CN108641724A - A kind of preparation method of water-loss reducer of soil - Google Patents
A kind of preparation method of water-loss reducer of soil Download PDFInfo
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- CN108641724A CN108641724A CN201810515958.2A CN201810515958A CN108641724A CN 108641724 A CN108641724 A CN 108641724A CN 201810515958 A CN201810515958 A CN 201810515958A CN 108641724 A CN108641724 A CN 108641724A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/14—Soil-conditioning materials or soil-stabilising materials containing organic compounds only
- C09K17/16—Soil-conditioning materials or soil-stabilising materials containing organic compounds only applied in a physical form other than a solution or a grout, e.g. as platelets or granules
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/14—Soil-conditioning materials or soil-stabilising materials containing organic compounds only
- C09K17/18—Prepolymers; Macromolecular compounds
- C09K17/20—Vinyl polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2101/00—Agricultural use
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- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Health & Medical Sciences (AREA)
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Abstract
The invention discloses a kind of preparation methods of water-loss reducer of soil, belong to soil remediation technology field.With polysuccinimide and hydrazine hydrate polymerisation occurs for the present invention, again with methacrylic acid, vinyl phosphoric acid dimethyl ester is raw material, crosslinking and initiator is added, phosphoric acid microspheres are prepared using the method for precipitation condistillation, phosphate radical is introduced on microballoon, it under the low humidity or even under anhydrous condition can be quickly from dissociation for pharmalyte phosphate radical, promote the transmission of film inner proton under the low humidity, polyether-ether-ketone is added and carries out sulfonation, phosphoric acid microspheres are filled into wherein, composite membrane is formed to wrap up retention activity object, form microcapsule structure, improve the water-absorbing-retaining ability of film, it enhances proton and is transmitted with transporting mechanism, it is mutually adjusted in the state that soil moisture abundance is with lack of moisture, ensure the balance of soil moisture.The present invention solves that current water-loss reducer of soil stability is poor, water conservation time short problem.
Description
Technical field
The present invention relates to soil remediation technology fields, and in particular to a kind of preparation method of water-loss reducer of soil.
Background technology
China's Arid＆semi-arid area gross area is 4,550,000 hm2, the 47% of territory total area is accounted for, with China's strategic emphasis
It is gradually shifted to western part, water resource increasingly becomes one of important restriction factor of the national economic development.China's agricultural water accounts for
The 73.4% of total water consumption, about 30,000,000,000 m of annual agricultural water shortage3, since water shortage and water production efficiency are low, agricultural water crisis is not
Disconnected aggravation.The water-saving irrigation and dry farming water conservation and moisture-holding technology developed centered on making full use of natural precipitation has become agricultural
The inevitable choice of sustainable development, wherein it is the water-saving one kind of modern agriculture effectively way to reach water-saving and yield-increasing using soil moisturizing agent
Diameter and method.Soil moisturizing agent is also known as water-loss reducer of soil, high water absorbent, is to have height using a kind of made of strong absorptive resin
The high molecular polymer of water-absorbing-retaining ability, the moisture of its hundreds times or even thousands of times of energy absorptance itself weight, and slow release
It is absorbed and utilized for crop, to enhance water retention, reduces the deep percolation and loss of soil nutrient of water, improve water utilization
Rate.Soil moisturizing agent can both absorb moisture from humid air, can also absorb the steam that deep subsoil moves upwards, enhancing
The moisture holding capacity of soil.Moisturizer is a kind of novel high polymer material with super-strong moisture absorbing, water retention property, to inhibiting the soil water
Significant effect is lost in shunting, and can alleviate well influences caused by precipitation is on the low side agricultural production.Apply moisturizing first in the world
The country of agent is the U.S., the research center of United States Department of Agriculture the north in 1969（NRRC）Moisturizer is developed first and in the seventies
Phase is applied to corn and soya seeds coating, sapling transplanting etc..Then, United States Department of Agriculture forest service department and some
University uses Terra-sorb（TAB）Carried out a series of experiments, find TAB for ground spread fertilizer over the fields can using water wisely 50% ~
85%.1974, moisturizer realized industrialized production in u s company.But Japan has then paid a high price for its patent, and herein
On the basis of catch up with rapidly and be more than the U.S., develop polyacrylate super absorbent resin in succession.The beginning of the eighties, Lyons, France
Sha Feimu chemical companies succeed in developing moisturizer, and are applied to the soil improvement of Saudi Arabia arid area.1998,
World's moisturizer total demand is at 700,000 tons or so, and nearly 2 years are incremented by with 8% amplitude.In addition, developing country such as ink west
Brother, Southeast Asia and Middle East also begin to promote and apply.
Invention content
The technical problems to be solved by the invention：It is poor for current water-loss reducer of soil stability, water conservation time short problem,
A kind of preparation method of water-loss reducer of soil is provided.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of preparation method of water-loss reducer of soil, which is characterized in that the preparation method includes the following steps：
（1）Take polysuccinimide in mass ratio 1：4 ~ 6 are added N, and N '-dimethyl formamide is stirred in 75 ~ 80 DEG C, then
The hydrazine hydrate of dimethylformamide quality 20 ~ 25% is added, is stirred in 35 ~ 40 DEG C, filters, takes filter residue and drying, obtain drying
Object；
（2）Take dried object in mass ratio 1：7 ~ 10 are added deionized water, adjust pH to 9 ~ 10, add deionized water quality 3 ~ 5%
Ethylene glycol diglycidylether, be stirred in 45 ~ 50 DEG C, obtain stirring mixture, it is spare；
（3）According to the mass fraction, take 15 ~ 20 parts of methacrylic acids, 10 ~ 15 parts of vinyl phosphoric acid dimethyl esters, 2 ~ 4 parts of 2,2'- even
Nitrogen bis-isobutyronitrile, 50 ~ 70 parts of acetonitriles, ultrasonic disperse obtain mixture, take mixture in mass ratio 80 ~ 90：1 ~ 3 is added ethylene glycol
Dimethylacrylate is warming up to 95 ~ 100 DEG C and is stirred, must stir mixture A, takes stirring mixture A in mass ratio 1：5~
7 are added in hydrochloric acid, are stirred in 100 ~ 105 DEG C, rotary evaporation, centrifuge, and precipitation is taken to be washed through deionized water, dry, obtain dry
Dry object A；
（4）Take polyether-ether-ketone in mass ratio 1：10 ~ 13 are added sulfuric acid, are stirred in 25 ~ 30 DEG C, are warming up to 40 ~ 45 DEG C of heat preservations 6
~ 8h adjusts pH to 7 ~ 7.5, obtains mixture A, take dried object A, step（2）Spare stirring mixture in mass ratio 2 ~ 5：3~7：
10 ~ 13 are added N, and N '-dimethyl formamide is stirred 30 ~ 40min, obtains mixed liquor A, takes mixture A in mass ratio 1：4 ~ 6 add
Enter N, N '-dimethyl formamide is stirred 40 ~ 50min, obtains mixed liquid B, takes mixed liquor A in mass ratio 2 ~ 5:3 ~ 6 additions are mixed
Liquid B is closed, is stirred in 25 ~ 30 DEG C, 10 ~ 12h is kept the temperature in 60 ~ 80 DEG C, is cooled to room temperature, be freeze-dried to get soil water-retaining
Agent.
Compared with other methods, advantageous effects are the present invention：
（1）With polysuccinimide and hydrazine hydrate polymerisation occurs for the present invention, then occurs with ethylene glycol diglycidylether
Reaction obtains the network structure being bonded with tertiary amine, ehter bond, and when temperature is higher, ester bond will not occur for the water-keeping gel of formation
Hydrolytic cleavage improves the stability of water conservation；
（2）Crosslinking and initiator is added using methacrylic acid, vinyl phosphoric acid dimethyl ester as raw material in the present invention, altogether using precipitation
The method of distillation prepares phosphoric acid microspheres, and phosphate radical is introduced on microballoon, is pharmalyte, both can as proton donor or
It can be used as receptor, and quick dynamic hydrogen bond network can be formed between phosphate radical and soil water molecule, promote proton
Carrier movement activity, in addition, phosphate radical can promote film inner proton to exist quickly from dissociating under the low humidity or even under anhydrous condition
Transmission under low humidity is added polyether-ether-ketone and carries out sulfonation, and phosphoric acid microspheres are filled into wherein, forms composite membrane to retention activity
Object is wrapped up, and microcapsule structure is formed, while a large amount of phosphate radical in micro-capsule surface promotes proton to be transmitted with Hopping mechanism,
Micro-capsule inner cavity provides a large amount of space for the storage of water, improves the water-absorbing-retaining ability of film, enhances proton with transporter
Reason is transmitted, and is mutually adjusted in the state that soil moisture abundance is with lack of moisture, is ensured the balance of soil moisture.
Specific implementation mode
A kind of preparation method of water-loss reducer of soil, includes the following steps：
（1）Take polysuccinimide in mass ratio 1：4 ~ 6 are added N, N '-dimethyl formamide, it is stirred 20 in 75 ~ 80 DEG C ~
30min adds the hydrazine hydrate of dimethylformamide quality 20 ~ 25%, and 3 ~ 4h is stirred in 35 ~ 40 DEG C, filters, takes filter residue
It is dry, obtain dried object；
（2）Take dried object in mass ratio 1：7 ~ 10 are added deionized water, adjust pH to 9 ~ 10, add deionized water quality 3 ~ 5%
Ethylene glycol diglycidylether, be stirred 2 ~ 3h in 45 ~ 50 DEG C, obtain stirring mixture, it is spare；
（3）According to the mass fraction, take 15 ~ 20 parts of methacrylic acids, 10 ~ 15 parts of vinyl phosphoric acid dimethyl esters, 2 ~ 4 parts of 2,2'- even
Nitrogen bis-isobutyronitrile, 50 ~ 70 parts of acetonitriles, 20 ~ 30min of ultrasonic disperse obtain mixture, take mixture in mass ratio 80 ~ 90：1 ~ 3 adds
Enter ethylene glycol dimethacrylate, be warming up to 95 ~ 100 DEG C and be stirred 60 ~ 70min, mixture A must be stirred, takes stirring mixed
Close object A in mass ratio 1：5 ~ 7 are added in the hydrochloric acid of a concentration of 10mol/L, it is stirred 18 in 100 ~ 105 DEG C ~ for 24 hours, rotation is steamed
Hair, centrifugation take precipitation to be washed through deionized water, dry, obtain dried object A；
（4）Take polyether-ether-ketone in mass ratio 1：10 ~ 13 are added the sulfuric acid that mass fractions are 98%, it is stirred 1 in 25 ~ 30 DEG C ~
2h is warming up to 40 ~ 45 DEG C of 6 ~ 8h of heat preservation, adjusts pH to 7 ~ 7.5, obtain mixture A, take dried object A, step（2）Spare stirring
Mixture in mass ratio 2 ~ 5：3~7：10 ~ 13 are added N, and N '-dimethyl formamide is stirred 30 ~ 40min, obtains mixed liquor A, takes
Mixture A in mass ratio 1：4 ~ 6 are added N, and N '-dimethyl formamide is stirred 40 ~ 50min, obtains mixed liquid B, takes mixed liquor A
In mass ratio 2 ~ 5:3 ~ 6 are added mixed liquid B, and 1 ~ 2h is stirred in 25 ~ 30 DEG C, keep the temperature 10 ~ 12h in 60 ~ 80 DEG C, are cooled to room
Temperature is freeze-dried to get water-loss reducer of soil.
Embodiment 1
A kind of preparation method of water-loss reducer of soil, includes the following steps：
（1）Take polysuccinimide in mass ratio 1：4 are added N, and N '-dimethyl formamide is stirred 20min in 75 DEG C, then
The hydrazine hydrate of dimethylformamide quality 20% is added, 3h is stirred in 35 DEG C, filters, takes filter residue and drying, obtain dried object；
（2）Take dried object in mass ratio 1：7 are added deionized water, adjust pH to 9, add the ethylene glycol of deionized water quality 3%
Diglycidyl ether is stirred 2h in 45 DEG C, obtains stirring mixture, spare；
（3）According to the mass fraction, 15 parts of methacrylic acids, 10 parts of vinyl phosphoric acid dimethyl esters, 2 parts of 2,2'- azos, two isobutyls are taken
Nitrile, 50 parts of acetonitriles, ultrasonic disperse 20min obtain mixture, take mixture in mass ratio 80：1 is added ethyleneglycol dimethacrylate
Ester is warming up to 95 DEG C and is stirred 60min, must stir mixture A, takes stirring mixture A in mass ratio 1：5 additions are a concentration of
In the hydrochloric acid of 10mol/L, 18h, rotary evaporation are stirred in 100 DEG C, centrifugation takes precipitation to be washed through deionized water, dry, obtains
Dried object A；
（4）Take polyether-ether-ketone in mass ratio 1：10 are added the sulfuric acid that mass fraction is 98%, are stirred 1h in 25 DEG C, are warming up to
40 DEG C of heat preservation 6h, adjust pH to 7, obtain mixture A, take dried object A, step（2）Spare stirring mixture in mass ratio 2：3：
10 are added N, and N '-dimethyl formamide is stirred 30min, obtains mixed liquor A, takes mixture A in mass ratio 1：4 are added N, N '-
Dimethylformamide is stirred 40min, obtains mixed liquid B, takes mixed liquor A in mass ratio 2:3 are added mixed liquid B, are stirred in 25 DEG C
Mixing 1h is mixed, 10h is kept the temperature in 60 DEG C, is cooled to room temperature, be freeze-dried to get water-loss reducer of soil.
Embodiment 2
A kind of preparation method of water-loss reducer of soil, includes the following steps：
（1）Take polysuccinimide in mass ratio 1：5 are added N, and N '-dimethyl formamide is stirred 25min in 78 DEG C, then
The hydrazine hydrate of dimethylformamide quality 23% is added, 3.5h is stirred in 38 DEG C, filters, takes filter residue and drying, obtain dried object；
（2）Take dried object in mass ratio 1：9 are added deionized water, adjust pH to 9.5, add the second two of deionized water quality 4%
Alcohol diglycidyl ether is stirred 2.5h in 48 DEG C, obtains stirring mixture, spare；
（3）According to the mass fraction, 18 parts of methacrylic acids, 13 parts of vinyl phosphoric acid dimethyl esters, 3 parts of 2,2'- azos, two isobutyls are taken
Nitrile, 60 parts of acetonitriles, ultrasonic disperse 25min obtain mixture, take mixture in mass ratio 85：2 are added ethyleneglycol dimethacrylate
Ester is warming up to 98 DEG C and is stirred 65min, must stir mixture A, takes stirring mixture A in mass ratio 1：6 additions are a concentration of
In the hydrochloric acid of 10mol/L, 21h, rotary evaporation are stirred in 103 DEG C, centrifugation takes precipitation to be washed through deionized water, dry, obtains
Dried object A；
（4）Take polyether-ether-ketone in mass ratio 1：11 are added the sulfuric acid that mass fraction is 98%, and 1.5h is stirred in 28 DEG C, heat up
To 43 DEG C of heat preservation 7h, pH to 7.3 is adjusted, mixture A is obtained, takes dried object A, step（2）Spare stirring mixture is in mass ratio
3：5：12 are added N, and N '-dimethyl formamide is stirred 35min, obtains mixed liquor A, takes mixture A in mass ratio 1：5 are added N,
N '-dimethyl formamide is stirred 45min, obtains mixed liquid B, takes mixed liquor A in mass ratio 4:5 are added mixed liquid B, in 28 DEG C
It is stirred 1.5h, 11h is kept the temperature in 70 DEG C, is cooled to room temperature, be freeze-dried to get water-loss reducer of soil.
Embodiment 3
A kind of preparation method of water-loss reducer of soil, includes the following steps：
（1）Take polysuccinimide in mass ratio 1：6 are added N, and N '-dimethyl formamide is stirred 30min in 80 DEG C, then
The hydrazine hydrate of dimethylformamide quality 25% is added, 4h is stirred in 40 DEG C, filters, takes filter residue and drying, obtain dried object；
（2）Take dried object in mass ratio 1：10 are added deionized water, adjust pH to 10, add the second two of deionized water quality 5%
Alcohol diglycidyl ether is stirred 3h in 50 DEG C, obtains stirring mixture, spare；
（3）According to the mass fraction, 20 parts of methacrylic acids, 15 parts of vinyl phosphoric acid dimethyl esters, 4 parts of 2,2'- azos, two isobutyls are taken
Nitrile, 70 parts of acetonitriles, ultrasonic disperse 30min obtain mixture, take mixture in mass ratio 90：3 are added ethyleneglycol dimethacrylate
Ester is warming up to 100 DEG C and is stirred 70min, must stir mixture A, takes stirring mixture A in mass ratio 1：7 additions are a concentration of
It in the hydrochloric acid of 10mol/L, is stirred for 24 hours, rotary evaporation, centrifuges in 105 DEG C, precipitation is taken to be washed through deionized water, it is dry, it obtains
Dried object A；
（4）Take polyether-ether-ketone in mass ratio 1：13 are added the sulfuric acid that mass fraction is 98%, are stirred 2h in 30 DEG C, are warming up to
45 DEG C of heat preservation 8h, adjust pH to 7.5, obtain mixture A, take dried object A, step（2）Spare stirring mixture in mass ratio 5：
7：13 are added N, and N '-dimethyl formamide is stirred 40min, obtains mixed liquor A, takes mixture A in mass ratio 1：6 are added N,
N '-dimethyl formamide is stirred 50min, obtains mixed liquid B, takes mixed liquor A in mass ratio 5:6 are added mixed liquid B, in 30 DEG C
It is stirred 2h, 12h is kept the temperature in 80 DEG C, is cooled to room temperature, be freeze-dried to get water-loss reducer of soil.
Comparative example：The soil moisturizing agent of Linyi City company production.
Soil moisturizing agent obtained by embodiment 1,2,3 and comparative example is respectively used to, to wheat bud ratio statistical test, select
The plantation of wheat is carried out to the wheat planting of 4 pieces of identical planting conditions, water capacity 60% is applied by 5kg/ mus of amount respectively
Add water-retaining agent.Sowing wheat counts the bud ratio of wheat after 15 days, 30 days, and test result is shown in Table 1.
Table 1：
In summary, soil moisturizing agent moisture-holding capacity produced by the present invention is big it can be seen from detection data in upper table, is retained the time
It is longer, it has broad application prospects.
Claims (1)
1. a kind of preparation method of water-loss reducer of soil, which is characterized in that the preparation method includes the following steps：
Take polysuccinimide in mass ratio 1：4 ~ 6 are added N, and N '-dimethyl formamide is stirred in 75 ~ 80 DEG C, adds
The hydrazine hydrate of dimethylformamide quality 20 ~ 25% is stirred in 35 ~ 40 DEG C, is filtered, is taken filter residue and drying, obtain dried object；
Take dried object in mass ratio 1：7 ~ 10 are added deionized water, adjust pH to 9 ~ 10, add deionized water quality 3 ~ 5%
Ethylene glycol diglycidylether is stirred in 45 ~ 50 DEG C, obtains stirring mixture, spare；
According to the mass fraction, 15 ~ 20 parts of methacrylic acids, 10 ~ 15 parts of vinyl phosphoric acid dimethyl esters, 2 ~ 4 parts of 2,2'- azos two are taken
Isobutyronitrile, 50 ~ 70 parts of acetonitriles, ultrasonic disperse obtain mixture, take mixture in mass ratio 80 ~ 90：1 ~ 3 is added glycol dinitrate
Base acrylate is warming up to 95 ~ 100 DEG C and is stirred, obtains stirring mixture, takes stirring mixture A in mass ratio 1：5 ~ 7 are added
It in hydrochloric acid, is stirred, rotary evaporation, centrifuges in 100 ~ 105 DEG C, precipitation is taken to be washed through deionized water, it is dry, obtain dried object A；
Take polyether-ether-ketone in mass ratio 1：10 ~ 13 be added sulfuric acid, be stirred in 25 ~ 30 DEG C, be warming up to 40 ~ 45 DEG C heat preservation 6 ~
8h adjusts pH to 7 ~ 7.5, obtains mixture A, take dried object A, step（2）Spare stirring mixture in mass ratio 2 ~ 5：3~7：
10 ~ 13 are added N, and N '-dimethyl formamide is stirred 30 ~ 40min, obtains mixed liquor A, takes mixture A in mass ratio 1：4 ~ 6 add
Enter N, N '-dimethyl formamide is stirred 40 ~ 50min, obtains mixed liquid B, takes mixed liquor A in mass ratio 2 ~ 5:3 ~ 6 additions are mixed
Liquid B is closed, is stirred in 25 ~ 30 DEG C, 10 ~ 12h is kept the temperature in 60 ~ 80 DEG C, is cooled to room temperature, be freeze-dried to get soil water-retaining
Agent.
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Cited By (1)
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| CN111330652A (en) * | 2020-03-11 | 2020-06-26 | 无锡瑞格生物科技有限责任公司 | Preparation method of monodisperse high-load hydrophilic ion exchange polymethacrylate microspheres |
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| CN111330652A (en) * | 2020-03-11 | 2020-06-26 | 无锡瑞格生物科技有限责任公司 | Preparation method of monodisperse high-load hydrophilic ion exchange polymethacrylate microspheres |
| CN111330652B (en) * | 2020-03-11 | 2023-03-10 | 无锡瑞格生物科技有限责任公司 | Preparation method of monodisperse high-load hydrophilic ion exchange polymethacrylate microspheres |
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