CN108610459A - A kind of preparation method of quick absorption-type super absorbent resin - Google Patents
A kind of preparation method of quick absorption-type super absorbent resin Download PDFInfo
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- CN108610459A CN108610459A CN201810494164.2A CN201810494164A CN108610459A CN 108610459 A CN108610459 A CN 108610459A CN 201810494164 A CN201810494164 A CN 201810494164A CN 108610459 A CN108610459 A CN 108610459A
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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
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
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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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
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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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
Abstract
The present invention relates to a kind of preparation methods of quick absorption-type super absorbent resin, acrylic acid and quantitative water are added in a kettle, lye progress neutralization reaction is added, it is separately added into crosslinking agent, foaming agent, wood fibre, polyethylene glycol, add toner, initiator and reducing agent through crushing and screening 100 mesh of ＞, it is foam colloid after polymerisation, by chopping, granulation, drying, crushing, screening, by surface-crosslinked processing, quick absorption-type super absorbent resin is made.Invention introduces composite foamable agent, improve foaming effect, wood fibre is added, improve water-retaining property and permeability, add stabilization and gel strength that polyethylene glycol improves colloidal foam with toner, special installation need not be increased in production process, the generation of production by-product is also reduced simultaneously, and the absorption rate, water-retaining property, performance indicator for effectively increasing product are more balanced, shorten drying time, improve production efficiency, are conducive to amplification production.
Description
Technical field
The present invention relates to a kind of preparation methods of super absorbent resin, concretely relate to a kind of quick absorption-type height suction
The preparation method of water-base resin.
Background technology
Super absorbent resin (super absorbent polymer SAP), is to have good absorbent and water conservation
The general name of the high molecular polymer of performance is can absorb because of the ability with the hundred times or even thousands of times of water for absorbing own wt
The physiological saline (0.9% sodium chloride) of tens times or even hundreds of times, and water-retaining property is high, so widely used.With society
Development, the raising of people’s lives level, domestic and international expert, scholar to the synthesis and application of super absorbent resin, done largely
Waterproofing agent, drier, extinguishing chemical, agricultural water-retaining agent, conditioning agent, fertilizer corrosion inhibiter etc. are industrially done in research and development, special
It is not that Acrylates super absorbent resin is had into more application and development in health field, such as：Sweat towel, blotting paper, patient
Diaper, diaper, protection pad, paper diaper, sanitary napkin etc. are it may be said that an indispensable part in having become for people's lives.So high
The research of water-absorbing resins has extensive foreground with production.
The production method of super absorbent resin mainly has：Suspension polymerization, emulsion polymerization, inverse suspension polymerization and reverse phase
Suspension precipitation polymerization method, water solution polymerization process etc., comparative maturity, aqueous solution are poly- with production for the research of super absorbent resin at present
It is legal to have：Belt polymerization, tunnel type polymerization, disk type polymerism method, dry and spray polymerization seasoning etc. of transferring shares can be achieved, China is high
The production of water-absorbing resins is mainly based on Acrylates aqua-solution method, and superabsorbent polyacrylate resin is most suitable for
The application in terms of hygienic material is done, therefore the raising of development and production Acrylates super absorbent resin main performance index is particularly
It is important：There are preferable water absorbing properties, especially to have the characteristics of quick absorption.
It is industrial at present generally to be deposited based on crosslinked salt polyacrylate using aqueous solution polymerization production super absorbent resin
Water absorbing properties are unbalanced, the faster product uptake of rate of water absorption is low, poor water retention property, have perhaps in super absorbent resin field
Multi-expert, scholar are that can produce the product haveing excellent performance and be made that very big contribution, so there is many methods for high suction at present
The performance improvement of water-base resin, such as the structure of design super absorbent resin, introducing carbonate or bicarbonate formation foaming are more
Hole etc., and it is unstable for product poor water retention property, performance, and amplification production has the problems such as certain difficulty, introduces polyvinyl alcohol sulfonic acid
Sodium make super absorbent resin formed inierpeneirating network structure method, can solve improve water-absorbing resins correlated performance, but by
It is complicated in the synthesis technology of the substance polyvinyl alcohol sodium sulfonate of introducing, therefore amplify production difficulty, it is unfavorable in these processes
Industrialized production.
Invention content
Of the existing technology in order to overcome the problems, such as, the present invention provides a kind of simple for process, good water-retaining property, performances to stablize
Quick absorption-type super absorbent resin preparation method.
A kind of preparation method of quick absorption-type super absorbent resin, includes the following steps：
(1) acrylic acid, water, lye are added in the reactor and obtain liquid to be polymerized after being reacted；
(2) crosslinking agent, composite foamable agent, wood fibre, polyethylene glycol, resin-oatmeal are separately added into above-mentioned liquid to be polymerized
End, initiator carry out polymerisation；
(3) jello is by obtaining bladdery particle in irregular after polymerizeing after shredding, be granulated, dry, crush, screening
Powdex；
(4) quick absorption-type high-hydroscopicity tree is made in above-mentioned particle powder resin after surface treatment liquid cross-linking reaction
Fat.
Invention introduces composite foamable agents, improve foaming effect；The substance wood fibre of good hydrophilic property is added, improves and protects
Aqueous and permeability；Add stabilization and gel strength that polyethylene glycol improves colloidal foam with toner；In production process not
It needs to increase special installation, because polyethylene glycol and toner is added, foam granulating from colloid is unaffected, while also reducing life
The generation of by-product is produced, the absorption rate, water-retaining property, performance indicator for effectively increasing product are more balanced, shorten drying time, carry
High efficiency is conducive to amplification production.
Preferably, in step (1), the alkali in lye is sodium hydroxide, potassium hydroxide, ammonium hydroxide, sodium carbonate, bicarbonate
The arbitrary combination of one or two or more kinds in sodium, ammonium carbonate, ammonium hydrogen carbonate.
Preferably, in step (1), acrylic acid mass concentration is 30%~45% in liquid to be polymerized.
In liquid to be polymerized acrylic acid mass concentration be less than 30% when, active quantities are low, consumption of calorie is fast, polymerization time too
It is long, polymerization chain termination is easy tod produce, gel strength reduces, and level of residual monomers is high；When higher than 45%, reaction solution concentration is excessively high, gathers
It closes heat and is not easy the polymerization high fever that sheds, instantaneously reaches, production is difficult to control, and the big index of product solubility is unstable.
Preferably, in step (2), the crosslinking agent is epoxy resin, epoxychloropropane, polyethylene glycol diglycidyl
The arbitrary combination of one or two or more kinds in ether, N, N- methylene-bisacrylamide, polyethyleneglycol diacrylate, dosage are
The 0.005%~0.5% of acrylic acid quality.
Certain density crosslinking agent can make water absorbing properties stable, insoluble, can be with compound more than difunctional：
Epoxy resin, epoxychloropropane, polyethyleneglycol diglycidylether；Or there are two double bond unsaturated monomers for band：N, N- methylene
Bisacrylamide or polyethyleneglycol diacrylate (PEGnDA) are that crosslinking agent or the one or two kinds of of them are used in combination, and are added
The preferable dosage of dosage is 0.01%~0.2%.It when additive amount is low, is not easy to form tridimensional network, the degree of cross linking is low, gel strength
Low, resolvability is big；When dosage is big, crosslink density is big, cyberspace is small, influences water swelling, reduces water absorbing capacity, loses height
Water absorbing properties.
Preferably, the composite foamable agent by foam microspheres powder with sodium bicarbonate powder is compound forms, dosage third
The 1.0%~7.0% of olefin(e) acid quality.
Composite foamable agent can improve the specific surface area of water-absorbing resins or reduce resin particle density, can improve product
Absorption rate：It is composite foamed with sodium bicarbonate powder using foam microspheres powder (F-36 or WU-140), it reduces grain density and increases
Specific surface area, dosage is more, and product becomes fragile, the small water-retaining property of density reduces, preferable dosage be acrylic acid quality 2.0%~
4.2%.
Preferably, the wood fibre dosage is the 0.2%~10% of acrylic acid quality.Suitable high-hydrophilic is added
Wood fibre is conducive to increase water-retaining property, the excessive water-retaining property of additive amount reduces instead, bleeds back quickening, and the small effect of dosage is unknown
Aobvious, preferable dosage is the 0.5%~2% of acrylic acid quality.
Preferably, the polyethylene glycol dosage is the 0.03%~0.3% of acrylic acid quality, the mesh of the toner
>=100 mesh of number, dosage are the 4%~20% of acrylic acid quality.Addition polyethylene glycol can improve colloidal foam with toner
Stability.
Preferably, the initiator is the composite initiator that azo-initiator is formed with persulfate, hydrogen peroxide,
The reducing agent is sodium sulfite or sodium hydrogensulfite, and initiator amount is the 0.06%~0.6% of acrylic acid quality, reducing agent
Dosage is the 0.02%~0.3% of acrylic acid quality.
The present invention uses combined oxidation reduction initiating system, azo-initiator 2,2'- azo diisobutyl amidine disalts
Hydrochlorate (V-50 initiators), the initiator added in polymerisation in solution：Persulfate (sylvite, sodium salt, ammonium salt etc.), mistake may be used
Redox initiator, persulfate-sodium sulfite or sodium hydrogensulfite can also be used in hydrogen oxide, can also use azo
Initiator or composite initiator etc., because using composite initiation system, stable polymerization reaction, the stabilization for being conducive to properties of product.
Preferably, in step (3), 80 DEG C~130 DEG C of dry environment temperature, 2~12 hours drying times, sieving screening
40~100 mesh materials.
Preferably, in step (4), surface treatment liquid is by water, aluminum sulfate, methanol or ethyl alcohol, ethylene glycol diglycidyl
Ether, glycerine composition, the aluminum sulfate, deionization, methanol or ethyl alcohol, ethylene glycol diglycidylether, glycerine mass ratio be 1：5
~15：1~9：0.01~0.3：0.1~1.0；Cross-linking reaction temperature is 50 DEG C~110 DEG C, and the reaction time is 20~80min, instead
It should 5~10min of rear re-dry dehumidifying.
Micelle that jello after polymerization is shredded into 4~6mm of Φ, by drying, is ground into granulated powder, dry
Material afterwards is through crushing, screening granulated powder, and after being sieved by 40~100 mesh, powdex is added in mixing reactor,
Above treatment fluid addition is quickly mixed evenly again, 50 DEG C~110 DEG C is heated, reacts 20~80min, re-dry
Dehumidify 5~10min, water-absorbing resin after this method is handled, be effectively reduced level of residual monomers, improve gel strength, water suction
Balancing performance, absorption speed are fast.
The present invention makees auxiliary agent using combined foaming and high-hydrophilic object, and wood fibre, which is utilized, has irregular gap
Feature improves hydrophily and water-retaining property performance, and polymerisation efficiency is improved by composite initiation system, it is made to polymerize steady, hair
Bubble is uniform, changes Super Absorbent Polymer Particles form and increases specific surface area, the present invention can make super absorbent resin performance indicator equal
Weighing apparatus improves rate of water absorption, has the characteristics that simple for process, easy to operate, energy saving, efficient, suitable industrialized production.
Specific implementation mode
The present invention is further explained in the light of specific embodiments, but invention which is intended to be protected is not limited to
This.
Water absorbent rate measures：
Be added in beaker 500ml pure water, weigh 0.3g super absorbent resins be added in beaker of water, after timing 30min, fall
Enter 15min in 100 mesh or 200 mesh nets loan and filter off moisture, then weighs gel weight W, calculates the water suction of resin with following equation
Multiplying power Q, unit g/g：
Q=(W-0.3)/0.3
1min Water uptake measurements：
Set puts 100 mesh or 200 mesh mesh bags in 500ml beakers, and 500ml pure water is added, weighs 1.0g high-hydroscopicity trees
Fat is added in beaker of water, timing 1.0min, immediately carried mesh bag, hang 2min, elimination moisture, then weighing gel weight W,
Resin, the water absorbent rate Q of 1min, unit g/g are calculated with following equation：
Q=W-1.0
The measurement (swirl method) of rate of water absorption
It weighs 2.0gSAP (being accurate to 0.01g) and 100ml beakers is added 50g physiological saline (0.9%), puts into rotor
It in brine, is placed on magnetic stirring apparatus, rotating speed is set as 1400rpm.2.00gSAP is put into brine rapidly, while being pressed immediately
Lower stopwatch starts timing, when rotor disappears in brine whirlpool in beaker, the time required to writing down, as inhales brine rate.
Inhale 0.9% brine multiplying power measurement
Test method is measured according to 0.9% brine multiplying power is inhaled in GB/T22875-2008.
The measurement of water-retaining property
Test method according to water holding capacity in GB/T22905-2008 measurement.
Embodiment 1
Acrylic acid, the deionized water 70g of 100g are added in the 1000ml there-necked flasks with stirring, there-necked flask is put into and is added
Have in the water termostat water-bath of cold water, install constant pressure addition funnel, be inserted into thermometer, the sodium hydroxide for weighing 32wt% is molten
Liquid is added in dropping funel, starts stirring, lye neutralization is added dropwise, and depending on controlling neutralization reaction temperature, temperature is controlled at 42 DEG C
Hereinafter, obtaining the liquid to be polymerized of degree of neutralization 75%, monomer concentration 41% after neutralizing.
It is separately added into N, N '-methylene-bisacrylamides (MBA) aqueous solution 1.1g (MBA concentration 2wt%), foaming agent：F-
36+NaHCO3(0.6 ﹕ 2.0) 2.6g, wood fibre 1.0g, polyethylene glycol 0.15g, then add >=100 mesh toner 10g, fully
Dispersion swelling 15min, keeps 41~42 DEG C of temperature.
It is added 2,2'- azo diisobutyl amidine dihydrochloride (initiator V-50) aqueous solutions 3.5g, 2wt%'s of 3wt%
Sodium persulfate aqueous solution 3.5g stirs evenly, is added the aqueous solution of sodium bisulfite 4g of 1.5wt%, pours into plastic reactor
Polymerisation.
Foam after polymerization colloid is shredded with scissors, is granulated with electrical meat mincer, and band air blast and micro- induced air type drying box are dried,
120 DEG C of drying temperature, 2.5h, grinding and sieving screen 40~100 mesh, obtain bladdery particle powder resin in irregular.
Treatment fluid：Water 6.0g, ethyl alcohol 3.0g, aluminum sulfate 1.0g, ethylene glycol diglycidylether 0.030g, glycerine 0.50g,
It is for use after dissolving mixing.100g powder particle resins are put into container, the treatment fluid prepared is added and is uniformly mixed,
Cross-linking reaction, heat preservation 60min, 100 DEG C of dry 6min, obtain quick absorption-type super absorbent resin at 100 DEG C.
Test result is shown in Table 1.
Embodiment 2
Acrylic acid, the deionized water 70g of 100g are added in the 1000ml there-necked flasks with stirring, there-necked flask is put into and is added
Have in the water termostat water-bath of cold water, install constant pressure addition funnel, be inserted into thermometer, weighs the sodium hydroxide of 32wt%, adds
Enter in dropping funel, start stirring, be added dropwise lye neutralize, depending on controlling neutralization reaction temperature, temperature control at 42 DEG C hereinafter,
The liquid to be polymerized of degree of neutralization 75%, monomer concentration 41% is obtained after neutralization.
After neutralization, it is separately added into polyethyleneglycol diacrylate (PEGDA) 5wt% aqueous solutions 1.3g, foaming agent：F-36+
NaHCO3(1.0 ﹕ 1.0) 2.0g, wood fibre 1.0g, polyethylene glycol 0.15g, then add >=100 mesh toner 10g, fully divide
Swelling 15min is dissipated, 41~42 DEG C of temperature is kept.
The mistake of 2,2'- azo diisobutyl amidine dihydrochloride (initiator V-50) aqueous solutions 5g, 2wt% of 3wt% is added
Aqueous sodium persulfate solution 5g stirs evenly, is added the aqueous solution of sodium bisulfite 5g of 1.5wt%, pours into plastic reactor and polymerize
Reaction.
Foam after polymerization colloid is shredded with scissors, is granulated with electrical meat mincer, and band air blast and micro- induced air type drying box are dried,
120 DEG C of drying temperature, 2.5h, grinding and sieving screen 40~100 mesh, obtain bladdery particle powder resin in irregular.
Treatment fluid：Water 6.0g, ethyl alcohol 3.0g, aluminum sulfate 1.0g, ethylene glycol diglycidylether 0.030g, glycerine 0.50g,
It is for use after dissolving mixing.100g powder particle resins are put into container, the treatment fluid prepared is added and is uniformly mixed,
Cross-linking reaction, heat preservation 60min, 100 DEG C of dry 6min, obtain quick absorption-type super absorbent resin at 100 DEG C.
Embodiment 3
Acrylic acid, the deionized water 70g of 100g are added in the 1000ml there-necked flasks with stirring, there-necked flask is put into and is added
Have in the water termostat water-bath of cold water, install constant pressure addition funnel, be inserted into thermometer, weighs the sodium hydroxide of 32wt%, adds
Enter in dropping funel, start stirring, be added dropwise lye neutralize, depending on controlling neutralization reaction temperature, temperature control at 42 DEG C hereinafter,
The liquid to be polymerized of degree of neutralization 75%, monomer concentration 41% is obtained after neutralization.
After neutralization, it is separately added into polyethyleneglycol diacrylate (PEGDA) 5wt% aqueous solutions 1.3g, foaming agent：F-36+
NaHCO3(0.2 ﹕ 4.0) 4.2g, wood fibre 1.0g, polyethylene glycol 0.15g, then add >=100 mesh toner 10g, fully divide
Swelling 15min is dissipated, 41~42 DEG C of temperature is kept, 2,2'- azo diisobutyl amidine dihydrochlorides (the initiator V- of 3wt% is added
50) the sodium persulfate aqueous solution 2g of aqueous solution 5g, 2wt% stirs evenly, is added the aqueous solution of sodium bisulfite 4g of 1.5wt%,
Pour into polymerisation in plastic reactor.
Foam after polymerization colloid is shredded with scissors, is granulated with electrical meat mincer, and band air blast and micro- induced air type drying box are dried,
120 DEG C of drying temperature, 2.5h, grinding and sieving screen 40~100 mesh, obtain bladdery particle powder resin in irregular.
Treatment fluid：Water 6.0g, ethyl alcohol 3.0g, aluminum sulfate 1.0g, ethylene glycol diglycidylether 0.030g, glycerine 0.50g,
It is for use after dissolving mixing.100g powder particle resins are put into container, the treatment fluid prepared is added and is uniformly mixed,
Cross-linking reaction, heat preservation 60min, 100 DEG C of dry 6min, obtain quick absorption-type super absorbent resin at 100 DEG C.
Embodiment 4
Acrylic acid, the deionized water 70g of 100g are added in the 1000ml there-necked flasks with stirring, there-necked flask is put into and is added
Have in the water termostat water-bath of cold water, install constant pressure addition funnel, be inserted into thermometer, weighs the sodium hydroxide of 32wt%, adds
Enter in dropping funel, start stirring, be added dropwise lye neutralize, depending on controlling neutralization reaction temperature, temperature control at 42 DEG C hereinafter,
The liquid to be polymerized of degree of neutralization 75%, monomer concentration 41% is obtained after neutralization.
After neutralization, it is separately added into polyethyleneglycol diacrylate (PEGDA) 5wt% aqueous solutions 1.3g, foaming agent：F-36+
NaHCO3(0.6 ﹕ 2.0) 2.6g, wood fibre 5.0g, polyethylene glycol 0.2g, then add >=100 mesh toner 20g fully dispersed
It is swollen 15min, keeps 41~42 DEG C of temperature.
The mistake of 2,2'- azo diisobutyl amidine dihydrochloride (initiator V-50) aqueous solutions 5g, 2wt% of 3wt% is added
Aqueous sodium persulfate solution 2g stirs evenly, is added the aqueous solution of sodium bisulfite 4g of 1.5wt%, pours into plastic reactor and polymerize
Reaction, foam after polymerization colloid are shredded with scissors, are granulated with electrical meat mincer, and band air blast and micro- induced air type drying box are dried, and are done
120 DEG C of dry temperature, 2.5h, grinding and sieving screen 40~100 mesh, obtain bladdery particle powder resin in irregular.
Treatment fluid：Water 6.0g, ethyl alcohol 3.0g, aluminum sulfate 1.0g, ethylene glycol diglycidylether 0.030g, glycerine 0.50g,
It is for use after dissolving mixing.100g powder particle resins are put into container, the treatment fluid prepared is added and is uniformly mixed,
Cross-linking reaction, heat preservation 60min, 100 DEG C of dry 6min, obtain quick absorption-type super absorbent resin at 100 DEG C.
Embodiment 5
Acrylic acid, the deionized water 70g of 100g are added in the 1000ml there-necked flasks with stirring, there-necked flask is put into and is added
Have in the water termostat water-bath of cold water, install constant pressure addition funnel, be inserted into thermometer, weighs the sodium hydroxide of 32wt%, adds
Enter in dropping funel, start stirring, be added dropwise lye neutralize, depending on controlling neutralization reaction temperature, temperature control at 42 DEG C hereinafter,
The liquid to be polymerized of degree of neutralization 75%, monomer concentration 41% is obtained after neutralization.
After neutralization, it is separately added into polyethyleneglycol diacrylate (PEGDA) 5wt% aqueous solutions 0.9g, foaming agent：F-36+
NaHCO3(0.6 ﹕ 2.0) 2.6g, wood fibre 0.5g, polyethylene glycol 0.1g, then add >=100 mesh toner 10g, it is fully dispersed
It is swollen 15min, keeps 41~42 DEG C of temperature, 2, the 2'- azo diisobutyl amidine dihydrochlorides (initiator V-50) of 3wt% are added
The sodium persulfate aqueous solution 2g of aqueous solution 5g, 2wt% stir evenly, are added the aqueous solution of sodium bisulfite 4g of 1.5wt%,
Enter polymerisation in plastic reactor.
Foam after polymerization colloid is shredded with scissors, is granulated with electrical meat mincer, and band air blast and micro- induced air type drying box are dried,
120 DEG C of drying temperature, 2.5h, grinding and sieving screen 40~100 mesh, obtain bladdery particle powder resin in irregular.
Treatment fluid：Water 6.0g, ethyl alcohol 3.0g, aluminum sulfate 1.0g, ethylene glycol diglycidylether 0.030g, glycerine 0.50g,
It is for use after dissolving mixing.100g powder particle resins are put into container, the treatment fluid prepared is added and is uniformly mixed,
Cross-linking reaction, heat preservation 60min, 100 DEG C of dry 6min, obtain quick absorption-type super absorbent resin at 100 DEG C.
Comparative example 1
Acrylic acid, the deionized water 70g of 100g are added in the 1000ml there-necked flasks with stirring, there-necked flask is put into and is added
Have in the water termostat water-bath of cold water, install constant pressure addition funnel, be inserted into thermometer, weighs the sodium hydroxide of 32wt%, adds
Enter in dropping funel, start stirring, be added dropwise lye neutralize, depending on controlling neutralization reaction temperature, temperature control at 42 DEG C hereinafter,
The liquid to be polymerized of degree of neutralization 75%, monomer concentration 41% is obtained after neutralization.
After neutralization, it is separately added into polyethyleneglycol diacrylate (PEGDA) 5wt% aqueous solutions 1.3g, 15min, keeps temperature
41~42 DEG C of degree, is added the sodium persulfate aqueous solution 5.0g of 2wt%, the sodium hydrogensulfite for stirring evenly, being added 1.5wt% is water-soluble
Liquid 5.0g pours into polymerisation in plastic reactor.
Colloid is shredded with scissors, is granulated with electrical meat mincer after polymerization, and band air blast and micro- induced air type drying box are dried, dry
120 DEG C of temperature, 2.5h, grinding and sieving screen 40~100 mesh, obtain irregular particle powder resin.
Treatment fluid：Water 6.0g, ethyl alcohol 3.0g, aluminum sulfate 1.0g, ethylene glycol diglycidylether 0.030g, glycerine 0.50g,
It is for use after dissolving mixing.100g powder particle resins are put into container, the treatment fluid prepared is added and is uniformly mixed,
Cross-linking reaction, heat preservation 60min, 100 DEG C of dry 6min, obtain super absorbent resin at 100 DEG C.
Comparative example 2
Acrylic acid, the deionized water 70g of 100g are added in the 1000ml there-necked flasks with stirring, there-necked flask is put into and is added
Have in the water termostat water-bath of cold water, install constant pressure addition funnel, be inserted into thermometer, weighs the sodium hydroxide of 32wt%, adds
Enter in dropping funel, start stirring, be added dropwise lye neutralize, depending on controlling neutralization reaction temperature, temperature control at 42 DEG C hereinafter,
The liquid to be polymerized of degree of neutralization 75%, monomer concentration 41% is obtained after neutralization.
After neutralization, adds the N of 2wt% respectively, N '-methylene-bisacrylamides (MBA) aqueous solution 1.1g, 15min, keep temperature
41~42 DEG C of degree, is added the sodium persulfate aqueous solution 5.0g of 2Wt%, the sodium hydrogensulfite for stirring evenly, being added 1.5wt% is water-soluble
Liquid 5.0g pours into polymerisation in plastic reactor.
Foam after polymerization colloid is shredded with scissors, is granulated with electrical meat mincer, and band air blast and micro- induced air type drying box are dried,
120 DEG C of drying temperature, 2.5h, grinding and sieving screen 40~100 mesh, obtain irregular particle powder resin.
Treatment fluid：Water 6.0g, ethyl alcohol 3.0g, aluminum sulfate 1.0g, ethylene glycol diglycidylether 0.030g, glycerine 0.50g,
It is for use after dissolving mixing.100g powder particle resins are put into container, the treatment fluid prepared is added and is uniformly mixed,
Cross-linking reaction, heat preservation 60min, 100 DEG C of dry 6min, obtain super absorbent resin at 100 DEG C.
The test result of Examples 1 to 5 and comparative example 1,2 is as shown in table 1：
Table 1
The present invention makees auxiliary agent using combined foaming and high-hydrophilic object, and it is special with irregular gap to use wood-fibred
Point improves hydrophily and water-retaining property performance, uses composite initiation system, improves polymerisation efficiency, polymerize steady, foaming
Uniformly, change Super Absorbent Polymer Particles form increases specific surface area, the method can make the equilibrium of super absorbent resin performance indicator,
Improve rate of water absorption.The method is simple for process, easy to operate, energy saving, colleges and universities, suitable industrialized production.
Claims (10)
1. a kind of preparation method of quick absorption-type super absorbent resin, it is characterised in that include the following steps：
(1) acrylic acid, water, lye are added in the reactor and obtain liquid to be polymerized after being reacted；
(2) it is separately added into crosslinking agent in above-mentioned liquid to be polymerized, composite foamable agent, wood fibre, polyethylene glycol, toner, draws
It sends out agent and reducing agent carries out polymerisation；
(3) jello is by obtaining bladdery particle powder in irregular after polymerizeing after shredding, be granulated, dry, crush, screening
Resin；
(4) quick absorption-type super absorbent resin is made in above-mentioned particle powder resin after surface treatment liquid cross-linking reaction.
2. the preparation method of quick absorption-type super absorbent resin according to claim 1, it is characterised in that：Step (1)
In, the alkali in lye is one kind in sodium hydroxide, potassium hydroxide, ammonium hydroxide, sodium carbonate, sodium bicarbonate, ammonium carbonate, ammonium hydrogen carbonate
Or two kinds of any of the above combinations.
3. the preparation method of quick absorption-type super absorbent resin according to claim 1, it is characterised in that：Step (1)
In, acrylic acid mass concentration is 30%~45% in liquid to be polymerized.
4. the preparation method of quick absorption-type super absorbent resin according to claim 1, it is characterised in that：Step (2)
In, the crosslinking agent be epoxy resin, epoxychloropropane, polyethyleneglycol diglycidylether, N, N- methylene-bisacrylamide,
The arbitrary combination of one or two or more kinds in polyethyleneglycol diacrylate, dosage be acrylic acid quality 0.005%~
0.5%.
5. the preparation method of quick absorption-type super absorbent resin according to claim 4, it is characterised in that：It is described compound
Foaming agent by foam microspheres powder with sodium bicarbonate powder is compound forms, dosage is the 1.0%~7.0% of acrylic acid quality.
6. the preparation method of quick absorption-type super absorbent resin according to claim 5, it is characterised in that：It is described wooden
Fiber consumption is the 0.2%~10% of acrylic acid quality.
7. the preparation method of quick absorption-type super absorbent resin according to claim 6, it is characterised in that：The poly- second
Glycol dosage is the 0.03%~0.3% of acrylic acid quality, and the mesh of the mesh number of the toner >=100, dosage is acrylic acid matter
The 4%~20% of amount.
8. the preparation method of quick absorption-type super absorbent resin according to claim 7, it is characterised in that：The initiation
Agent is the arbitrary combination of one or two or more kinds in azo-initiator, persulfate, hydrogen peroxide, and reducing agent is sodium sulfite
Or sodium hydrogensulfite, initiator amount are the 0.06%~0.6% of acrylic acid quality, reducing agent dosage is acrylic acid quality
0.02%~0.3%.
9. the preparation method of quick absorption-type super absorbent resin according to claim 1, it is characterised in that：Step (3)
In, 80 DEG C~130 DEG C of dry environment temperature, 2~12 hours drying times, sieving 40~100 mesh materials of screening.
10. the preparation method of quick absorption-type super absorbent resin according to claim 1, it is characterised in that：Step (4)
In, surface treatment liquid is made of water, aluminum sulfate, methanol or ethyl alcohol, ethylene glycol diglycidylether, glycerine, and the aluminum sulfate is gone
Ion, methanol or ethyl alcohol, ethylene glycol diglycidylether, glycerine mass ratio be 1：5~15：1~9：0.01~0.3：0.1~
1.0；Cross-linking reaction temperature is 50 DEG C~110 DEG C, and the reaction time is 20~80min, 5~10min of re-dry dehumidifying after reaction.
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| CN112266750A (en) * | 2020-11-06 | 2021-01-26 | 重庆博恩富克医疗设备有限公司 | Amphiphilic polymer material and preparation method thereof |
| CN112939506A (en) * | 2021-01-31 | 2021-06-11 | 湖北工业大学 | Preparation method of crack self-healing quick response additive for concrete |
| CN114571816A (en) * | 2022-02-17 | 2022-06-03 | 福建德普乐能源科技有限公司 | Preparation method of passive humidity adjusting sheet |
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| CN106750475A (en) * | 2017-02-27 | 2017-05-31 | 江苏虹创新材料有限公司 | It is a kind of to resist the preparation method for returning the super absorbent resin for oozing performance with height |
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