CN102408505B - Method for preparing super absorbent resin by inverse suspension polymerization - Google Patents
Method for preparing super absorbent resin by inverse suspension polymerization Download PDFInfo
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- CN102408505B CN102408505B CN201110307721.3A CN201110307721A CN102408505B CN 102408505 B CN102408505 B CN 102408505B CN 201110307721 A CN201110307721 A CN 201110307721A CN 102408505 B CN102408505 B CN 102408505B
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Abstract
The invention relates to a method for preparing super absorbent resin by inverse suspension polymerization. With a hydrophobic and lipophilic organic substance as the solvent and a proper compound as the dispersant, the method subjects part of a neutralized acrylic acid solution to an inverse suspension polymerization reaction in the presence of a thickening agent, a cross-linking agent as well as a water-soluble initiator, and then employs a surface cross-linking agent for surface cross-linking treatment. The super absorbent resin prepared by the method of the invention has an average particle size of 100-200 micrometers, a saline water adsorption rate of over 45g/g in 1min, and an imbibition speed of less than 20s.
Description
Technical field
The present invention relates to via Inverse-Phase Suspension Polymerization and prepare the method for High hydrophilous resin, say further, relate to the preparation method with the fast High hydrophilous resin of rate of liquid aspiration.
Background technology
High hydrophilous resin is a kind of hydrophilic radicals such as carboxyl that have, and has the water-swellable superpolymer of certain degree of crosslinking, can absorb the extremely water of thousands of times of own wt hundred times.In the last few years, High hydrophilous resin was widely used in the various fields such as agricultural horticultural soil improved materials, cable material water-proof material, anti-condensation material, medical material such as sanitary product material, the water-holding agents such as paper diaper.
The preparation method of High hydrophilous resin mainly contains solution polymerization process and via Inverse-Phase Suspension Polymerization.Solution polymerization process manufacturing process is simple, but product yield is lower, aftertreatment difficulty, and product rate of liquid aspiration is slower.The relative solution polymerization process of via Inverse-Phase Suspension Polymerization has the following advantages: can direct production go out to specify the product of particle diameter, aftertreatment is easy, excellent product performance.
As the example of preparing super absorbent resin by inverse suspension polymerization, disclosed to have the vinylformic acid of take, acrylamide, cationic vinyl monomer be raw material, adopts via Inverse-Phase Suspension Polymerization to synthesize a kind of zwitterionic High hydrophilous resin (CN101012290); Take vinylformic acid, acrylamide is raw material, and hexadecanol phosphatide or stearyl alcohol phosphatide are that dispersion agent is prepared High hydrophilous resin (CN101215354); Take the vinylformic acid of part neutralization and heterogeneous ring compound that methylene radical replaces prepares the super absorbent resin (CN101134793) of fully biodegradable as raw material; Take vinylformic acid as monomer, and hexanaphthene is solvent.Tegin 55G, Arlacel-60 and stearyl alcohol phosphatide are that dispersion agent is prepared polypropylene (salt) High hydrophilous resin (CN1834122) etc.Although people have done a lot of research to inverse suspension polymerization, because inverse suspension polymerization system is unstable, when polymerization, be still easy to occur the phenomenon of implode and caking.Although can prevent by adjusting dispersion agent the generation of implode, but conventionally also can only obtain fine powder or bulk product, being difficult to directly obtain median size is the super absorbent resin fat prod of 100～200 μ m, and the performance of High hydrophilous resin will be affected like this, and then also can be restricted in application.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing super absorbent resin by inverse suspension polymerization, the stability of selecting suitable dispersion agent and thickening material to increase reaction system, strictly controlling polymerization process condition, to control size distribution and the absorptive character of particle be the key of inverse suspension polymerization synthesizing super absorbent resin.
The method of preparing super absorbent resin by inverse suspension polymerization of the present invention, the hydrophobic lipophilicity organism of take is solvent, selecting hydrophile-lipophile balance value (HLB) to be less than 8 compound is dispersion agent, makes the acrylic acid solution generation inverse suspension polymerization reaction of part neutralization at thickening material, linking agent and water soluble starter under the condition existing; Component distillation is sloughed unnecessary moisture afterwards; Then using surface crosslinking agent to carry out surface-crosslinked processing obtains.
The present invention adopts following technical scheme to realize:
A method for preparing super absorbent resin by inverse suspension polymerization, concrete steps are as follows:
1) dispersion agent is added in solvent, in 40～60 ℃ of heating for dissolving;
2) add quantitative vinylformic acid, in ice-water bath, with sodium hydroxide solution neutralization, after neutralization, add thickening material, linking agent and water soluble starter, obtain Acrylic Acid Monomer solution;
3) Acrylic Acid Monomer solution is added in solvent, pass into while stirring nitrogen 30～60 minutes, temperature is increased to 60～80 ℃, react 2～5 hours;
4) after reaction finishes, temperature is increased to 85～95 ℃, carries out azeotropic dehydration;
5) after dehydration finishes, be cooled to 40～60 ℃ and filter, use absolute ethanol washing, at 60～80 ℃, be dried 30～60 minutes;
6) use surface crosslinking agent to carry out surface-crosslinked processing, finally obtain super absorbent resin.
Solvent, should have hydrophobic lipophilicity.From making the stable angle of polymerization system consider, preferred petroleum hydrocarbon compound, Skellysolve A for example, normal hexane, normal heptane, octane, hexanaphthene, cyclooctane and methylcyclohexane one or more.These solvents are preferably used separately.Wherein normal heptane and hexanaphthene are because stable performance is the preferred solvent of the present invention.
The consumption of solvent is generally the 50%-600% of Acrylic Acid Monomer quality, preferably 200%-400%.The amount of solvent is less than 50% of Acrylic Acid Monomer quality, difficult control of temperature, and reaction heat has little time to remove, and the phenomenon of implode and caking easily occurs; Solvent load is more than 600% of Acrylic Acid Monomer quality, and polyreaction is slow, generally can only obtain having the gel of stickiness.
As the dispersion agent of inverse suspension polymerization, from arriving the angle of desirable dispersion effect and protective colloid, the compound that should select hydrophile-lipophile balance value (HLB) to be less than 8.If HLB value is greater than 8, dispersion agent is difficult to play the effect of protective colloid, and implode phenomenon easily occurs during polymerization.Can list as octadecyl phosphoric acid ester, sucrose fatty ester, mono-glycerides, sorbitan fatty acid ester, sorbitan monooleate, anhydrous sorbitol tristearate, ethylene glycol monostearate, Ethylene Glycol Distearate, diethylene glycol monostearate, diethylene glycol bis-stearate, the two stearates of poly(oxyethylene glycol) 400, Macrogol 200 bilaurate, poly(oxyethylene glycol) 400 dioleic acid ester, polyoxyethylene carboxylate, Viscotrol C/hydrogenated castor oil and ethylene oxide condensate, three Polyglycerine list hard fatty acid esters, propylene glycol monostearate, molecular distillation glyceryl monolaurate, one or more of molecule distillating monoglyceride and olein.For this patent, in order to have reached good dispersion effect and to have synthesized the High hydrophilous resin that median size is 100～200 μ m, the mixture of our preferred Tripolyglycerol monostearates and sorbitan tristearate is as dispersion agent.
The consumption of dispersion agent is generally the 0.1%-10% of Acrylic Acid Monomer quality, preferably 0.5%-10%.The ratio of Tripolyglycerol monostearates and sorbitan tristearate is that 1:2～2:1 is advisable.In order to access the narrow product of size distribution, the proportioning of dispersion agent should be strict controlled in aforementioned proportion.
As thickening material, can list Natvosol, hydroxypropylcellulose, methylcellulose gum, carboxymethyl cellulose, polyoxyethylene glycol, polyacrylamide, polyethylene, the polyacrylic acid of part neutralization, partial cross-linked polyacrylic acid etc.Thickening material can regulation system viscosity, can make High hydrophilous resin particle reach required particle size range.In order to achieve the above object, the preferred Natvosol of the present invention, carboxymethyl cellulose, a kind of as thickening material in polyoxyethylene glycol.
The consumption of thickening material is generally 0.01%～5% of Acrylic Acid Monomer quality, and preferably 0.05～1%.The consumption of thickening material, lower than 0.01% of Acrylic Acid Monomer quality, is difficult to play the effect of thickening, and the particle diameter of product is very thin; The consumption of thickening material is higher than 5% of Acrylic Acid Monomer quality, and the viscosity of system is too high, reacts unstable, and the phenomenon of caking easily occurs.
As water soluble starter, can list Potassium Persulphate, Sodium Persulfate, ammonium persulphate, hydrogen peroxide, tertbutyl peroxide, isopropyl benzene hydroperoxide, 2,2'-azo diisobutyl amidine dihydrochloride etc.Due to the restriction of polymerizing condition, do not advise using redox class initiator.From efficiency of initiation, consider the preferred Potassium Persulphate of the present invention.
The consumption of water soluble starter is generally 0.05～3% of Acrylic Acid Monomer quality, is preferable over 0.1～1%.The amount of initiator surpasses 3%, and velocity of initiation is too fast, and the heat of system is not easy to remove, and implode easily occurs; The amount of initiator is lower than 0.05%, and velocity of initiation is excessively slow, and polymerization time can be very long, and product performance can decline to a great extent.
As linking agent, can list ethylene glycol, propylene glycol, glycerol, ethylene glycol diglycidylether, polyethyleneglycol diglycidylether, propanetriol-diglycidyl-ether, one contracting two propanetriol-diglycidyl-ethers, sorbyl alcohol glycidyl ether, N, N'-methylene-bisacrylamide, N-n-methylolacrylamide, EDIA, polyethylene glycol acrylate, propylene glycol acrylate, triallylamine etc.The preferred propylene glycol diglycidylether of the present invention is as linking agent.
The consumption of linking agent is generally 0.01～3% of Acrylic Acid Monomer quality, is preferable over 0.05～1%.The consumption of linking agent is lower than 0.01%, and cross-linkage of resin is very low, has water-soluble; The consumption of linking agent surpasses 3%, and cross-linkage of resin is too high, and water absorbing properties declines.
In the present invention, owing to using Potassium Persulphate, be water soluble starter, polymerization temperature should be controlled at 60～80 ℃ and be advisable.Temperature is lower than 60 ℃, and trigger rate is slow, long reaction time; Temperature is higher than 80 ℃, and trigger rate is too fast, and reaction is difficult to control, and implode easily occurs.Polymerization time is controlled at 2-5 hour, and synthetic like this resin has good performance.
After polyreaction finishes, need carry out component distillation and slough unnecessary moisture, solvent refluxing is to reactor.The object of doing is like this to prevent that gel particle from sticking together in dry process.In the process of azeotropic dehydration, generally to slough more than 90% water of theoretical water content, if water content higher than 10%, particle easily bonds, and affects the effect of surface-crosslinked processing, makes the degradation of product.
From adding dispersion agent to start to finish to azeotropic dehydration, whole process all needs to stir.Stirring velocity is generally at 200～500rpm.
After azeotropic dehydration finishes, be cooled to 40～60 ℃ and filter, use absolute ethanol washing, remove the dispersion agent that sticks to resin surface.At 60～80 ℃, be dried 30～60 minutes.
Surface-crosslinked processing generally can be carried out after dry.As surface crosslinking agent, can list as ethanol, ethylene glycol, Diethylene Glycol, polyoxyethylene glycol, glycerol, polyglycerol, Virahol, 1,4-butyleneglycol, diethanolamine, trolamine, polyethenoxy ether, ethylene glycol diglycidylether, polyethyleneglycol diglycidylether, glycerol diglycidylether,, one contracting two propanetriol-diglycidyl-ethers, vinyl alcohol diglycidylether, epoxy chloropropane, quadrol, diethylenetriamine, triethylene tetramine, aluminum chloride, magnesium chloride, calcium chloride, Tai-Ace S 150, magnesium sulfate, calcium sulfate etc.In order to obtain good surface-crosslinked effect, at least one of preferred alcohol of the present invention, propylene glycol, glycerol, Virahol, vinyl alcohol diglycidylether.
The consumption of surface crosslinking agent, is used 0.5～30 part with respect to the resin of 100 parts of quality, preferably 1～20 part.The amount of surface crosslinking agent is less than 0.5 part, and cross-linking effect is not obvious; The amount of surface crosslinking agent is higher than 30 parts, and High hydrophilous resin forms fine and close upper layer, and water-retaining capacity declines.
Surface-crosslinked temperature is generally determined according to the surface crosslinking agent using.The surface crosslinking agent using according to the present invention, general 70～200 ℃ of surface-crosslinked temperature, preferably 80～150 ℃.The surface-crosslinked time is generally 0.5～1 hour.
The method of preparing super absorbent resin by inverse suspension polymerization of the present invention, the High hydrophilous resin median size making is 100～200 μ m.Resin 1min absorption salt ratio is more than 45g/g, and rate of liquid aspiration is in 20s.
The testing method of High hydrophilous resin of the present invention is as follows:
(1) median size
By JIS standard sieve by upper beginning according to 830 μ m(20 orders), 550 μ m(30 orders), 270 μ m(50 orders), 180 μ m(80 orders) 150 μ m(100 orders), 106 μ m(150 orders), 75 μ m(200 orders) sequential combination, on the sieve of the superiors, put into High hydrophilous resin 100g left and right, use laboratory sifter screening 20 minutes.Then, the High hydrophilous resin in 6 screen clothes of the 2nd screen cloth to the is counted to heavy (particles above due to 830 μ m and below 106 μ m are less and using value is not high, therefore not at the row of statistics), its weight is respectively A
2, A
3, A
4, A
5, A
6.Calculate according to the following formula the median size of High hydrophilous resin:
(2) water-intake rate
In the beaker of 2L, pour the deionized water of 1000mL into.Accurately take 0.2g High hydrophilous resin, pack into after Nylon Bag, be soaked in deionized water.After 1 hour, Nylon Bag is hung to liquid level, naturally drip 10 minutes, claim that now total mass is M
1.Use does not have the Nylon Bag of sample to carry out blank assay simultaneously, and the quality that takes blank Nylon Bag is M
2.Water-intake rate is calculated as follows:
(3) absorption salt ratio
In 1000ml beaker, pour the physiological saline of 500ml0.9% into.Accurately take 0.2g High hydrophilous resin, pack into after tea-bag, be soaked in 0.9% physiological saline.After 30 minutes, the tea-bag that sample is housed is brought out, under stationary state, drip 10 minutes, claim that now total mass is W
1.Use does not have the tea-bag of sample to carry out blank assay simultaneously, and the quality that takes blank tea-bag is W
2.Absorption salt ratio is calculated as follows:
(4) 1 minutes absorption salt ratios
In 1000ml beaker, pour the physiological saline of 500ml0.9% into.Accurately take 0.2g High hydrophilous resin, pack into after tea-bag, be soaked in 0.9% physiological saline.After 1 minute, the tea-bag that sample is housed is brought out, under stationary state, drip 10 minutes, claim that now total mass is W
1.Use does not have the tea-bag of sample to carry out blank assay simultaneously, and the quality that takes blank tea-bag is W
2.1 minute absorption salt ratio is pressed absorption salt ratio formula and is calculated.
(5) rate of liquid aspiration
In the 100mL beaker with rotor, pack 0.9% physiological saline 50g into, beaker is placed on magnetic stirrer, with the speed of 600 revs/min, stirs, accurately take the polymer of 2.0g, put in whirlpool, with stopwatch, start timing, when whirlpool disappears, when liquid level becomes horizontality simultaneously, as terminal, record its time.
More than test is all carried out in the time of 25 ℃.
Embodiment
Embodiment 1: 342.5g normal heptane is joined in five mouthfuls of round-bottomed flasks of 1L that agitator, reflux exchanger, dropping funnel, thermometer and nitrogen inlet tube are housed.Add wherein 0.75g Tripolyglycerol monostearates and 0.85g sorbitan tristearate, be warming up to 50 ℃, with the stirring velocity of 350rpm, make it dispersed.
By 130 g mass concentrations, be 75%(wt%) acrylic acid aqueous solution join in 500 ml erlenmeyer flasks.130.2g32 wt% aqueous sodium hydroxide solution is added drop-wise in this erlenmeyer flask.Then, add wherein 0.5g Potassium Persulphate, 0.2g propylene glycol diglycidylether, 0.12g Natvosol, obtains the Acrylic Acid Monomer aqueous solution.
This Acrylic Acid Monomer aqueous solution is joined in above-mentioned five mouthfuls of round-bottomed flasks, pass into while stirring nitrogen 30～60 minutes.Then by warming-in-water to 75 ℃, react 3 hours.After reaction finishes, temperature continues to rise to 92 ℃ and carries out azeotropic dehydration, removes altogether 110g water.Temperature is cooled to 50 ℃ and filters, use absolute ethanol washing, at 60～80 ℃, be dried 30～60 minutes.
4.4g ethanol, 3.2g Virahol, 0.4g vinyl alcohol diglycidylether are mixed, be sprayed onto uniformly the above-mentioned resin surface of 100g, in the baking oven of 140 ℃, surface-crosslinked processing is 50 minutes, obtains the High hydrophilous resin of white granular.
Embodiment 2: except changing the consumption of Tripolyglycerol monostearates and sorbitan tristearate into 0.9g and 0.7g, stirring velocity are adjusted into 380rpm, other operate with embodiment 1.
Embodiment 3: 380g hexanaphthene is joined in five mouthfuls of round-bottomed flasks of 1L that agitator, reflux exchanger, dropping funnel, thermometer and nitrogen inlet tube are housed.Add wherein 0.7g Tripolyglycerol monostearates and 0.7g sorbitan tristearate, be warming up to 50 ℃, with the stirring velocity of 320rpm, make it dispersed.
The acrylic acid aqueous solution of 130 g 75wt% is joined in 500 ml erlenmeyer flasks.130.2g32 wt% aqueous sodium hydroxide solution is added drop-wise in this erlenmeyer flask.Then, add wherein 0.45g Potassium Persulphate, 0.015g propylene glycol diglycidylether, 0.1g Natvosol, obtains the Acrylic Acid Monomer aqueous solution.
This Acrylic Acid Monomer aqueous solution is joined in above-mentioned five mouthfuls of round-bottomed flasks, pass into while stirring nitrogen 30～60 minutes.Then by warming-in-water to 70 ℃, react 3.5 hours.After reaction finishes, temperature continues to rise to 88 ℃ and carries out azeotropic dehydration, removes altogether 110g water.Temperature is cooled to 50 ℃ and filters, use absolute ethanol washing, at 60～80 ℃, be dried 30～60 minutes.
4.4g ethanol, 3.2g Virahol, 0.4g vinyl alcohol diglycidylether are mixed, be sprayed onto uniformly the above-mentioned resin surface of 100g, in the baking oven of 140 ℃, surface-crosslinked processing is 50 minutes, obtains the High hydrophilous resin of white granular.
Embodiment 4: except changing the consumption of Tripolyglycerol monostearates and sorbitan tristearate into 0.85g and 0.55g, stirring velocity are adjusted into 360rpm, other operate with embodiment 3.
Embodiment 5: 342.5g normal heptane is joined in five mouthfuls of round-bottomed flasks of 1L that agitator, reflux exchanger, dropping funnel, thermometer and nitrogen inlet tube are housed.Add wherein 0.7g Tripolyglycerol monostearates and 0.9g sorbitan tristearate, be warming up to 50 ℃, with the stirring velocity of 400rpm, make it dispersed.
The acrylic acid aqueous solution of 130 g 75wt% is joined in 500 ml erlenmeyer flasks.130.2g32 wt% aqueous sodium hydroxide solution is added drop-wise in this erlenmeyer flask.Then, 0.5g Potassium Persulphate, 0.2g propylene glycol diglycidylether wherein, 0.1g Walocel MT 20.000PV, obtains the Acrylic Acid Monomer aqueous solution.
This Acrylic Acid Monomer aqueous solution is joined in above-mentioned five mouthfuls of round-bottomed flasks, pass into while stirring nitrogen 30～60 minutes.Then by warming-in-water to 76 ℃, react 2.5 hours.After reaction finishes, temperature continues to rise to 92 ℃ and carries out azeotropic dehydration, removes altogether 110g water.Temperature is cooled to 50 ℃ and filters, use absolute ethanol washing, at 60～80 ℃, be dried 30～60 minutes.
4.4g ethanol, 1.2g propylene glycol, 0.6g glycerol, 0.4g vinyl alcohol diglycidylether are mixed, be sprayed onto uniformly the above-mentioned resin surface of 100g, in the baking oven of 150 ℃, surface-crosslinked processing is 40 minutes, obtains the High hydrophilous resin of micro-yellow particle shape.
Embodiment 6: 380g hexanaphthene is joined in five mouthfuls of round-bottomed flasks of 1L that agitator, reflux exchanger, dropping funnel, thermometer and nitrogen inlet tube are housed.Add wherein 0.8g Tripolyglycerol monostearates and 0.8g sorbitan tristearate, be warming up to 50 ℃, with the stirring velocity of 390rpm, make it dispersed.
The acrylic acid aqueous solution of 130 g 75wt% is joined in 500 ml erlenmeyer flasks.130.2g32 wt% aqueous sodium hydroxide solution is added drop-wise in this erlenmeyer flask.Then, add wherein 0.5g Potassium Persulphate, 0.02g propylene glycol diglycidylether, 0.1g Walocel MT 20.000PV, obtains the Acrylic Acid Monomer aqueous solution.
This Acrylic Acid Monomer aqueous solution is joined in above-mentioned five mouthfuls of round-bottomed flasks, pass into while stirring nitrogen 30～60 minutes.Then by warming-in-water to 72 ℃, react 3 hours.After reaction finishes, temperature continues to rise to 88 ℃ and carries out azeotropic dehydration, removes altogether 110g water.Temperature is cooled to 50 ℃ and filters, use absolute ethanol washing, at 60～80 ℃, be dried 30～60 minutes.
4.4g ethanol, 1.2g propylene glycol, 0.6g glycerol, 0.4g vinyl alcohol diglycidylether are mixed, be sprayed onto uniformly the above-mentioned resin surface of 100g, in the baking oven of 150 ℃, surface-crosslinked processing is 40 minutes, obtains the High hydrophilous resin of micro-yellow particle shape.
Comparative example 1: except only using 1.5g sorbitan tristearate as dispersion agent, other operate with embodiment 1.Obtain white oarse-grained High hydrophilous resin.
Comparative example 2: except not adding Natvosol, other operate with embodiment 1, obtain the High hydrophilous resin of white powder.
The performance test of the High hydrophilous resin obtaining in table 1 embodiment and comparative example
| ? | Outward appearance | Median size (μ m) | Water-intake rate (g/g) | Absorption salt ratio (g/g) | 1 minute absorption salt ratio (g/g) | Rate of liquid aspiration (s) |
| Embodiment 1 | White particle | 290 | 360 | 58 | 48 | 18 |
| Embodiment 2 | White particle | 230 | 345 | 54 | 45 | 14 |
| Embodiment 3 | White particle | 274 | 420 | 60 | 46 | 16 |
| Embodiment 4 | White particle | 216 | 380 | 58 | 45 | 12 |
| Embodiment 5 | Micro-yellow particle | 180 | 330 | 56 | 48 | 8 |
| Embodiment 6 | Micro-yellow particle | 168 | 345 | 56 | 50 | 7 |
| Comparative example 1 | White particle | 500 | 280 | 52 | 21 | 65 |
| Comparative example 2 | White powder | 90 | 250 | 43 | 40 | 5 |
From the test result of table 1, the High hydrophilous resin obtaining in embodiment 1-6, median size, between 150-300 μ m, has moderate water-intake rate and absorption salt ratio, faster rate of liquid aspiration.On the other hand, only use sorbitan tristearate to make dispersion agent, grain diameter is thicker, and rate of liquid aspiration is slow; Do not use thickening material, particle diameter is partially thin, affects its use value.
Claims (9)
1. a method for preparing super absorbent resin by inverse suspension polymerization, is characterized in that
1) take hydrophobic lipophilicity organism is solvent, and the 0.1%-10% dispersion agent that is Acrylic Acid Monomer quality by consumption adds in solvent, in 40～60 ℃ of heating for dissolving;
2) add quantitative vinylformic acid, in ice-water bath, with sodium hydroxide solution neutralization, after neutralization, adding consumption is 0.01%～5% thickening material, linking agent and the water soluble starter of Acrylic Acid Monomer quality, obtains Acrylic Acid Monomer solution;
3) Acrylic Acid Monomer solution is added in solvent, pass into while stirring nitrogen 30～60 minutes, temperature is increased to 60～80 ℃, react 2～5 hours;
4) after reaction finishes, temperature is increased to 85～95 ℃, carries out azeotropic dehydration;
5) after dehydration finishes, be cooled to 40～60 ℃ and filter, use afterwards absolute ethanol washing, then at 60～80 ℃, be dried 30～60 minutes;
6) use surface crosslinking agent to carry out surface-crosslinked processing, finally obtain super absorbent resin;
Described dispersion agent be take Tripolyglycerol monostearates and the sorbitan tristearate that ratio is 1: 2～2: 1 and is formed;
Described thickening material is selected from one or more of Natvosol, hydroxypropylcellulose, methylcellulose gum and carboxymethyl cellulose.
2. the method for preparing super absorbent resin by inverse suspension polymerization according to claim 1, it is characterized in that described solvent is selected from Skellysolve A, normal hexane, normal heptane, octane, hexanaphthene, cyclooctane and methylcyclohexane one or more, consumption is the 50%-600% of described Acrylic Acid Monomer quality.
3. the method for preparing super absorbent resin by inverse suspension polymerization according to claim 1, is characterized in that described water soluble starter is Potassium Persulphate, and consumption is 0.05～3% of Acrylic Acid Monomer quality.
4. the method for preparing super absorbent resin by inverse suspension polymerization according to claim 1, it is characterized in that described linking agent is selected from ethylene glycol, propylene glycol, glycerol, ethylene glycol diglycidylether, polyethyleneglycol diglycidylether, propanetriol-diglycidyl-ether, one contracting two propanetriol-diglycidyl-ethers, sorbyl alcohol glycidyl ether, N.N '-methylene-bisacrylamide, N hydroxymethyl acrylamide, EDIA, polyethylene glycol acrylate, one or more of propylene glycol acrylate and triallylamine, consumption is 0.01～3% of Acrylic Acid Monomer quality.
5. the method for preparing super absorbent resin by inverse suspension polymerization according to claim 1, is characterized in that described inverse suspension polymerization temperature of reaction is 60～80 ℃, and the time is 2-5 hour.
6. the method for preparing super absorbent resin by inverse suspension polymerization according to claim 1, it is characterized in that described surface crosslinking agent is selected from ethanol, ethylene glycol, Diethylene Glycol, polyoxyethylene glycol, glycerol, polyglycerol, Virahol, 1, 4-butyleneglycol, diethanolamine, trolamine, polyethenoxy ether, ethylene glycol diglycidylether, epoxy chloropropane, quadrol, diethylenetriamine, triethylene tetramine, aluminum chloride, magnesium chloride, calcium chloride, Tai-Ace S 150, one or more of magnesium sulfate and calcium sulfate, consumption is used 0.5～30 part with respect to the resin of 100 parts of quality.
7. the method for preparing super absorbent resin by inverse suspension polymerization according to claim 1, is characterized in that 70～200 ℃ of described surface-crosslinked temperature, and the time is 0.5-1 hour.
8. the method for preparing super absorbent resin by inverse suspension polymerization according to claim 1, the described High hydrophilous resin median size making is 100～200 μ m.
9. the method for preparing super absorbent resin by inverse suspension polymerization according to claim 1, the described High hydrophilous resin 1min absorption salt ratio making is more than 45g/g, and rate of liquid aspiration is in 20s.
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