CN101712785A - Novel super absorbent resin/inorganic nanoparticle composite material, preparation method thereof and usage thereof - Google Patents
Novel super absorbent resin/inorganic nanoparticle composite material, preparation method thereof and usage thereof Download PDFInfo
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- CN101712785A CN101712785A CN200810200793A CN200810200793A CN101712785A CN 101712785 A CN101712785 A CN 101712785A CN 200810200793 A CN200810200793 A CN 200810200793A CN 200810200793 A CN200810200793 A CN 200810200793A CN 101712785 A CN101712785 A CN 101712785A
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Abstract
The invention belongs to the field of nano composite materials, and in particular relates to a super absorbent resin/inorganic nanoparticle composite material prepared by in-situ polymerization. The composite material is prepared by firstly dispersing nanoparticles into crylic acid aqueous solution (neutralization degree of 5 to 40 percent), and then adding initiator, a crosslinking agent and an optional copolymer substrate (such as starch, cellulose, acrylamide and the like); raising temperature, reacting the product under nitrogen for certain time and taking the product out; and washing, drying and crushing to obtain the final super absorbent resin nano composite material. The nano composite material shows excellent absorption properties, thermal properties and mechanical properties, and can replace the conventional super absorbent resin to be applied in the fields of seeding protection in agriculture and forestry, sanitary materials, petrochemical industry, environment protection and the like.
Description
Technical field
The invention belongs to the polymer nanocomposites field, relate in particular to a kind of novel super absorbent resin/inorganic nanometer particle compesite.
Background technology
High hydrophilous resin is a kind of new functional macromolecule material that grows up nearly decades, since its on molecular structure, have have in a large number very strong hydrophilic chemical based because of, and these chemical based absorb water and high water retention characteristic thereby make such material have height because of forming various corresponding complex constructions.Because of having unique suction and water retention capacity, for example its water and pressurization that can absorb tens of times to thousands of times is not dewatered yet, and fields such as High hydrophilous resin is kept a full stand of seedings in agricultural, sanitary material, petrochemical complex, environment protection have all obtained using widely.According to the raw material classification, High hydrophilous resin can be divided into following several: (1) starch based, starch are the poly-hydroxy natural compoundss that a kind of raw material sources are extensive, kind is many, cheap.The monomer that carries out graft copolymerization with starch mainly is to become hydrophilic vinyl monomer after wetting ability and the hydrolysis.(2) synthetic resin mainly contains acrylic acid or the like, polypropylene alcohols etc., and is wherein most important with acrylic acid or the like; (3) cellulose family, the fibrous material wide material sources, can with multiple low molecular reaction, be an aspect of High hydrophilous resin development over past ten years.
Nano composite material is normally defined in two-phase or multiphase mixture, has the matrix material of the unidimensional scale (as length, width or thickness) of a phase less than 100 nanometers (nm) at least.Inorganic nano-particle can be divided into three types by its form: (1) sphere, as nano silicon, zinc oxide and aluminum oxide etc.; (2) sheet is as layered silicate (montmorillonite, kaolin etc.), layered double-hydroxide; (3) fibrous, as carbon nanotube and sepiolite etc.At current material science, a developing direction brand-new, that have a extensive future is design and preparation organic-inorganic nanocomposite.The size that reduces inorganic phase can greatly increase interfacial area between organic phase and the inorganic phase to nanoscale, give nano composite material aspect physical and chemical performances such as mechanics, heat, electricity and magnetic than the more excellent material property of single organic or inorganic component.
Summary of the invention
The purpose of this invention is to provide a kind of High hydrophilous resin/inorganic nanometer particle compesite.
Another object of the present invention provides the preparation method of High hydrophilous resin/inorganic nanometer particle compesite.
Application for Field such as the preparation method that an also purpose of the present invention provides High hydrophilous resin/inorganic nanometer particle compesite keeps a full stand of seedings in agricultural, sanitary material, petrochemical complex, environment protection.
The content of the inorganic nano-particle in water-absorbing resin/inorganic nanometer particle compesite of the present invention is 0.05～50wt%, and preferred content is 0.1～50wt%, and more preferably content is 0.5～20wt%.
The preparation of High hydrophilous resin/inorganic nanometer particle compesite of the present invention is: at first inorganic nano-particle is distributed in the acrylic acid aqueous solution (degree of neutralization is 5-40%), add a certain amount of copolymerization matrix, initiator and linking agent after after dispersion liquid stir process for some time, feed nitrogen and fully stirring, be warming up to 30-75 ℃ of following stirring reaction 2-8 hour.Promptly obtained High hydrophilous resin/inorganic nanometer particle compesite product after taking out reaction product washing, drying, pulverizing.This nano composite material has excellent absorption properties, good water retention property and lower vinylformic acid residual quantity.The super absorbent resin resin composite material that contains inorganic nano-particle can be used for the applied various fields of conventional High hydrophilous resin.
The preparation method of High hydrophilous resin/inorganic nanometer particle compesite of the present invention carries out in the following order:
(a) a certain amount of inorganic nano-particle is distributed in vinylformic acid (degree of neutralization the is 5-40%) aqueous solution, normal temperature stirred 1～2 hour down, promptly obtained the inorganic nanoparticle dispersion liquid that concentration is 0.5～20wt%;
(b) selectable copolymerization matrix, initiator and linking agent are joined in the dispersion liquid that step (a) obtains, feed nitrogen, be warming up to 30-75 ℃ of following stirring reaction 2-8 hour.
(c) promptly obtained High hydrophilous resin/inorganic nanometer particle compesite product after the reaction product washing that step (b) is obtained, drying, the pulverizing.
Described inorganic nano-particle comprises nano spherical particle, as nano silicon, zinc oxide and aluminum oxide etc.; The flake nano particle is as layered silicate (montmorillonite, kaolin etc.), layered double-hydroxide; And the fibrous nano particle, as carbon nanotube and sepiolite etc.And one or more the mixture in the above-mentioned nanoparticle.
Characteristics of the present invention are:
1) fabricating technology of the present invention is simple, can carry out in the ready-made processing unit of High hydrophilous resin synthetic, need not transform existing equipment.
2) the High hydrophilous resin excellent absorption properties has been given in the adding of inorganic nano-particle, has improved the gel-strength of High hydrophilous resin simultaneously, and is significant for the water-retentivity that improves High hydrophilous resin.
Embodiment
Embodiment 1
In there-necked flask, add vinylformic acid 80g (adjusting degree of neutralization to about 20% with sodium hydroxide in advance) and N; N '-methylene-bisacrylamide 0.03g; add the 5g na-montmorillonite; feed nitrogen after mixing 2h; continue to stir and be heated to predetermined temperature of reaction with water-bath; add Potassium Persulphate initiator 0.6g; reacted about 4 hours in water-bath about 65 ℃ and nitrogen protection and under stirring; be incubated half an hour, obtain crude product, pulverize the back washing with alcohol; remove ethanol in 60 ℃ of following vacuum-dryings to constant weight; desciccate is pulverized with pulverizer, finally obtains white powder shape product, is polyacrylic acid/montmorillonite nano-composite material of the present invention.After tested, the receptivity of matrix material is as follows:
Inhale deionized water 2200g/g, absorb physiological saline and reach 215g/g;
Embodiment 2
In there-necked flask, add vinylformic acid 80g (adjusting degree of neutralization to about 20% with sodium hydroxide in advance) and N; N '-methylene-bisacrylamide 0.03g; add the 6g nano-calcium carbonate; feed nitrogen after mixing 2h; continue to stir and be heated to predetermined temperature of reaction with water-bath; add Potassium Persulphate initiator 0.6g; reacted about 4 hours in water-bath about 65 ℃ and nitrogen protection and under stirring; be incubated half an hour, obtain crude product, pulverize the back washing with alcohol; remove ethanol in 60 ℃ of following vacuum-dryings to constant weight; desciccate is pulverized with pulverizer, finally obtains white powder shape product, is polyacrylic acid/calcium carbonate nano composite material of the present invention.After tested, the receptivity of matrix material is as follows:
Inhale deionized water 2150g/g, absorb physiological saline and reach 220g/g;
Embodiment 3
In there-necked flask, add vinylformic acid 80g (adjusting degree of neutralization to about 20% with sodium hydroxide in advance) and N; N '-methylene-bisacrylamide 0.03g; add the 6g sepiolite; feed nitrogen after mixing 2h; continue to stir and be heated to predetermined temperature of reaction with water-bath; add Potassium Persulphate initiator 0.6g; reacted about 4 hours in water-bath about 65 ℃ and nitrogen protection and under stirring; be incubated half an hour, obtain crude product, pulverize the back washing with alcohol; remove ethanol in 60 ℃ of following vacuum-dryings to constant weight; desciccate is pulverized with pulverizer, finally obtains white powder shape product, is polyacrylic acid of the present invention/sepiolite nano composite material.After tested, the receptivity of matrix material is as follows:
Inhale deionized water 2250g/g, absorb physiological saline and reach 195g/g;
Embodiment 4
The carboxymethyl cellulose that in there-necked flask, adds 10g; 5g na-montmorillonite and a certain amount of deionized water; under nitrogen protection; stir and be heated to predetermined temperature of reaction with water-bath; add vinylformic acid 90g (adjusting degree of neutralization to about 30% with sodium hydroxide in advance) and N after half an hour; N '-methylene-bisacrylamide 0.03g; after mixing; add Potassium Persulphate initiator 0.6g; reacted about 4 hours in water-bath about 65 ℃ and nitrogen protection and under stirring; be incubated half an hour; obtain crude product; pulverize the back and use washing with alcohol, remove ethanol in 60 ℃ of following vacuum-dryings to constant weight, desciccate is pulverized with pulverizer; finally obtain white powder shape product, be carboxymethyl cellulose grafted polyacrylic acid/montmorillonite nano-composite material of the present invention.After tested, the receptivity of matrix material is as follows:
Inhale deionized water 1250g/g, absorb physiological saline and reach 105g/g;
Embodiment 5
The W-Gum that in there-necked flask, adds 10g; 5g na-montmorillonite and a certain amount of deionized water; under nitrogen protection; stir and be heated to predetermined temperature of reaction with water-bath; add vinylformic acid 90g (adjusting degree of neutralization to about 30% with sodium hydroxide in advance) and N after half an hour; N '-methylene-bisacrylamide 0.03g; after mixing; add ceric ammonium nitrate initiator 0.5g; reacted about 4 hours in water-bath about 65 ℃ and nitrogen protection and under stirring; be incubated half an hour; obtain crude product; pulverize the back and use washing with alcohol, remove ethanol in 60 ℃ of following vacuum-dryings to constant weight, desciccate is pulverized with pulverizer; finally obtain white powder shape product, be starch-grafted polyacrylic acid/montmorillonite nano-composite material of the present invention.After tested, the matrix material receptivity is as follows:
Inhale deionized water 1050g/g, absorb physiological saline and reach 85g/g;
Embodiment 6
The W-Gum that in there-necked flask, adds 10g; 5g nano-calcium carbonate and a certain amount of deionized water; under nitrogen protection; stir and be heated to predetermined temperature of reaction with water-bath; add vinylformic acid 90g (adjusting degree of neutralization to about 30% with sodium hydroxide in advance) and N after half an hour; N '-methylene-bisacrylamide 0.03g; after mixing; add ceric ammonium nitrate initiator 0.5g; reacted about 4 hours in water-bath about 65 ℃ and nitrogen protection and under stirring; be incubated half an hour; obtain crude product; pulverize the back and use washing with alcohol, remove ethanol in 60 ℃ of following vacuum-dryings to constant weight, desciccate is pulverized with pulverizer; finally obtain white powder shape product, be starch-grafted polyacrylic acid/calcium carbonate nano composite material of the present invention.After tested, the matrix material receptivity is as follows:
Inhale deionized water 1250g/g, absorb physiological saline and reach 86g/g;
Embodiment 7
The W-Gum that in there-necked flask, adds 10g; 4g titanium dioxide and a certain amount of deionized water; under nitrogen protection; stir and be heated to predetermined temperature of reaction with water-bath; add vinylformic acid 90g (adjusting degree of neutralization to about 40% with sodium hydroxide in advance) and N after half an hour; N '-methylene-bisacrylamide 0.03g; after mixing; add ceric ammonium nitrate initiator 0.5g; reacted about 4 hours in water-bath about 65 ℃ and nitrogen protection and under stirring; be incubated half an hour; obtain crude product; pulverize the back and use washing with alcohol, remove ethanol in 60 ℃ of following vacuum-dryings to constant weight, desciccate is pulverized with pulverizer; finally obtain white powder shape product, be starch-grafted polyacrylic acid/titanic oxide nano compound material of the present invention.After tested, the matrix material receptivity is as follows:
Inhale deionized water 1050g/g, absorb physiological saline and reach 85g/g;
Embodiment 8
The W-Gum that in there-necked flask, adds 10g; 4g silicon-dioxide and a certain amount of deionized water; under nitrogen protection; stir and be heated to predetermined temperature of reaction with water-bath; add vinylformic acid 90g (adjusting degree of neutralization to about 40% with sodium hydroxide in advance) and N after half an hour; N '-methylene-bisacrylamide 0.03g; after mixing; add ceric ammonium nitrate initiator 0.5g; reacted about 4 hours in water-bath about 65 ℃ and nitrogen protection and under stirring; be incubated half an hour; obtain crude product; pulverize the back and use washing with alcohol, remove ethanol in 60 ℃ of following vacuum-dryings to constant weight, desciccate is pulverized with pulverizer; finally obtain white powder shape product, be starch-grafted polyacrylic acid/silicon dioxide nano composite material of the present invention.After tested, the matrix material receptivity is as follows:
Inhale deionized water 1160g/g, absorb physiological saline and reach 95g/g.
Claims (9)
1. a novel High hydrophilous resin/inorganic nanometer particle compesite is characterized in that: the nanoparticle that contains the 0.05～60wt% that has an appointment in this High hydrophilous resin.
2. High hydrophilous resin/inorganic nanometer particle compesite according to claim 1 is characterized in that: the content of described nanoparticle is 0.1～60wt%.
3. High hydrophilous resin/inorganic nanometer particle compesite according to claim 2 is characterized in that: the content of described nanoparticle is 0.5～20wt%.
4. according to claim 1,2 or 3 described nano composite materials, it is characterized in that: described inorganic nano-particle is the laminar silicic acid salt, as natural montmorillonite, na-montmorillonite, ca-montmorillonite, lithium base montmorillonite, acidifying montmorillonite, synthetic montmorillonite), one or more the mixture in the organically-modified thing of rectorite leng, talcum powder and above-mentioned layered silicate, and nano titanium oxide, silicon-dioxide, zinc oxide, lime carbonate etc. and above-mentioned mixture.
5. the preparation method according to each described nano composite material of claim 1～4 is characterized in that, this method is carried out in the following order:
(a) nanoparticle is distributed in the acrylic acid aqueous solution (degree of neutralization is 5-40%), stirs, obtain the nanoparticle dispersion liquid that concentration is 0.5～20wt%;
(b) selectable copolymerization matrix, initiator and linking agent are joined in the dispersion liquid that step (a) obtains, feed nitrogen, be warming up to 30-75 ℃ of following stirring reaction 2-8 hour.
(c) promptly obtained High hydrophilous resin/inorganic nanometer particle compesite product after the washing of taking-up reaction product, drying, the pulverizing.
6. method according to claim 5 is characterized in that: described initiator comprises: Potassium Persulphate, ammonium persulphate, ceric ammonium nitrate, potassium permanganate, hydrogen peroxide/Sulfothiorine, Diisopropyl azodicarboxylate etc. and above-mentioned mixture.
7. method according to claim 5 is characterized in that: described linking agent is N, N '-methylene-bisacrylamide.
8. method according to claim 5 is characterized in that: described copolymerization matrix is starch and starch derivative, Mierocrystalline cellulose and derivatived cellulose and acrylamide.
9. according to the purposes of each described super absorbent resin resin composite material of claim 1～4, it is characterized in that: described High hydrophilous resin/inorganic nano composite material is applied to fields such as agricultural are kept a full stand of seedings, sanitary material, petrochemical complex, environment protection.
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