solution B.
Accurately transferring 30mL of acrylic acid solution, adding 1300mg of initiator benzoyl peroxide, 1400mg of cross-linking agent N, N' -methylene bisacrylamide and 700mg of pore-forming agent hexadecyl trimethyl ammonium bromide, and magnetically stirring for 30min at 36 ℃ to obtain a transparent mixed solution C.
And mixing the mixed solution B and the mixed solution C, and then adding 20.00mL of GO solution to obtain a mixed solution D.
Pouring the mixed solution D into a single-neck round-bottom flask, putting the single-neck round-bottom flask into a water bath of an ultrasonic cleaner, connecting a condenser to the upper port, and connecting condensed water. The ultrasound was started to warm up compared to the water bath.
Heating and ultrasonic treatment are carried out from the water temperature of 40 ℃. The two-stage procedure of heating and regulating the ultrasonic power includes the first step of heating from 40 deg.c to 50 deg.c in 5 min at frequency of 40KHz in 200W and the second step of heating from 50 deg.c to 60 deg.c in 5 min at frequency of 40KHz in 400W and for 15 min. And finally obtaining the composite hydrogel H-Cu-AA-GO with uniform texture distribution.
Selecting a 5mg/L ammonia nitrogen 40mL water sample as a research object, investigating the ammonia nitrogen removal efficiency of 80mg composite hydrogel, and after 22H of adsorption, achieving adsorption balance, wherein the ammonia nitrogen concentration in the treated water sample cannot reach the detection limit of instruments and equipment, which indicates that the removal rate of the H-Cu-AA-GO composite hydrogel to a 5mg/L ammonium chloride solution reaches 100%. And soaking the composite hydrogel after adsorption saturation in 0.15mol/L sodium chloride solution for 20 minutes to ensure that ammonia nitrogen of the composite hydrogel is completely desorbed into the solution.
Example 2:
weighing 400mg of graphite oxide powder, adding 100.00mL of deionized water, and treating for 12 hours in an ultrasonic water bath with power of 600W/frequency of 40kHz to obtain a graphene oxide solution with concentration of 4mg/mL, wherein the graphene oxide solution is marked as graphene oxide GO solution.
Accurately transferring 30mL of acrylic acid solution, adding 1.2g of copper oxalate solution, placing the solution into a water bath with ultrasonic waves with the power of 600W/frequency of 40kHz, and treating for 30min to obtain a transparent mixed solution B.
Accurately transferring 30mL of acrylic acid solution, adding 1300mg of initiator benzoyl peroxide, 1400mg of cross-linking agent N.N' -methylene bisacrylamide and 700mg of pore-forming agent hexadecyl trimethyl ammonium bromide, and magnetically stirring for 30min at 36 ℃ to obtain a transparent mixed solution C.
And mixing the mixed solution B and the mixed solution C, and then adding 20.00mL of GO solution to obtain a mixed solution D.
Pouring the mixed solution D into a single-neck round-bottom flask, putting the single-neck round-bottom flask into a water bath of an ultrasonic cleaner, connecting a condenser at the upper port, and connecting condensed water. The ultrasound was started to warm up compared to the water bath.
Heating and ultrasonic processing are carried out from the water temperature of 40 ℃. The two-stage program heating and ultrasonic power adjustment, wherein in the first step, the ultrasonic power is 200 watts and the frequency is 40KHz, the temperature is increased from 40 ℃ to 50 ℃ within 5 minutes, and the duration is 5 minutes, in the second step, the temperature is increased from 50 ℃ to 60 ℃, the ultrasonic power is 400 watts and the frequency is 40KHz within 5 minutes, and the duration is 15 minutes; and finally obtaining the composite hydrogel H-Cu-AA-GO with uniform texture distribution.
Comparative example 1:
in the examples, comparative tests were carried out, and the copper oxalate-graphene oxide-acrylic acid composite hydrogel prepared by mechanical and magnetic stirring under the same conditions was characterized by: the graphene is unevenly distributed in the acrylic acid composite hydrogel, so that the composite hydrogel has a poor structure, some structures are compact and some structures are loose, and the distribution of pores is also uneven.
The copper-graphene-acrylic acid composite gel with more uniform texture and structure can be obtained.
Example 3:
the composite gel provided by the invention can achieve a good desorption effect on ammonia nitrogen.
Selecting a 5mg/L ammonia nitrogen 40mL water sample as a research object, investigating the removal efficiency of 80mg composite hydrogel on ammonia nitrogen, and after 22H of adsorption, achieving adsorption balance, wherein the ammonia nitrogen concentration of the treated water sample is 0.5mg/L, and the removal rate of the H (1) -Cu-AA-GO composite hydrogel on a 5mg/L ammonium chloride solution reaches 90%. And soaking the saturated composite hydrogel in 0.15mol/L sodium chloride solution for 20 minutes to ensure that ammonia nitrogen of the composite hydrogel is completely desorbed into the solution.
The composite hydrogel can realize that more than 98% of adsorbed ammonia nitrogen can be desorbed, so that the effective regeneration of the hydrogel is realized, and the ammonia nitrogen removal result is shown in table 1.
Table 1 results of ammonia nitrogen removal using the copper oxalate-graphene oxide-acrylic acid composite gel of the present invention
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention in any way, and any simple modifications, equivalents and improvements made by those skilled in the art without departing from the technical scope of the present invention are all within the scope of the present invention.
Claims (10)
1. A preparation method of copper-graphene-acrylic acid composite gel is characterized by comprising the following steps: the method comprises the following steps:
step (1): weighing graphite oxide powder, adding deionized water, and performing ultrasonic water bath treatment with the power of 600W and the frequency of 40kHz to obtain a graphene oxide GO solution;
step (2): measuring an acrylic acid solution, adding a copper oxalate solution, and putting the solution into a water bath of ultrasonic waves with the power of 600W and the frequency of 40kHz to fully dissolve the solution to obtain a mixed solution B;
and (3): measuring an acrylic acid solution, sequentially adding an initiator, a cross-linking agent and a pore-forming agent, and magnetically stirring for a period of time to obtain a mixed solution C;
and (4): mixing the mixed solution B with the mixed solution C, and adding the graphene oxide GO solution subjected to ultrasonic treatment to obtain a mixed solution D;
and (5): putting the mixed solution D into a reaction container provided with a condenser, and introducing cooling water into the condenser to move the reaction container into an ultrasonic reactor containing water;
and (6): two-stage temperature programming is adopted, and the ultrasonic power is adjusted: the first stage, ultrasonic power is 200W, frequency is 40KHz, heating ultrasonic from initial water temperature 40 deg.C, raising temperature from 40 deg.C to 50 deg.C within 5 min, and maintaining for 5 min; in the second stage, the ultrasonic power is 400 watts, the frequency is 40KHz, the temperature is increased from 50 ℃ to 60 ℃ within 5 minutes, and the duration is 15 minutes; finally, the copper-graphene-acrylic acid composite gel H-Cu-AA-GO with uniform texture distribution is obtained.
2. The method for preparing the copper-graphene-acrylic acid composite gel according to claim 1, wherein: in the step (1), the concentration of the graphene oxide is 4mg/ml; in the step (1), ultrasonic treatment is adopted for 12 hours.
3. The method for preparing the copper-graphene-acrylic acid composite gel according to claim 1, characterized in that: the amount of acrylic acid used in step (2) and the amount of acrylic acid used in step (3) are each half of the total amount of acrylic acid used in the reaction.
4. The method for preparing the copper-graphene-acrylic acid composite gel according to claim 1, wherein: in the step (2), the adding ratio of the acrylic acid to the copper oxalate is 30.2-1.6 mL/g.
5. The method for preparing the copper-graphene-acrylic acid composite gel according to claim 1, characterized in that: and (3) performing ultrasonic treatment for 20-30min in the step (2) to fully dissolve the copper oxalate.
6. The method for preparing the copper-graphene-acrylic acid composite gel according to claim 1, characterized in that: the volume ratio of the total amount of acrylic acid used in the reaction to the amount of the graphene oxide GO solution added in the step (4) is 3.
7. The method for preparing the copper-graphene-acrylic acid composite gel according to claim 1, wherein: and (3) adding an initiator, a cross-linking agent and a pore-forming agent in the step (3), and magnetically stirring for 30min at 36 ℃.
8. The method for preparing the copper-graphene-acrylic acid composite gel according to claim 1, characterized in that: in the step (3), benzoyl peroxide is adopted as an initiator, N' -methylene bisacrylamide is adopted as a cross-linking agent, and hexadecyl trimethyl ammonium bromide is adopted as a pore-forming agent.
9. The method for preparing the copper-graphene-acrylic acid composite gel according to claim 1, wherein: and (4) adding the graphene oxide GO solution subjected to ultrasonic treatment, continuing stirring for 15-20min, and fully mixing to obtain a mixed solution D.
10. The method for preparing the copper-graphene-acrylic acid composite gel according to claim 1, characterized in that: in the step (5), the reaction container adopts a single-mouth round-bottom flask, the upper mouth of the single-mouth round-bottom flask is connected with a condenser, the condenser is connected with condensed water, and the condensed water is placed into a water bath of the ultrasonic reactor; the ultrasonic reactor adopts an ultrasonic reactor with adjustable power and adjustable temperature.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02180633A (en) * | 1988-12-28 | 1990-07-13 | Toyota Central Res & Dev Lab Inc | Multi-component adsorption material |
| CN104801286A (en) * | 2015-05-14 | 2015-07-29 | 安徽大学 | Graphene oxide hydroxy propyl cellulose composite hydrogel as well as preparing method and application thereof |
| CN110511402A (en) * | 2019-09-12 | 2019-11-29 | 东华大学 | A kind of cobalt cross-linked hydrogel and preparation method thereof with high cross-link intensity |
| CN110746785A (en) * | 2019-11-25 | 2020-02-04 | 黄春美 | High-strength anti-freezing three-dimensional porous hydrogel adsorption material and preparation method thereof |
| CN110790856A (en) * | 2019-11-14 | 2020-02-14 | 淄博宏达助剂有限公司 | Graphene oxide/polyacrylic acid composite hydrogel and preparation method thereof |
| CN112246233A (en) * | 2020-10-20 | 2021-01-22 | 程龙 | Preparation method of GO/PVA composite hydrogel |
| CN114752075A (en) * | 2022-03-08 | 2022-07-15 | 武汉工程大学 | Preparation method of copper sulfide-graphene-polyaniline composite hydrogel |
-
2022
- 2022-11-11 CN CN202211408934.XA patent/CN115636896B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02180633A (en) * | 1988-12-28 | 1990-07-13 | Toyota Central Res & Dev Lab Inc | Multi-component adsorption material |
| CN104801286A (en) * | 2015-05-14 | 2015-07-29 | 安徽大学 | Graphene oxide hydroxy propyl cellulose composite hydrogel as well as preparing method and application thereof |
| CN110511402A (en) * | 2019-09-12 | 2019-11-29 | 东华大学 | A kind of cobalt cross-linked hydrogel and preparation method thereof with high cross-link intensity |
| CN110790856A (en) * | 2019-11-14 | 2020-02-14 | 淄博宏达助剂有限公司 | Graphene oxide/polyacrylic acid composite hydrogel and preparation method thereof |
| CN110746785A (en) * | 2019-11-25 | 2020-02-04 | 黄春美 | High-strength anti-freezing three-dimensional porous hydrogel adsorption material and preparation method thereof |
| CN112246233A (en) * | 2020-10-20 | 2021-01-22 | 程龙 | Preparation method of GO/PVA composite hydrogel |
| CN114752075A (en) * | 2022-03-08 | 2022-07-15 | 武汉工程大学 | Preparation method of copper sulfide-graphene-polyaniline composite hydrogel |
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