CN115926044A - Preparation method of high-strength microgel particles for emergency plugging - Google Patents
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- 239000002245 particle Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000017 hydrogel Substances 0.000 claims abstract description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 24
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920000642 polymer Polymers 0.000 claims abstract description 18
- 239000000178 monomer Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000005485 electric heating Methods 0.000 claims abstract description 13
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 claims abstract description 11
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 239000012763 reinforcing filler Substances 0.000 claims abstract description 10
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 9
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical group C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 8
- 239000003999 initiator Substances 0.000 claims abstract description 8
- 239000012802 nanoclay Substances 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229960000892 attapulgite Drugs 0.000 claims abstract description 4
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 229910052625 palygorskite Inorganic materials 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 9
- 239000008187 granular material Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 20
- 239000002351 wastewater Substances 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000012467 final product Substances 0.000 description 6
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- 230000008569 process Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000000903 blocking effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000010382 chemical cross-linking Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
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- 238000007906 compression Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 238000003889 chemical engineering Methods 0.000 description 1
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- 238000005345 coagulation Methods 0.000 description 1
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- 230000002708 enhancing effect Effects 0.000 description 1
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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Classifications
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
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Abstract
The invention discloses a preparation method of high-strength microgel particles for emergency plugging, which comprises the steps of preparing a hydrophilic monomer, an initiator, a reinforcing filler, a cross-linking agent and water into a pre-polymerization solution; the hydrophilic monomer is a mixture of acrylamide and 2-acrylamide-2-methylpropanesulfonic acid, the initiator is ammonium persulfate, the reinforcing filler is one of nano clay, nano attapulgite and graphene oxide, and the cross-linking agent is methylene bisacrylamide; placing the prepolymerization solution in an open-cover type electric heating reaction kettle to initiate polymerization reaction to obtain polymer hydrogel, drying the polymer hydrogel, grinding the dried polymer hydrogel by an industrial grinder until the dried polymer hydrogel passes through a 70-100-mesh sieve, and obtaining the high-strength microgel particle material for emergency plugging, wherein the high-strength microgel particle material has high mechanical strength, the compressive strength can reach 40MPa under the 80% strain condition, the water-fixing plugging can be completed within 20 seconds, and the unification of the performances of high strength and rapid water-fixing plugging is realized.
Description
Technical Field
The invention belongs to the technical field of environment treatment high polymer materials, and particularly relates to an engineering facility
The preparation method of the water leakage plugging microgel material is particularly suitable for being used for quickly plugging and stopping water in mine tailing ponds and metallurgical solid waste residue fields (ponds), and can also be used for plugging and stopping water in water conservancy projects such as reservoirs, river dams and the like.
Background
A hydrogel is a highly hydrophilic three-dimensional network polymer material, which usually forms a nanometer-scale network structure after Chemical crosslinking, but the high water content and the heterogeneity of the network determine that the mechanical strength of the hydrogel is generally low, which greatly limits the wide application of the hydrogel in the field with high requirements on the mechanical strength (Chemical Engineering Journal,2021,426 131900). Microgels, while very different in size from bulk hydrogels, do not differ much in chemical composition and in structural features on the nanometer scale. The mechanical properties of the conventional microgel generally show a brittle characteristic due to the high chemical crosslinking degree of the conventional microgel, and the high chemical crosslinking degree can greatly limit the water absorption of the microgel.
Hydrogels have found widespread use in ecological management and are due to their unique physicochemical properties such as high water absorption, excellent pore structure, and flexible side chain designability (Environmental Technology & Innovation,2020,20 101107, etc.). In the aspect of water fixation, the hydrogel is dehydrated to obtain xerogel which can absorb water again, so that the hydrogel also has good application value in the aspect of rapid water absorption and water fixation. At the initial stage of mine wastewater leakage (impermeable layer failure and piping under the failure of a drainage system), how to rapidly plug a leakage port is of great significance to prevent large-scale water seepage accidents, and the method can play an important role in preventing large-scale wastewater leakage. In an emergency state, the leakage of the waste water is sudden, so that the plugging material is required to have a rapid plugging performance in the emergency state, so as to meet the requirement of plugging immediately after use. When the water pressure is higher, the material has specific requirements on the mechanical property of the material, and the high mechanical strength can resist larger water pressure impact. Therefore, by utilizing the concept of water plugging, the hydrogel material has high requirements on rapid plugging and mechanical properties in an emergency state.
In the fixation of mine slag-containing wastewater, because the wastewater needing water fixation and plugging is usually flowing or has certain-strength seepage pressure, the working condition puts higher requirements on the mechanical property of the material, so that the improvement of the mechanical property of the microgel can show more excellent performance in more rigorous mine slag-containing wastewater prevention and control, and the development of similar materials has important practical significance.
There are many methods for enhancing hydrogel, wherein the typical method is to introduce sacrificial bonds into hydrogel network, and to achieve the purpose of dissipating energy by the fracture of sacrificial bonds when resisting external force, the commonly used sacrificial bonds include hydrogen bonds (macromolecular communications,2006,27 (13): 1023-1028), coordination bonds (Advanced Materials,2015,27 (12): 2054-2059), and hydrophobic effects (Macromolecules, 2011,44 (12): 4997-5005), etc., which are limited by the traditional preparation method of microgel, and these sacrificial bonds are not easy to introduce in the preparation process of microgel. In order to solve the problem, the method considers the factors of preparation cost, preparation process simplification and the like, aims to prepare the high-strength hydrogel by a method of firstly strengthening the mechanical strength of the body hydrogel and then mechanically crushing, gives consideration to important characteristics such as water absorption rate of the material and the like, and provides a material solution for fixing the wastewater under severe conditions so as to be better applied to actual working conditions.
Disclosure of Invention
The invention aims to provide the preparation method of the high-strength microgel particles for emergency plugging, which has the advantages of easily available raw materials, low production cost, simple preparation process, good mechanical property and capability of realizing perfect combination of high strength and rapid water-fixing plugging, aiming at solving the technical problems of complicated process, poor mechanical strength, high raw material price, high production cost, requirement of special equipment for production, difficulty in meeting the organic unification of high strength and rapid water-fixing plugging and the like of the traditional reversed-phase method for preparing the microgel materials.
In order to achieve the above purpose, the invention provides a preparation method of high-strength microgel particles for emergency plugging, which is implemented by adopting the following processes and steps:
1) Preparing a hydrophilic monomer, an initiator, a reinforcing filler, a cross-linking agent and water into a pre-polymerization solution; the hydrophilic monomer is a mixture of acrylamide and 2-acrylamide-2-methylpropanesulfonic acid, the initiator is ammonium persulfate, the reinforcing filler is one of nano clay, nano attapulgite and graphene oxide, and the cross-linking agent is methylene bisacrylamide;
in the pre-polymerization liquid, the content of the hydrophilic monomer is preferably 20 to 50 weight percent of the total weight of the pre-polymerization liquid; in the hydrophilic monomer, the molar weight ratio of acrylamide to 2-acrylamide-2-methylpropanesulfonic acid is preferably 1:1 to 1:4.
2) And (3) placing the prepolymerization solution in an open-cover type electric heating reaction kettle to initiate polymerization reaction at the temperature of 75-85 ℃ to obtain the polymer hydrogel.
According to experimental research, the temperature of the open-cover type electric heating reaction kettle is controlled within the range of 78-82 ℃, and the polymerization reaction time is more than or equal to 1h.
3) And (3) placing the prepared polymer hydrogel in a dryer at 90-115 ℃ for drying until the water content of the polymer is less than or equal to 5%, and then grinding the dried polymer hydrogel by an industrial grinder until the dried polymer hydrogel passes through a 70-100-mesh sieve, thereby obtaining the emergency plugging high-strength microgel granular material.
In a preferred embodiment of the present invention, the mass of the initiator is preferably 1 to 2wt% of the mass of the hydrophilic monomer; the amount of said reinforcing filler is generally 1 to 10% by weight of the total amount of prepolymer, and the amount of said cross-linking agent is generally 0.05 to 0.2mol% of the molar amount of hydrophilic monomer.
Furthermore, the amount of the reinforcing filler is 2.0 to 6.0 weight percent of the total amount of the prepolymerization liquid.
Further, the temperature of the dryer in the step 3) is 95-105 ℃, and the particles are ground by an industrial grinder until the particles pass through a 75-85-mesh sieve.
The further optimized technical scheme is as follows: in the step 2), the temperature of the open-cover type electric heating reaction kettle is controlled at 80 ℃; the temperature of the dryer in step 3) is controlled at 100 ℃, and the particles are ground by an industrial grinder until the particles pass through a 80-mesh sieve.
Compared with the prior art, the preparation method of the high-strength microgel particles for emergency plugging has the following positive effects:
(1) The high-strength microgel particles prepared by the method take high-strength body hydrogel as a source, have high mechanical strength, and have the compressive strength of 40MPa under the condition of 80% strain.
(2) Tests show that the high-strength microgel particles prepared by the method have the performances of short coagulation time and high early strength, can fulfill the aim of water-fixing plugging within 20 seconds, and realizes the unification of the performances of high strength and rapid water-fixing plugging.
(3) All raw materials required by the invention are industrially produced, and are cheap and easily available.
(4) The invention does not need any special production equipment, the preparation process only relates to the processes of polymerization reaction, drying, mechanical crushing and the like, and compared with the similar products in the market, the invention has no special and extra required process equipment, can realize large-scale preparation, and embodies the advantage of realizing performance improvement without increasing extra cost.
Detailed Description
For the purpose of describing the present invention, the following examples are provided to illustrate the preparation of high strength microgel particles for emergency plugging.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced otherwise than as specifically described herein, and it will be appreciated by those skilled in the art that the present invention may be practiced without departing from the spirit and scope of the present invention and that the present invention is not limited by the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Comparative example
(1) Weighing 20Kg of acrylamide, 17.50Kg of 2-acrylamide-2-methylpropanesulfonic acid, 0.75Kg of ammonium persulfate and 0.056Kg of methylene bisacrylamide, dissolving in 100Kg of water, uniformly mixing in an open-cover electric heating reaction kettle to obtain a pre-polymerization solution, controlling the temperature to 80 ℃, and carrying out polymerization reaction for 1 hour.
(2) And (2) taking out the hydrogel obtained in the step (1), placing the hydrogel in a dryer for drying at the temperature of 100 ℃ until the water content is less than 5%, and then grinding the hydrogel by an industrial grinder until the hydrogel passes through a 80-mesh sieve to obtain a final product.
Example 1
(1) Weighing 20Kg of acrylamide, 17.5Kg of 2-acrylamide-2-methylpropanesulfonic acid, 0.75Kg of ammonium persulfate, 0.056Kg of methylene bisacrylamide and 2.75Kg of nano clay, dissolving in 100Kg of water, uniformly mixing in an open-cover type electric heating reaction kettle to obtain a pre-polymerization solution, controlling the temperature to 80 ℃, and carrying out polymerization reaction for 1 hour.
(2) And (3) taking out the hydrogel obtained in the step (1), placing the hydrogel in a dryer, drying the hydrogel at the temperature of 100 ℃ until the water content is less than 5%, and then grinding the hydrogel by an industrial grinder until the hydrogel passes through a 80-mesh sieve to obtain a final product.
Example 2
(1) Weighing 20Kg of acrylamide, 17.5Kg of 2-acrylamide-2-methylpropanesulfonic acid, 0.75Kg of ammonium persulfate, 0.056Kg of methylene bisacrylamide and 5.5Kg of nano clay, dissolving in 100Kg of water, uniformly mixing in an open-cover electric heating reaction kettle to obtain a pre-polymerization liquid, controlling the temperature to 80 ℃, and carrying out polymerization reaction for 1 hour.
(2) And (2) taking out the hydrogel obtained in the step (1), placing the hydrogel in a dryer for drying at the temperature of 100 ℃ until the water content is less than 5%, and then grinding the hydrogel by an industrial grinder until the hydrogel passes through a 80-mesh sieve to obtain a final product.
Example 3
(1) Weighing 20Kg of acrylamide, 17.5Kg of 2-acrylamide-2-methylpropanesulfonic acid, 0.75Kg of ammonium persulfate, 0.056Kg of methylene bisacrylamide and 8.25Kg of nano clay, dissolving in 100Kg of water, uniformly mixing in an open-cover type electric heating reaction kettle to obtain a pre-polymerization solution, controlling the temperature to 80 ℃, and carrying out polymerization reaction for 1 hour.
(2) And (3) taking out the hydrogel obtained in the step (1), placing the hydrogel in a dryer, drying the hydrogel at the temperature of 100 ℃ until the water content is less than 5%, and then grinding the hydrogel by an industrial grinder until the hydrogel passes through a 80-mesh sieve to obtain a final product.
Example 4
(1) Weighing 20Kg of acrylamide, 17.5Kg of 2-acrylamide-2-methylpropanesulfonic acid, 0.75Kg of ammonium persulfate, 0.056Kg of methylene bisacrylamide and 8.25Kg of graphene oxide, dissolving in 100Kg of water, uniformly mixing in an open-cover type electric heating reaction kettle to obtain a pre-polymerization solution, controlling the temperature to 80 ℃, and carrying out polymerization reaction for 1 hour.
(2) And (3) taking out the hydrogel obtained in the step (1), placing the hydrogel in a dryer, drying the hydrogel at the temperature of 100 ℃ until the water content is less than 5%, and then grinding the hydrogel by an industrial grinder until the hydrogel passes through a 80-mesh sieve to obtain a final product.
Example 5
(1) Weighing 20Kg of acrylamide, 17.5Kg of 2-acrylamide-2-methylpropanesulfonic acid, 0.75g of ammonium persulfate, 0.056g of methylene bisacrylamide and 8.25Kg of attapulgite, dissolving in 100Kg of water, uniformly mixing in an open-cover electric heating reaction kettle to obtain a pre-polymerization liquid, controlling the temperature to 80 ℃, and carrying out polymerization reaction for 1 hour.
(2) And (3) taking out the hydrogel obtained in the step (1), placing the hydrogel in a dryer, drying the hydrogel at the temperature of 100 ℃ until the water content is less than 5%, and then grinding the hydrogel by an industrial grinder until the hydrogel passes through a 80-mesh sieve to obtain a final product.
Performance testing
The samples prepared in the comparative example and examples 1 to 5 were tested for their compression resistance, compression stress at 80% strain, swelling degree, plugging time and other performance indexes under the same test conditions, and the test results are shown in table 1.
TABLE 1
As can be seen from table 1, the comparative example and the example samples are compared in terms of performance, and the compressive strength and blocking performance of the comparative example are much lower than those of all the examples. It can be seen from examples 1 to 5 that the compressive strength of the material gradually increases with the increase of the filler content, and the reinforcing effect of different fillers on the sample is slightly different, and the most preferable is nanoclay, wherein the compressive strength of the bulk hydrogel of the sample prepared in example 3 exceeds 40MPa, and the sample shows excellent mechanical strength. The microgel particles are obtained by drying and crushing corresponding body hydrogel, which shows that the prepared microgel particles have excellent mechanical strength. In addition, the plugging performance is also greatly improved while the strength is improved, and the plugging time of all the examples is between 5 and 30 seconds, which is obviously superior to that of the comparative example. The mechanical strength is improved because the density of the sacrificial bonds in the material is increased due to the increase of the filler, and a better energy dissipation process is embodied when the material resists external loads, so that the mechanical strength is greatly improved. After the nano filler is added, the network of the microgel becomes more compact, the interaction force between the network molecular blocks is greatly improved, the water absorption capacity of the network is gradually reduced, and the swelling degree of the material is reduced. But the slow swelling speed of the material enables water to quickly permeate across particles, and the plugging performance of the material is greatly improved. Through the test data of the comparative example performance, it can be seen that the sample prepared by the embodiment provided by the invention has excellent mechanical properties and rapid water blocking performance, the blocking effect of the material is improved, the blocking speed is greatly improved, and the application value is important.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
According to the preparation method of the high-strength microgel particles for emergency plugging, disclosed by the invention, by adding the optimized nano filler to the components, the mechanical strength of the microgel is improved on the premise of keeping higher water absorption rate, and the slag-containing wastewater can be subjected to quick and efficient water-fixing plugging in a harsh environment.
Claims (10)
1. A preparation method of high-strength microgel particles for emergency plugging is characterized by comprising the following steps:
1) Preparing a hydrophilic monomer, an initiator, a reinforcing filler, a cross-linking agent and water into a pre-polymerization liquid; the hydrophilic monomer is a mixture of acrylamide and 2-acrylamide-2-methylpropanesulfonic acid, the initiator is ammonium persulfate, the reinforcing filler is one of nano clay, nano attapulgite and graphene oxide, and the cross-linking agent is methylene bisacrylamide;
2) Placing the pre-polymerization solution in an open-cover type electric heating reaction kettle to initiate polymerization reaction at the temperature of 75-85 ℃ to obtain polymer hydrogel;
3) And (3) placing the prepared polymer hydrogel in a dryer at 90-115 ℃ for drying until the water content of the polymer is less than or equal to 5%, and then grinding the dried polymer hydrogel by an industrial grinder until the dried polymer hydrogel passes through a 70-100-mesh sieve, thereby obtaining the emergency plugging high-strength microgel granular material.
2. The method of preparing high strength microgel particles for emergency plugging as claimed in claim 1, wherein: in the prepolymerization liquid, the content of the hydrophilic monomer is 20 to 50 weight percent of the total weight of the prepolymerization liquid.
3. The method of preparing high strength microgel particles for emergency plugging as claimed in claim 2, wherein: in the hydrophilic monomer, the molar weight ratio of acrylamide to 2-acrylamide-2-methylpropanesulfonic acid is 1:1 to 1:4.
4. The method for preparing microgel particles for emergency plugging as in claim 1, 2 or 3, wherein: the mass of the initiator is 1-2 wt% of that of the hydrophilic monomer.
5. The method for preparing microgel particles for emergency plugging as claimed in claim 4, wherein: the reinforcing filler accounts for 1-10 wt% of the total weight of the prepolymer.
6. The method of preparing high strength microgel particles for emergency plugging as claimed in claim 5, wherein: the crosslinking agent accounts for 0.05-0.2 mol% of the mol of the hydrophilic monomer.
7. The method of claim 6, wherein the microgel particles for emergency plugging have a high strength, and the method comprises the following steps: the reinforcing filler accounts for 2.0-6.0 wt% of the total weight of the prepolymerization liquid.
8. The method of claim 7, wherein the microgel particles for emergency plugging have a high strength, and the method comprises the following steps: in the step 2), the temperature of the open-cover type electric heating reaction kettle is controlled within the range of 78-82 ℃, and the polymerization reaction time is more than or equal to 1h.
9. The method of preparing high strength microgel particles for emergency plugging as claimed in claim 8, wherein: and 3) grinding the dried polymer hydrogel by an industrial grinder until the dried polymer hydrogel passes through a 75-85-mesh sieve at the temperature of 95-105 ℃ in the dryer in the step 3).
10. The method of preparing high strength microgel particles for emergency plugging as claimed in claim 9, wherein: in the step 2), the temperature of the open-cover type electric heating reaction kettle is controlled at 80 ℃; and 3) controlling the temperature of the dryer in the step 3) to be 100 ℃, and grinding the dried polymer hydrogel by using an industrial grinder until the polymer hydrogel passes through a 80-mesh sieve.
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