CN115636896B - Preparation method of copper-graphene-acrylic acid composite gel - Google Patents
Preparation method of copper-graphene-acrylic acid composite gel Download PDFInfo
- Publication number
- CN115636896B CN115636896B CN202211408934.XA CN202211408934A CN115636896B CN 115636896 B CN115636896 B CN 115636896B CN 202211408934 A CN202211408934 A CN 202211408934A CN 115636896 B CN115636896 B CN 115636896B
- Authority
- CN
- China
- Prior art keywords
- solution
- ultrasonic
- copper
- acrylic acid
- graphene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 26
- 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 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 14
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 42
- 239000011259 mixed solution Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 14
- 239000003999 initiator Substances 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000003431 cross linking reagent Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 238000009826 distribution Methods 0.000 claims description 6
- 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
- 238000010438 heat treatment Methods 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 2
- 238000005303 weighing Methods 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 7
- 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
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 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
- 230000007059 acute toxicity Effects 0.000 description 2
- 231100000403 acute toxicity Toxicity 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
- 239000011780 sodium chloride Substances 0.000 description 2
- 241000238553 Litopenaeus vannamei Species 0.000 description 1
- 241000238552 Penaeus monodon Species 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 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
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000032798 delamination 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
- 210000003608 fece Anatomy 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000000366 juvenile effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003361 porogen Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- 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
Abstract
The invention relates to a preparation method of copper-graphene-acrylic acid composite gel, which adopts a program to control and ultrasonic to control the polymerization reaction process, obtains polymerized hydrogel with uniform structure through suspension polymerization reaction, adopts an ultrasonic reactor with adjustable power 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 so as to obtain a hydrogel product with uniform structure. The composite hydrogel prepared by the invention has special stability and reliability in removing ammonia nitrogen with the concentration less than 5 mg/L. The ammonia nitrogen adsorbed on the surface of the composite hydrogel prepared by the method can be desorbed by more than 98%, so that the effective regeneration of the hydrogel is realized.
Description
Technical Field
The invention relates to the field of polymerization reaction, in particular to a preparation method of copper-graphene-acrylic acid composite gel.
Background
In an aquaculture base, some feeds are added into water to be fed to fishes and shrimps for eating, the temperature change fluctuation is large throughout the year, the residual feeds in the water and excreta of the fishes and shrimps are not timely eaten by the fishes and shrimps and 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.
Research in recent five years shows that ammonia nitrogen has acute toxicity to juvenile shrimps of penaeus monodon, penaeus vannamei boone and the like. The method selects acute toxic ammonia nitrogen of fishes and shrimps as a target substance, and introduces copper ions on a hydrogel framework while synthesizing acrylic acid and graphene hydrogel, so that the conventional acrylic acid-graphene oxide hydrogel is improved, and the ammonia nitrogen removal efficiency in aquaculture tail water is greatly improved by means of the stronger coordination of the copper ions and ammonia while the ion exchange effect of carboxylic acid and ammonium ions is fully exerted, so that the cost of removing the ammonia nitrogen can be effectively reduced. The organic unification of improving the ammonia nitrogen removal rate of the aquaculture tail water and reducing the cost is realized.
In the prior art, copper oxalate, graphene oxide solution and acrylic acid have different densities, so that homogeneous solution is difficult to obtain under the general mechanical stirring or magnetic stirring. Therefore, the compound hydrogel prepared by the traditional stirring and mixing method has the defects of uneven 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 can prepare the copper-graphene-acrylic acid composite gel with more uniform texture and structure, and the composite gel can have a better desorption effect on ammonia nitrogen.
In order to achieve the above 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 power of 600W and 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 with ultrasonic wave of which the power is 600W and the frequency is 40kHz to fully dissolve the solution to obtain a mixed solution B;
step (3): taking 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;
step (4): mixing the mixed solution B and the mixed solution C, and adding the graphene oxide GO solution treated by ultrasonic waves to obtain a mixed solution D;
step (5): placing the mixed solution D into a reaction vessel provided with a condenser, and introducing cooling water into the condenser to enable the reaction vessel to move into an ultrasonic reactor containing water;
step (6): adopts two-stage temperature programming, and simultaneously adjusts ultrasonic power: in the first stage, the ultrasonic power is 200W, the frequency is 40KHz, heating ultrasonic is started from the initial water temperature of 40 ℃, and the temperature is increased from 40 ℃ to 50 ℃ within 5 minutes, and the duration is 5 minutes; in the second stage, the ultrasonic power is 400 watts, the frequency is 40KHz, and the temperature is increased from 50 ℃ to 60 ℃ in 5 minutes for 15 minutes; finally, the copper-graphene-acrylic acid composite gel H-Cu-AA-GO with uniform texture distribution is obtained.
In the step (1), the concentration of graphene oxide is 4mg/ml; in the step (1), ultrasonic treatment was performed 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 addition ratio of the acrylic acid to the copper oxalate is 30:1.2-1.6mL/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 3:1.
And (3) adding an initiator, a cross-linking agent and a pore-forming agent, and magnetically stirring for 30min at 36 ℃.
In the step (3), benzoyl peroxide is adopted as an initiator, N.N' -methylene bisacrylamide is adopted as a cross-linking agent, and cetyltrimethylammonium bromide is adopted as a pore-forming agent.
In the step (4), adding the graphene oxide GO solution after ultrasonic treatment, and continuously stirring for 15-20min to fully mix the graphene oxide GO solution to obtain a mixed solution D.
In the step (5), a single-neck round-bottom flask is adopted as a reaction container, the upper opening of the single-neck round-bottom flask is connected with a condenser, the condenser is connected with condensed water, and the condensed water is put into a water bath of an ultrasonic reactor; the ultrasonic reactor is a power-adjustable and temperature-adjustable ultrasonic reactor.
Compared with the prior art, the invention has the beneficial effects that:
the method adopts the procedures of temperature control and ultrasonic wave control 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 the temperature, so that a hydrogel product with uniform structure is obtained.
According to the invention, copper oxalate is fully dissolved in the reaction, so that the copper oxalate can be uniformly distributed on the hydrogel framework in the subsequent reaction. Since the densities of acrylic acid, copper oxalate and graphene oxide, as well as other additives such as initiator, porogen, etc. are not exactly the same, a slight delamination phenomenon occurs during suspension polymerization, and in order to overcome this situation, a rapid temperature rise is required to allow the mixture to polymerize in solution as soon as possible, and the polymerization process is fastest at 55-60 ℃. The composite hydrogel prepared by the method disclosed by the invention is not layered, and the copper-graphene-acrylic acid composite gel with uniform texture distribution can be obtained.
The composite hydrogel prepared by the invention has special stability and reliability in removing ammonia nitrogen with the concentration less than 5 mg/L. The ammonia nitrogen adsorbed on the surface of the composite hydrogel prepared by the method can be desorbed by more than 98%, so that the effective regeneration of the hydrogel is realized, and a set of economic and feasible scheme for removing low-concentration ammonia nitrogen in water in the aquaculture industry can be provided.
Drawings
Fig. 1: the invention adopts a structural schematic diagram of the device.
Detailed Description
The above-described matters of the present invention will be further described in detail by way of examples, but it should not be construed that the scope of the above-described subject matter of the present invention is limited to the following examples, and all techniques realized based on the above-described matters of the present invention are within the scope of the present invention.
The experimental methods used in the examples below are conventional methods, and the reagents, methods and apparatus used are conventional in the art, unless otherwise indicated.
Example 1:
400mg of graphite oxide powder is weighed, 100.00mL of deionized water is added, the mixture is placed into a water bath with ultrasonic waves with the power of 600W/frequency of 40kHz, the mixture is treated for 12 hours, and a graphene oxide solution with the concentration of 4mg/mL is obtained and marked as a graphene oxide GO solution.
Accurately transferring 30mL of acrylic acid solution, adding 1.6g of copper oxalate solution, placing into a water bath with power of 600W/frequency of 40kHz, and treating for 20min to obtain transparent mixed solution B.
30mL of an acrylic acid solution is accurately removed, 1300mg of benzoyl peroxide serving as an initiator, 1400mg of N.N' -methylene bisacrylamide serving as a cross-linking agent and 700mg of cetyltrimethylammonium bromide serving as a pore-forming agent are added, and the mixture is magnetically stirred for 30min at 36 ℃ to obtain a transparent mixed solution C.
Mix solution B and mix solution C, then add 20.00mL GO solution to get mix 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, and connecting the upper opening of the single-neck round-bottom flask into a condenser and connecting condensed water. The ultrasound is initially warmed up over the water bath.
The heating ultrasound was started from a water temperature of 40 ℃. The two-stage procedure is to heat and adjust the ultrasonic power, wherein in the first step, the ultrasonic power is 200 watts, the frequency is 40KHz, the temperature is raised from 40 ℃ to 50 ℃ within 5 minutes, the duration is 5 minutes, in the second step, the ultrasonic power is 400 watts, the frequency is 40KHz, and the temperature is raised from 50 ℃ to 60 ℃ within 5 minutes, and the duration is 15 minutes. Finally, the composite hydrogel H-Cu-AA-GO with uniform texture distribution is obtained.
Selecting a water sample with ammonia nitrogen concentration of 40mL at 5mg/L as a research object, examining the ammonia nitrogen removal efficiency of 80mg of the composite hydrogel, and after 22H of adsorption, reaching adsorption balance, wherein the ammonia nitrogen concentration in the treated water sample can not reach the detection limit of an instrument and equipment, which indicates that the removal rate of the H-Cu-AA-GO composite hydrogel to an ammonium chloride solution at 5mg/L reaches 100%. The composite hydrogel after saturation is soaked in 0.15mol/L sodium chloride solution for 20 minutes, so that ammonia nitrogen in the composite hydrogel is completely desorbed into the solution.
Example 2:
400mg of graphite oxide powder is weighed, 100.00mL of deionized water is added, the mixture is treated for 12 hours in a water bath with ultrasonic waves with the power of 600W/frequency of 40kHz, and a graphene oxide solution with the concentration of 4mg/mL is obtained and marked as a graphene oxide GO solution.
Accurately transferring 30mL of acrylic acid solution, adding 1.2g of copper oxalate solution, placing into a water bath with power of 600W/frequency of 40kHz, and treating for 30min to obtain transparent mixed solution B.
30mL of an acrylic acid solution is accurately removed, 1300mg of benzoyl peroxide serving as an initiator, 1400mg of N.N' -methylene bisacrylamide serving as a cross-linking agent and 700mg of cetyltrimethylammonium bromide serving as a pore-forming agent are added, and the mixture is magnetically stirred for 30min at 36 ℃ to obtain a transparent mixed solution C.
Mix solution B and mix solution C, then add 20.00mL GO solution to get mix 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, and connecting the upper opening of the single-neck round-bottom flask into a condenser and connecting condensed water. The ultrasound is initially warmed up over the water bath.
The heating ultrasound was started from a water temperature of 40 ℃. The two-stage program heating and adjusting ultrasonic power, wherein the ultrasonic power is 200 watts, the frequency is 40KHz, the temperature is raised from 40 ℃ to 50 ℃ within 5 minutes for 5 minutes, the ultrasonic power is 400 watts, the frequency is 40KHz within 5 minutes, and the duration is 15 minutes; finally, the composite hydrogel H-Cu-AA-GO with uniform texture distribution is obtained.
Comparative example 1:
in the embodiment, a comparative test is carried out, and under the same conditions, the copper oxalate-graphene oxide-acrylic acid composite hydrogel prepared by mechanical and magnetic stirring is characterized in that: the graphene is unevenly distributed in the acrylic composite hydrogel, so that the composite hydrogel is not good in structure, compact in structure, loose in structure and uneven in pore distribution.
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 have a good desorption effect on ammonia nitrogen.
Selecting a water sample with ammonia nitrogen concentration of 5mg/L and 40mL as a research object, examining the ammonia nitrogen removal efficiency of 80mg of the composite hydrogel, and after 22H of adsorption, reaching adsorption balance, wherein the ammonia nitrogen concentration in the treated water sample is 0.5mg/L, and the ammonia chloride solution removal rate of the H (1) -Cu-AA-GO composite hydrogel on 5mg/L reaches 90%. The composite hydrogel after saturation is soaked in 0.15mol/L sodium chloride solution for 20 minutes, so that ammonia nitrogen in the composite hydrogel is completely desorbed into the solution.
The composite hydrogel can realize that the adsorbed ammonia nitrogen can be desorbed by more than 98%, so that the effective regeneration of the hydrogel is realized, and the ammonia nitrogen removal result is shown in Table 1.
TABLE 1 Ammonia nitrogen removal results using copper oxalate-graphene oxide-acrylic acid composite gel of the present invention
The present invention is not limited to the preferred embodiments, and any simple modification, equivalent replacement, and improvement made to the above embodiments by those skilled in the art without departing from the technical scope of the present invention, will fall within the scope of the present invention.
Claims (7)
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 power of 600W and 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 with ultrasonic wave of which the power is 600W and the frequency is 40kHz to fully dissolve the solution to obtain a mixed solution B; in the step (2), the addition ratio of the acrylic acid to the copper oxalate is 30:1.2-1.6 mL/g;
step (3): taking 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;
step (4): mixing the mixed solution B and the mixed solution C, and adding the graphene oxide GO solution treated by ultrasonic waves to obtain a mixed solution D;
step (5): placing the mixed solution D into a reaction vessel provided with a condenser, and introducing cooling water into the condenser to enable the reaction vessel to move into an ultrasonic reactor containing water;
step (6): adopts two-stage temperature programming, and simultaneously adjusts ultrasonic power: in the first stage, the ultrasonic power is 200W, the frequency is 40KHz, heating ultrasonic is started from the initial water temperature of 40 ℃, and the temperature is increased from 40 ℃ to 50 ℃ within 5 minutes, and the duration is 5 minutes; in the second stage, the ultrasonic power is 400 watts, the frequency is 40KHz, and the temperature is increased from 50 ℃ to 60 ℃ in 5 minutes for 15 minutes; finally, copper-graphene-acrylic acid composite gel H-Cu-AA-GO with uniform texture distribution is obtained;
in the step (1), the concentration of graphene oxide is 4mg/ml; in the step (1), ultrasonic treatment is adopted for 12 hours; 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 3:1.
2. The method for preparing the copper-graphene-acrylic composite gel according to claim 1, wherein the method comprises the following steps: 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.
3. The method for preparing the copper-graphene-acrylic composite gel according to claim 1, wherein the method comprises the following steps: and (3) performing ultrasonic treatment for 20-30min in the step (2) to fully dissolve the copper oxalate.
4. The method for preparing the copper-graphene-acrylic composite gel according to claim 1, wherein the method comprises the following steps: and (3) adding an initiator, a cross-linking agent and a pore-forming agent, and magnetically stirring for 30min at 36 ℃.
5. The method for preparing the copper-graphene-acrylic composite gel according to claim 1, wherein the method comprises the following steps: in the step (3), benzoyl peroxide is adopted as an initiator, N.N' -methylene bisacrylamide is adopted as a cross-linking agent, and cetyltrimethylammonium bromide is adopted as a pore-forming agent.
6. The method for preparing the copper-graphene-acrylic composite gel according to claim 1, wherein the method comprises the following steps: in the step (4), adding the graphene oxide GO solution after ultrasonic treatment, and continuously stirring for 15-20min to fully mix the graphene oxide GO solution to obtain a mixed solution D.
7. The method for preparing the copper-graphene-acrylic composite gel according to claim 1, wherein the method comprises the following steps: in the step (5), a single-neck round-bottom flask is adopted as a reaction container, the upper opening of the single-neck round-bottom flask is connected with a condenser, the condenser is connected with condensed water, and the condensed water is put into a water bath of an ultrasonic reactor; the ultrasonic reactor is a power-adjustable and temperature-adjustable ultrasonic reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211408934.XA CN115636896B (en) | 2022-11-11 | 2022-11-11 | Preparation method of copper-graphene-acrylic acid composite gel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211408934.XA CN115636896B (en) | 2022-11-11 | 2022-11-11 | Preparation method of copper-graphene-acrylic acid composite gel |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115636896A CN115636896A (en) | 2023-01-24 |
| CN115636896B true CN115636896B (en) | 2023-11-24 |
Family
ID=84949427
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211408934.XA Active CN115636896B (en) | 2022-11-11 | 2022-11-11 | Preparation method of copper-graphene-acrylic acid composite gel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115636896B (en) |
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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115636896A (en) | 2023-01-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108452780B (en) | It is a kind of selectively to fix selenous adsorbed film and preparation method thereof | |
| CN109601898B (en) | Method for improving gel strength of minced fillet | |
| CN109734174B (en) | Double-load core-shell hydrogel and preparation method and application thereof | |
| CN115636896B (en) | Preparation method of copper-graphene-acrylic acid composite gel | |
| CN101718041A (en) | Fiber base protein molecularly imprinted polymer aquagel and preparation method thereof | |
| CN107964544A (en) | A kind of microalgae algae ball and process for fixation | |
| CN112403282A (en) | Amphiphilic polypropylene porous membrane and preparation method and application thereof | |
| CN113861600B (en) | Bio-based porous material and preparation method and application thereof | |
| CN108906064A (en) | A kind of preparation method for the modified nano zinc oxide that photocatalytic degradation is strong | |
| CN108176351A (en) | A kind of sewage disposal vermiculite based material and its preparation method and application | |
| CN109251278A (en) | A kind of preparation method of mushroom bran base high water-absorption resin | |
| CN105779429A (en) | Preparation method of immobilized degrading bacteria for treating aquaculture ammonia-nitrogen wastewater | |
| CN104690291A (en) | Preparation method of graphene-nano-nickel composite wave-absorbing material | |
| CN107670635B (en) | Sewage treatment filler, preparation method and application | |
| CN112982022B (en) | Preparation method of copper-plated reduced graphene oxide wave-absorbing paper | |
| CN113252834B (en) | Magnetic-assisted matrix solid-phase dispersion extraction method based on hydrophilic effect | |
| CN113941711B (en) | Preparation method and device of high-fluidity micron silver particles | |
| CN116440297A (en) | Radioactive carbon microsphere and its preparation method and application | |
| CN108079950A (en) | A kind of heavy metal containing sewage processing material and its preparation method and application | |
| CN104448072B (en) | Auxiliary control method for phenylethylene polymerization by pulse electromagnetic fields | |
| CN105776403A (en) | Modified zeolite-nanocarbon cyanobacteria treatment agent and preparing method thereof | |
| CN109776731A (en) | A kind of preparation method of polyacrylic acid large-particle size bead-like water-absorbent resin | |
| CN109134957A (en) | A kind of preparation method of abrasive rubber | |
| CN219942447U (en) | Culture solution mixing device for stem cell culture | |
| CN108176352A (en) | A kind of inorganic agent of treated sewage and its preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |