CN103936918A - Water-absorbing acrylate foam material and preparation method and application thereof - Google Patents
Water-absorbing acrylate foam material and preparation method and application thereof Download PDFInfo
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- CN103936918A CN103936918A CN201410147721.5A CN201410147721A CN103936918A CN 103936918 A CN103936918 A CN 103936918A CN 201410147721 A CN201410147721 A CN 201410147721A CN 103936918 A CN103936918 A CN 103936918A
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Abstract
The invention discloses a water-absorbing acrylate foam material and a preparation method and application thereof. The prepared water-absorbing acrylate foam material has a certain toughness and is small in foam hole size and suitable for dispersing and storing waterborne fluid, the average deionized water absorption rate, average saline water absorption rate, average artificial urine absorption rate and average artificial blood absorption rate are larger than 15g/g, and the water retention rate within half an hour is over 80 percent. Therefore, the massive soft water-absorbing material is applied to the field of hygienic products.
Description
Technical field
The invention belongs to water-absorbing material field, be specifically related to a kind of water-absorbing acrylic ester foam materials and its preparation method and application.
Background technology
Present sanitary product, the water-absorbing material of the inside is mainly to have granular synthetic resins, water suction, inhale urine or suck blood after can form gel, easily agglomerating, cause the more difficult position that is fixed on, in actual use procedure, make us very uncomfortable.Therefore developing block soft water-absorbing material has great significance.
Common blood is made up of hemocyte, blood plasma etc.The diameter of hemocyte is 8 μ m left and right, and the diameter of acrylic molecules is much smaller than the diameter of hemocyte.The compositions such as therefore hemocyte is difficult for being absorbed by gelatinous super absorbent resin, can only rest on the surface of super absorbent resin, the blood plasma in the just blood of absorption.So exploitation multi-hole type polymkeric substance, to expand specific surface area, improves perviousness, the aspect such as absorption rate and specific absorption of accelerating liquid has important technical economic benefit and social benefit.
For adopting the foam materials prepared of acrylic ester monomer, prior art is disclosed in the ionogen that adds approximately 3.85% in water, in order to regulate the solubleness of acrylic ester monomer in water and to adjust the perforate degree of the micropore of foam materials.But electrolytical addition is very few, be difficult to achieve the above object, if but electrolytical addition is excessive, its other performance to foam materials can be brought negative impact.Electrolytical addition, closely related with the monomeric species that foam materials adopts, from the prior art, in existing foam materials formula, electrolytical concentration is generally not less than 3.5wt%.。
Summary of the invention
The object of the invention is to overcome above-mentioned the deficiencies in the prior art, a kind of preparation method of water-absorbing acrylic ester foam materials is provided.
Another object of the present invention is to provide the water-absorbing acrylic ester foam materials being prepared by preparation method of the present invention.
Another object of the present invention is to provide the application of described water-absorbing acrylic ester foam materials in sanitary product.
Above-mentioned purpose of the present invention is achieved by following technical solution:
The preparation method of water-absorbing acrylic ester foam materials, comprises the steps:
S1. prepare oil-based system: percentage ratio meter takes 25%～95% monofunctional acrylate class monomer, 2%～60% linking agent, 1%～15% emulsifier for mixing and mixes by weight;
S2. prepare aqueous phase system: the aqueous electrolyte liquid that preparation massfraction is 0.01～3%;
S3. at 60～80 DEG C, aqueous phase system is divided and add in oil-based system for 2～4 times, stir, the volume ratio of final water and oil phase is 10～100:1;
S4. in the mixed system of step S3, add water soluble starter to carry out emulsion polymerization;
S5. step S4 gained polymerisate is placed in to isothermal curing at 80～100 DEG C, washs, dehydrates and obtain product;
Described monofunctional acrylate class monomer is one or more in simple function alkyl acrylate or simple function alkyl methacrylate;
Described linking agent is one or more in multifunctional alkyl acrylate or multifunctional alkyl methacrylate.
Preferably, the consisting of of oil-based system described in step S1: percentage ratio meter takes 45%～75% monofunctional acrylate class monomer, 15%～40% linking agent, 5%～15% emulsifying agent by weight.
Ionogen of the present invention is the conventional solubility ionogen in this area, and object is that the salt ionic concentration of raising system reduces oil-soluble monomer, the comonomer solubleness in water, and preferably, described ionogen is one or more in metal ion compound.
Preferably, the positively charged ion of described metal ion compound is potassium ion, sodium ion, calcium ion, magnesium ion, aluminum ion, zine ion or iron ion, and negatively charged ion is chlorion, nitrate ion, borate ion, phosphate anion or carbanion; The ionic compound of above-mentioned positively charged ion and negatively charged ion combination water insoluble or be slightly soluble in water except.
Preferably, described metal ion compound is calcium chloride, nitrocalcite, aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, potassiumphosphate, sodium phosphate, potassium borate, Sodium Tetraborate, salt of wormwood or sodium carbonate.Above-mentioned ionogen comprises strong base-weak acid salt or strong acid soft base salt, and these salt have certain pH value shock-absorbing capacity, are more conducive to carrying out smoothly of letex polymerization.In addition, those skilled in the art can get rid of the situation that many kinds of metal ions compound combination uses generation to precipitate according to general knowledge.
Preferably, described metal ion compound is calcium chloride, nitrocalcite or aluminum chloride.
The inventor finds in experiment, in the formula described in the application, in aqueous electrolyte liquid the massfraction of solute under the concentration conventional lower than prior art, still can make abscess-size more evenly, consistent; Even and electrolytical concentration is low to moderate 0.01%, compared with not adding ionogen, still tool is significantly improved the effect of water absorbing properties, and the snappiness of material is better, is difficult for splitting.
Therefore, preferably, the massfraction of described aqueous electrolyte liquid is 0.01%～1%.
Further preferably, the massfraction of described aqueous electrolyte liquid is 0.02%～0.1%.
Preferably, described simple function alkyl acrylate is Isooctyl acrylate monomer, isodecyl acrylate, vinylformic acid stearyl or lauryl acrylate, and described simple function alkyl methacrylate is Isooctyl methacrylate, isodecyl methacrylate, methacrylic acid stearyl or lauryl methacrylate(LMA).
Further preferably, described monofunctional acrylate class monomer is the mixture of Isooctyl acrylate monomer and Isooctyl methacrylate.
The inventor finds in experiment, the mass ratio that changes Isooctyl acrylate monomer and Isooctyl methacrylate can significantly improve the water-absorbent of acrylate foam materials and the abscess-size of foam materials, further improves the specific absorption of acrylate foam materials and widens its Application Areas.
Therefore, preferably, the mass ratio of described Isooctyl acrylate monomer and Isooctyl methacrylate is 7:1～11:1.
Further preferably, the mass ratio of described Isooctyl acrylate monomer and Isooctyl methacrylate is 9:1.
Described multifunctional alkyl acrylate is hexanediol diacrylate, triethylene glycol diacrylate, propylene glycol diacrylate or tripropylene glycol diacrylate, and described multifunctional alkyl methacrylate is Ethylene glycol dimethacrylate, TEGDMA, dipropylene glycol dimethacrylate or tripropylene glycol dimethacrylate.
It is to form emulsion with monomer that the present invention adds the effect of emulsifying agent, for letex polymerization provides condition, because monomer used in the present invention is substantially water insoluble, thereby use hydrophobic emulsifying agent to be more conducive to disperse monomer of the present invention and reduce its solubleness in water; Preferably, described emulsifying agent comprises side chain C
16～C
24lipid acid, the unsaturated C of straight chain
16～C
22the saturated C of lipid acid or straight chain
12～C
14the sorbitan monoesters of lipid acid.
Further preferably, described emulsifying agent is tween 20, Tween-40, Tween-60, tween-80 or Glycerol dimer list isostearate.
The consumption of the initiator that the present invention uses can be selected according to this area conventional emulsion polymerization, is generally 0.1%～20% of monomer weight.
The kind of described initiator also can be selected according to the kind of this area polymerization single polymerization monomer, and as persulfate initiator, preferably, described initiator is ammonium persulphate, Sodium Persulfate or Potassium Persulphate.
The present invention is after definite water and the final ratio of oil phase, water divides 2～4 times and adds in oil phase, become sticky before thick and add again water once in emulsion, object is that the mode of adding the employing multistage can be under identical mixing residence time, make the emulsion of high water and oil phase weight ratio, can also make the abscess-size of product simultaneously evenly, unanimously.Preferably, water is divided into 2/3 and 1/3 two portions, first oil phase is mixed with 2/3 water, become sticky and add again 1/3 remaining water to mix before thick in emulsion.
Described in step S5, be cured as reacted polymerisate emulsion is poured into and in mould, put into constant temperature oven and solidify, the object that is controlled at isothermal curing under 80～100 DEG C of conditions is that acrylate is quick-setting ensures that water does not seethe with excitement simultaneously allowing, and avoids producing pore not of uniform size at material surface.
Described in step S5, wash object and be to remove remaining initial water and equate impurity, described in dehydrate also and carry out in constant temperature oven or vacuum drying oven, dehydrating temperature is 80～100 DEG C.
The water-absorbing acrylic ester foam materials obtaining according to above-mentioned preparation method.
The present invention is by specific formula, adopt the water-absorbing acrylic ester foam materials that specific preparation method makes to have certain toughness, abscess-size is small, has good water suction, inhales urine, the performance of sucking blood, the specific absorption of material is high, has great application prospect in hygiene article sector.Concrete preparation technology's flow process can be with reference to shown in figure 1.
The range of cell sizes that acrylate foam materials of the present invention has is 10 μ m to 30 μ m, so be applicable to disperseing and storing aqueous fluid.In addition,, because the diameter of human body hemocyte is 8 μ m left and right, the diameter of existing acrylic molecules is much smaller than the diameter of hemocyte, thereby acrylate foam materials of the present invention is particularly suitable for the Material Field of sucking blood.
Compared with prior art, the present invention has following beneficial effect:
The present invention discloses a kind of water-absorbing acrylic ester foam materials and its preparation method and application, the water-absorbing acrylic ester foam materials making has certain toughness, abscess-size is small, it on average sucks ionized water rate, average absorption salt ratio, on average inhale artificial urine rate, on average inhale artificial blood rate is all greater than 15g/g, halfhour water retention is all more than 80%, be suitable for disperseing and storing aqueous fluid, therefore the soft water-absorbing material of bulk of the present invention is well suited for being applied to hygiene article sector.
Brief description of the drawings
Fig. 1 is water-absorbing acrylic ester foam materials preparation technology flow process reference drawing.
Embodiment
Below in conjunction with specific embodiment, the present invention is further explained, but embodiments of the present invention is not limited in any way.Unless stated otherwise, in embodiment, related reagent, method is the conventional reagent in this area and method.
embodiment 1
One, the preparation of water-absorbing acrylic ester foam materials
(1) preparation oil-based system, take Isooctyl acrylate monomer 7.2g, Isooctyl methacrylate 0.8g, Ethylene glycol dimethacrylate 4.8g, hexanediol diacrylate 0.4g, tween-80 1.3g, oil phase is stirred stand-by, wherein, the mass ratio of Isooctyl acrylate monomer and Isooctyl methacrylate is 9:1.
(2) preparation aqueous phase system, take calcium chloride 0.096g, then add water to 480g make its dissolve, now, the massfraction of electrolytic solution is 0.02%, stand-by.
(3) preparation initiator phase, takes ammonium persulphate 1.71g, adds water to 10g it is dissolved, stand-by.
(4) the water 320g making is proceeded in the there-necked flask of 1000ml, start to stir, be warming up to 75 DEG C, stirring velocity turns above 800, then the oil phase stirring is added in there-necked flask, etc. emulsion become sticky thick before, drip again 160g water in flask, finally drip initiator in flask, after polyreaction, mixed solution is poured in large tetrafluoroethylene square plate into cover lid, put into 97 DEG C of baking ovens 0.5 hour, after forming and hardening, take out extruding and washing, then take the oven dry of baking oven the inside.
Two, product test
Prepared product out has certain toughness, and abscess-size is small, and by scanning electronic microscope (SEM) test, the abscess-size of product is 10～30 μ m.It on average sucks ionized water rate be that 19.8g/g, average absorption salt ratio are 20.2g/g, on average to inhale artificial urine rate be 21.2g/g, on average inhale artificial blood rate is 21.6g/g, halfhour water retention is all more than 88%, be suitable for disperseing and storing aqueous fluid, be suitable for hygiene article sector.
embodiment 2
One, the preparation of water-absorbing acrylic ester foam materials
(1) preparation oil-based system, take Isooctyl acrylate monomer 5.6g, Isooctyl methacrylate 0.8g, Ethylene glycol dimethacrylate 4.8g, hexanediol diacrylate 0.4g, tween-80 1.3g, oil phase is stirred stand-by, wherein, the mass ratio of Isooctyl acrylate monomer and Isooctyl methacrylate is 7:1.
(2) preparation aqueous phase system, take calcium chloride 0.48g, then add water to 480g make its dissolve, now, the massfraction of electrolytic solution is 0. 1%, stand-by.
(3) preparation initiator phase, takes ammonium persulphate 1.71g, adds water to 10g it is dissolved, stand-by.
(4) the water 320g making is proceeded in the there-necked flask of 1000ml, start to stir, be warming up to 75 DEG C, stirring velocity turns above 800, then the oil phase stirring is added in there-necked flask, etc. emulsion become sticky thick before, drip again 160g water in flask, finally drip initiator in flask, after polyreaction, mixed solution is poured in large tetrafluoroethylene square plate into cover lid, put into 97 DEG C of baking ovens 0.5 hour, after forming and hardening, take out extruding and washing, then take the oven dry of baking oven the inside.
Two, product test
Prepared product out has certain toughness, and abscess-size is small, and by scanning electronic microscope (SEM) test, the abscess-size of product is 10～30 μ m.It on average sucks ionized water rate be that 18.4g/g, average absorption salt ratio are 18.2g/g, on average to inhale artificial urine rate be 18.0g/g, on average inhale artificial blood rate is 19.16g/g, halfhour water retention is all more than 86%, be suitable for disperseing and storing aqueous fluid, be suitable for hygiene article sector.
embodiment 3
One, the preparation of water-absorbing acrylic ester foam materials
(1) preparation oil-based system, take Isooctyl acrylate monomer 8.8g, Isooctyl methacrylate 0.8g, Ethylene glycol dimethacrylate 4.8g, hexanediol diacrylate 0.4g, tween-80 1.3g, oil phase is stirred stand-by, wherein, the mass ratio of Isooctyl acrylate monomer and Isooctyl methacrylate is 11:1.
(2) preparation aqueous phase system, take calcium chloride 4.8g, then add water to 480g make its dissolve, now, the massfraction of electrolytic solution is 1%, stand-by.
(3) preparation initiator phase, takes ammonium persulphate 1.71g, adds water to 10g it is dissolved, stand-by.
(4) the water 320g making is proceeded in the there-necked flask of 1000ml, start to stir, be warming up to 75 DEG C, stirring velocity turns above 800, then the oil phase stirring is added in there-necked flask, etc. emulsion become sticky thick before, drip again 160g water in flask, finally drip initiator in flask, after polyreaction, mixed solution is poured in large tetrafluoroethylene square plate into cover lid, put into 97 DEG C of baking ovens 0.5 hour, after forming and hardening, take out extruding and washing, then take the oven dry of baking oven the inside.
Two, product test
Prepared product out has certain toughness, and abscess-size is small, and by scanning electronic microscope (SEM) test, the abscess-size of product is 10～30 μ m.It on average sucks ionized water rate be that 18.4g/g, average absorption salt ratio are 20.17g/g, on average to inhale artificial urine rate be 19.9g/g, on average inhale artificial blood rate is 20.01g/g, halfhour water retention is all more than 86%, be suitable for disperseing and storing aqueous fluid, be suitable for hygiene article sector.
embodiment 4
One, the preparation of water-absorbing acrylic ester foam materials
(1) preparation oil-based system, take Isooctyl acrylate monomer 8.8g, Isooctyl methacrylate 0.8g, Ethylene glycol dimethacrylate 4.8g, hexanediol diacrylate 0.4g, tween-80 1.3g, oil phase is stirred stand-by, wherein, the mass ratio of Isooctyl acrylate monomer and Isooctyl methacrylate is 11:1.
(2) preparation aqueous phase system, take nitrocalcite 14.4g, then add water to 480g make its dissolve, now, the massfraction of electrolytic solution is 3%, stand-by.
(3) preparation initiator phase, takes ammonium persulphate 1.71g, adds water to 10g it is dissolved, stand-by.
(4) the water 320g making is proceeded in the there-necked flask of 1000ml, start to stir, be warming up to 75 DEG C, stirring velocity turns above 800, then the oil phase stirring is added in there-necked flask, etc. emulsion become sticky thick before, drip again 160g water in flask, finally drip initiator in flask, after polyreaction, mixed solution is poured in large tetrafluoroethylene square plate into cover lid, put into 97 DEG C of baking ovens 0.5 hour, after forming and hardening, take out extruding and washing, then take the oven dry of baking oven the inside.
Two, product test
Prepared product out has certain toughness, and abscess-size is small, and by scanning electronic microscope (SEM) test, the abscess-size of product is 10～30 μ m.It on average sucks ionized water rate be that 13.4g/g, average absorption salt ratio are 12.9g/g, on average to inhale artificial urine rate be 13.9g/g, on average inhale artificial blood rate is 16.04g/g, halfhour water retention is all more than 80%, be suitable for disperseing and storing aqueous fluid, be suitable for hygiene article sector.
embodiment 5
One, the preparation of water-absorbing acrylic ester foam materials
(1) preparation oil-based system, take Isooctyl acrylate monomer 8.8g, Isooctyl methacrylate 0.8g, Ethylene glycol dimethacrylate 4.8g, hexanediol diacrylate 0.4g, tween-80 1.3g, oil phase is stirred stand-by, wherein, the mass ratio of Isooctyl acrylate monomer and Isooctyl methacrylate is 11:1.
(2) preparation aqueous phase system, take nitrocalcite 0.48g, then add water to 480g make its dissolve, now, the massfraction of electrolytic solution is 0.1%, stand-by.
(3) preparation initiator phase, takes ammonium persulphate 1.71g, adds water to 10g it is dissolved, stand-by.
(4) the water 320g making is proceeded in the there-necked flask of 1000ml, start to stir, be warming up to 75 DEG C, stirring velocity turns above 800, then the oil phase stirring is added in there-necked flask, etc. emulsion become sticky thick before, drip again 160g water in flask, finally drip initiator in flask, after polyreaction, mixed solution is poured in large tetrafluoroethylene square plate into cover lid, put into 97 DEG C of baking ovens 0.5 hour, after forming and hardening, take out extruding and washing, then take the oven dry of baking oven the inside.
Two, product test
Prepared product out has certain toughness, and abscess-size is small, and by scanning electronic microscope (SEM) test, the abscess-size of product is 10～30 μ m.It on average sucks ionized water rate be that 17.8g/g, average absorption salt ratio are 18.6g/g, on average to inhale artificial urine rate be 17.2g/g, on average inhale artificial blood rate is 19.0g/g, halfhour water retention is all more than 88%, be suitable for disperseing and storing aqueous fluid, be suitable for hygiene article sector.
embodiment 6
One, the preparation of water-absorbing acrylic ester foam materials
(1) preparation oil-based system, take Isooctyl acrylate monomer 8.8g, Isooctyl methacrylate 0.8g, Ethylene glycol dimethacrylate 4.8g, hexanediol diacrylate 0.4g, tween-80 1.3g, oil phase is stirred stand-by, wherein, the mass ratio of Isooctyl acrylate monomer and Isooctyl methacrylate is 11:1.
(2) preparation aqueous phase system, take nitrocalcite 0.096g, then add water to 480g make its dissolve, now, the massfraction of electrolytic solution is 0.02%, stand-by.
(3) preparation initiator phase, takes Potassium Persulphate 1.37g, adds water to 10g it is dissolved, stand-by.
(4) the water 320g making is proceeded in the there-necked flask of 1000ml, start to stir, be warming up to 80 DEG C, stirring velocity turns above 800, then the oil phase stirring is added in there-necked flask, etc. emulsion become sticky thick before, drip again 160g water in flask, finally drip initiator in flask, after polyreaction, mixed solution is poured in large tetrafluoroethylene square plate into cover lid, put into 80 DEG C of baking ovens 1 hour, after forming and hardening, take out extruding and washing, then take the oven dry of baking oven the inside.
Two, product test
Prepared product out has certain toughness, and abscess-size is small, and by scanning electronic microscope (SEM) test, the abscess-size of product is 10～30 μ m.It on average sucks ionized water rate be that 17.7g/g, average absorption salt ratio are 18.0g/g, on average to inhale artificial urine rate be 17.7g/g, on average inhale artificial blood rate is 18.6g/g, halfhour water retention is all more than 87%, be suitable for disperseing and storing aqueous fluid, be suitable for hygiene article sector.
embodiment 7
One, the preparation of water-absorbing acrylic ester foam materials
(1) preparation oil-based system, takes lauryl acrylate 11.4g, tripropylene glycol dimethacrylate 3.0g, tripropylene glycol diacrylate 5.8g, Tween-40 2.0g, oil phase is stirred stand-by.
(2) preparation aqueous phase system, take aluminum chloride 0.48g, then add water to 480g make its dissolve, now, the massfraction of electrolytic solution is 0.1%, stand-by.
(3) preparation initiator phase, takes Sodium Persulfate 1.81g, adds water to 10g it is dissolved, stand-by.
(4) the water 160g making is proceeded in the there-necked flask of 1000ml, start to stir, be warming up to 65 DEG C, stirring velocity turns above 800, then the oil phase stirring is added in there-necked flask, etc. emulsion become sticky thick before, again 320g water is successively added drop-wise in flask at twice, finally drip initiator in flask, after polyreaction, mixed solution is poured in large tetrafluoroethylene square plate into cover lid, put into 85 DEG C of baking ovens 1 hour, after forming and hardening, take out extruding and washing, then take the oven dry of baking oven the inside.
Two, product test
Prepared product out has certain toughness, and abscess-size is small, and by scanning electronic microscope (SEM) test, the abscess-size of product is 10～30 μ m.It on average sucks ionized water rate be that 16.3g/g, average absorption salt ratio are 16.8g/g, on average to inhale artificial urine rate be 15.9g/g, on average inhale artificial blood rate is 16.1g/g, halfhour water retention is all more than 82%, be suitable for disperseing and storing aqueous fluid, be suitable for hygiene article sector.
embodiment 8
One, the preparation of water-absorbing acrylic ester foam materials
(1) preparation oil-based system, takes methacrylic acid stearyl 9.4g, lauryl methacrylate(LMA) 3.8g, propylene glycol diacrylate 1.8g, tripropylene glycol dimethacrylate 1.4g, Tween-60 2.5g, oil phase is stirred stand-by.
(2) preparation aqueous phase system, take aluminum chloride 0.288g, then add water to 480g make its dissolve, now, the massfraction of electrolytic solution is 0.06%, stand-by.
(3) preparation initiator phase, takes ammonium persulphate 1.91g, adds water to 10g it is dissolved, stand-by.
(4) the water 240g making is proceeded in the there-necked flask of 1000ml, start to stir, be warming up to 70 DEG C, stirring velocity turns above 800, then the oil phase stirring is added in there-necked flask, etc. emulsion become sticky thick before, drip again 240g water in flask, finally drip initiator in flask, after polyreaction, mixed solution is poured in large tetrafluoroethylene square plate into cover lid, put into 90 DEG C of baking ovens 0.5 hour, after forming and hardening, take out extruding and washing, then take the oven dry of baking oven the inside.
Two, product test
Prepared product out has certain toughness, and abscess-size is small, and by scanning electronic microscope (SEM) test, the abscess-size of product is 10～30 μ m.It on average sucks ionized water rate be that 16.5g/g, average absorption salt ratio are 17.4g/g, on average to inhale artificial urine rate be 16.7g/g, on average inhale artificial blood rate is 17.2g/g, halfhour water retention is all more than 84%, be suitable for disperseing and storing aqueous fluid, be suitable for hygiene article sector.
embodiment 9
One, the preparation of water-absorbing acrylic ester foam materials
(1) preparation oil-based system, takes methacrylic acid stearyl 9.4g, lauryl methacrylate(LMA) 3.8g, propylene glycol diacrylate 1.8g, tripropylene glycol dimethacrylate 1.4g, Tween-60 2.5g, oil phase is stirred stand-by.
(2) preparation aqueous phase system, take aluminum chloride 0.384g, then add water to 480g make its dissolve, now, the massfraction of electrolytic solution is 0.08%, stand-by.
(3) preparation initiator phase, takes ammonium persulphate 1.91g, adds water to 10g it is dissolved, stand-by.
(4) the water 240g making is proceeded in the there-necked flask of 1000ml, start to stir, be warming up to 70 DEG C, stirring velocity turns above 800, then the oil phase stirring is added in there-necked flask, etc. emulsion become sticky thick before, drip again 240g water in flask, finally drip initiator in flask, after polyreaction, mixed solution is poured in large tetrafluoroethylene square plate into cover lid, put into 90 DEG C of baking ovens 0.5 hour, after forming and hardening, take out extruding and washing, then take the oven dry of baking oven the inside.
Two, product test
Prepared product out has certain toughness, and abscess-size is small, and by scanning electronic microscope (SEM) test, the abscess-size of product is 10～30 μ m.It on average sucks ionized water rate be that 16.5g/g, average absorption salt ratio are 16.4g/g, on average to inhale artificial urine rate be 17.7g/g, on average inhale artificial blood rate is 18.4g/g, halfhour water retention is all more than 85%, be suitable for disperseing and storing aqueous fluid, be suitable for hygiene article sector.
comparative example 1
One, the preparation of water-absorbing acrylic ester foam materials
(1) preparation oil-based system, take Isooctyl acrylate monomer 16g, Isooctyl methacrylate 0.8g, Ethylene glycol dimethacrylate 4.8g, hexanediol diacrylate 0.4g, tween-80 1.3g, oil phase is stirred stand-by, wherein, the mass ratio of Isooctyl acrylate monomer and Isooctyl methacrylate is 20:1.
(2) preparation aqueous phase system, take calcium chloride 0.096g, then add water to 480g make its dissolve, now, the massfraction of electrolytic solution is 0.02%, stand-by.
(3) preparation initiator phase, takes ammonium persulphate 1.71g, adds water to 10g it is dissolved, stand-by.
(4) water 320g is proceeded in the there-necked flask of 1000ml, start to stir, be warming up to 75 DEG C, stirring velocity turns above 800, then the oil phase stirring is added in there-necked flask, etc. emulsion become sticky thick before, drip again 160g water in flask, finally drip initiator in flask, after polyreaction, mixed solution is poured in large tetrafluoroethylene square plate into cover lid, put into 97 DEG C of baking ovens 0.5 hour, after forming and hardening, take out extruding and washing, then take the oven dry of baking oven the inside.
Two, product test
Prepared product out has poor toughness and hard and crisp, and the larger and skewness of abscess-size, tests by scanning electronic microscope (SEM), and the abscess-size of product is more than 100 μ m.It on average sucks ionized water rate be that 12.5g/g, average absorption salt ratio are 10.4g/g, on average to inhale artificial urine rate be 9.7g/g, on average inhale artificial blood rate is 9.4g/g, halfhour water retention only has 55% left and right, disperse and store aqueous fluid ability a little less than, be not suitable for hygiene article sector.
comparative example 2
One, the preparation of water-absorbing acrylic ester foam materials
(1) preparation oil-based system, take Isooctyl acrylate monomer 7.2g, Isooctyl methacrylate 0.8g, Ethylene glycol dimethacrylate 4.8g, hexanediol diacrylate 0.4g, tween-80 1.3g, oil phase is stirred stand-by, wherein, the mass ratio of Isooctyl acrylate monomer and Isooctyl methacrylate is 9:1.
(2) preparation aqueous phase system, take calcium chloride 19.2g, then add water to 480g make its dissolve, now, the massfraction of electrolytic solution is 4%, stand-by.
(3) preparation initiator phase, takes ammonium persulphate 1.71g, adds water to 10g it is dissolved, stand-by.
(4) the water 320g making is proceeded in the there-necked flask of 1000ml, start to stir, be warming up to 75 DEG C, stirring velocity turns above 800, then the oil phase stirring is added in there-necked flask, etc. emulsion become sticky thick before, drip again 160g water in flask, finally drip initiator in flask, after polyreaction, mixed solution is poured in large tetrafluoroethylene square plate into cover lid, put into 97 DEG C of baking ovens 0.5 hour, after forming and hardening, take out extruding and washing, then take the oven dry of baking oven the inside.
Two, product test
Prepared product out has certain toughness, and abscess-size is small, and by scanning electronic microscope (SEM) test, the abscess-size of product is 10～30 μ m.It on average sucks ionized water rate be that 11.2g/g, average absorption salt ratio are 11.8g/g, on average to inhale artificial urine rate be 11.3g/g, on average inhale artificial blood rate is 10.2g/g, halfhour water retention only has 70% left and right, disperse and store aqueous fluid ability a little less than, be not suitable for hygiene article sector.
comparative example 3
One, the preparation of water-absorbing acrylic ester foam materials
(1) preparation oil-based system, takes isodecyl acrylate 16.4g, dipropylene glycol dimethacrylate 4.0g, triethylene glycol diacrylate 0.8g, Glycerol dimer list isostearate 2.0g, oil phase is stirred stand-by.
(2) preparation aqueous phase system, take calcium chloride 17.71g, then add water to 480g make its dissolve, now, the massfraction of electrolytic solution is 3.6%, stand-by.
(3) preparation initiator phase, takes Sodium Persulfate 2.11g, adds water to 10g it is dissolved, stand-by.
(4) the water 320g making is proceeded in the there-necked flask of 1000ml, start to stir, be warming up to 60 DEG C, stirring velocity turns above 800, then the oil phase stirring is added in there-necked flask, etc. emulsion become sticky thick before, drip again 160g water in flask, finally drip initiator in flask, after polyreaction, mixed solution is poured in large tetrafluoroethylene square plate into cover lid, put into 95 DEG C of baking ovens 0.5 hour, after forming and hardening, take out extruding and washing, then take the oven dry of baking oven the inside.
Two, product test
Prepared product out has certain toughness, and abscess-size is small, and by scanning electronic microscope (SEM) test, the abscess-size of product is 10～30 μ m.It on average sucks ionized water rate be that 9.4g/g, average absorption salt ratio are 8.2g/g, on average to inhale artificial urine rate be 7.1g/g, on average inhale artificial blood rate is 7.3g/g, halfhour water retention only has 70% left and right, disperse and store aqueous fluid ability a little less than, be not suitable for hygiene article sector.
comparative example 4
One, the preparation of water-absorbing acrylic ester foam materials
(1) preparation oil-based system, takes isodecyl acrylate 16.4g, dipropylene glycol dimethacrylate 4.0g, triethylene glycol diacrylate 0.8g, Glycerol dimer list isostearate 2.0g, oil phase is stirred stand-by.
(2) preparation aqueous phase system, 480g is stand-by in water intaking.
(3) preparation initiator phase, takes Sodium Persulfate 2.11g, adds water to 10g it is dissolved, stand-by.
(4) the water 320g making is proceeded in the there-necked flask of 1000ml, start to stir, be warming up to 60 DEG C, stirring velocity turns above 800, then the oil phase stirring is added in there-necked flask, etc. emulsion become sticky thick before, drip again 160g water in flask, finally drip initiator in flask, after polyreaction, mixed solution is poured in large tetrafluoroethylene square plate into cover lid, put into 95 DEG C of baking ovens 0.5 hour, after forming and hardening, take out extruding and washing, then take the oven dry of baking oven the inside.
Two, product test
Prepared product out has poor toughness and hard and crisp, and the larger and skewness of abscess-size, tests by scanning electronic microscope (SEM), and the abscess-size of product is more than 100 μ m.It on average sucks ionized water rate be that 4.2g/g, average absorption salt ratio are 4.5g/g, on average to inhale artificial urine rate be 4.3g/g, on average inhale artificial blood rate is 4.7g/g, halfhour water retention only has 20% left and right, and do not there is snappiness, and be easy to split, be not suitable for disperseing and storing aqueous fluid.
Claims (10)
1. the preparation method of water-absorbing acrylic ester foam materials, is characterized in that, comprises the steps:
S1. prepare oil-based system: percentage ratio meter takes 25%～95% monofunctional acrylate class monomer, 2%～60% linking agent, 1%～15% emulsifier for mixing and mixes by weight;
S2. prepare aqueous phase system: the aqueous electrolyte liquid that preparation massfraction is 0.01～3%;
S3. at 60～80 DEG C, aqueous phase system is divided and add in oil-based system for 2～4 times, stir, the volume ratio of final water and oil phase is 10～100:1;
S4. in the mixed system of step S3, add water soluble starter to carry out emulsion polymerization;
S5. step S4 gained polymerisate is placed in to isothermal curing at 80～100 DEG C, washs, dehydrates and obtain product;
Described monofunctional acrylate class monomer is one or more in simple function alkyl acrylate or simple function alkyl methacrylate;
Described linking agent is one or more in multifunctional alkyl acrylate or multifunctional alkyl methacrylate.
2. preparation method according to claim 1, is characterized in that, the consisting of of oil-based system described in step S1: percentage ratio meter takes 45%～75% monofunctional acrylate class monomer, 15%～40% linking agent, 5%～15% emulsifying agent by weight.
3. according to preparation method described in claim 1 or 2, it is characterized in that, described ionogen is one or more in metal ion compound, the positively charged ion of described metal ion compound is potassium ion, sodium ion, calcium ion, magnesium ion, aluminum ion, zine ion or iron ion, and negatively charged ion is chlorion, nitrate ion, borate ion, phosphate anion or carbanion.
4. preparation method according to claim 3, is characterized in that, metal ion compound is calcium chloride, nitrocalcite, aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, potassiumphosphate, sodium phosphate, potassium borate, Sodium Tetraborate, salt of wormwood or sodium carbonate.
5. preparation method according to claim 4, is characterized in that, described metal ion compound is calcium chloride, nitrocalcite or aluminum chloride.
6. according to preparation method described in claim 1 or 2, it is characterized in that, described simple function alkyl acrylate is Isooctyl acrylate monomer, isodecyl acrylate, vinylformic acid stearyl or lauryl acrylate, and described simple function alkyl methacrylate is Isooctyl methacrylate, isodecyl methacrylate, methacrylic acid stearyl or lauryl methacrylate(LMA);
Described multifunctional alkyl acrylate is hexanediol diacrylate, triethylene glycol diacrylate, propylene glycol diacrylate or tripropylene glycol diacrylate, and described multifunctional alkyl methacrylate is Ethylene glycol dimethacrylate, TEGDMA, dipropylene glycol dimethacrylate or tripropylene glycol dimethacrylate.
7. according to preparation method described in claim 1 or 2, it is characterized in that, described emulsifying agent is side chain C
16～C
24lipid acid, the unsaturated C of straight chain
16～C
22the saturated C of lipid acid or straight chain
12～C
14the sorbitan monoesters of lipid acid; Described initiator is ammonium persulphate, Sodium Persulfate or Potassium Persulphate.
8. preparation method according to claim 7, is characterized in that, described emulsifying agent is tween 20, Tween-40, Tween-60, tween-80 or Glycerol dimer list isostearate.
9. the water-absorbing acrylic ester foam materials that described in any claim of claim 1 to 8, preparation method prepares.
Described in claim 9 water-absorbing acrylic ester foam materials in the application of preparing in sanitary product.
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| CN113637278B (en) * | 2021-09-17 | 2022-10-21 | 佛山市嘉信盈科技有限公司 | Short fiber toughened water-absorbent acrylate polymer material and preparation method thereof |
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