CN102391512A - Organic-inorganic composite water-absorbing material based on polyaspartic acid and nano montmorillonite and preparation method thereof - Google Patents
Organic-inorganic composite water-absorbing material based on polyaspartic acid and nano montmorillonite and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an organic-inorganic composite water-absorbing material based on polyaspartic acid and nano montmorillonite and a preparation method thereof. The preparation method of the composite material can be carried out by two modes such as an in-situ polymerization method and physical blending and modification. In the in-situ polymerization method, a product is prepared by carrying out in-situ polymerization on montmorillonite and L-aspartic acid of polyaspartic acid monomer, and comprises the following components in parts by weight: 100 parts of L-aspartic acid and 2-10 parts of nano montmorillonite. In the blending and modification of the polyaspartic acid/nano montmorillonite, the improvement on the mechanical performance of polyaspartic acid resin is realized by the modification action of the montmorillonite on the polyaspartic acid, and the obtained product comprises the following components in parts by weight: 100 parts of polyaspartic acid and 2-15 parts of nano montmorillonite. The high-performance polyaspartic acid/nano montmorillonite composite material provided by the invention has the advantages of convenience in preparation, excellent water-absorbing performance, high water-absorbing rate, strong repeated water-absorbing capability, good salt resistance and high impact resistance and the like, and can be used for the fields of high-molecular water-absorbing materials and sand fixing agents and the like.
Description
Technical field
The present invention relates to a kind of high-performance organic-inorganic composite absorbent material and preparation method thereof, particularly relate to nano montmorillonite modified SAP 73 composite absorbent material and preparation method thereof.
Background technology
Along with science and technology development, to the application performance requirement raising day by day of polymer materials.People when constantly developing novel high molecular polymer, more modifications that lay particular emphasis on through research known polymer material more prepare have new function matrix material to satisfy the demands.Wherein, nano composite polymer-montmorillonoid material is present emerging a kind of polymer base inorganic nano-composite material, compares with conventional matrix material, has few, good thermostability of packing volume mark and dimensional stability, cost performance advantages of higher.Because can forming nano level in polymkeric substance, disperses montmorillonite layer, so the adding of polynite all improves significantly intensity, modulus, barrier property and the thermotolerance etc. of matrix material.
The super absorbent resin material is called for short high-absorbent material; It is a kind of water swelling type high molecular polymer that contains strongly hydrophilic groups such as hydroxyl, carboxyl and have certain degree of crosslinking; Have high suction and water retaining function; Its water regain is tens times and even several thousand times of sole mass, belongs to the functional polymer compound, English full name Super Absorbent Polymers (being called for short SAP).Traditional SAP has three major types by the raw material sources branch: synthesize single polymers system, starch-grafted polymerization system and cellulose graft polymerization etc., these SAP have received very big restriction because over-all properties is relatively poor on using.To the open defect that traditional SAP exists, people just are being devoted to the compoundization functionalization research of SAP.Concentrate at present and how to improve its water-retaining capacity under the load-bearing situation and inhale the electrolyte solution ability, exploitation absorbent composites and copoly type water-absorbing resin are a kind of domestic methods.
SAP 73, molecular formula are C
4H
6NO
3(C
4H
5NO
3)
nC
4H
6NO
4, be a kind of biodegradable, nontoxic, do not destroy ecotope, be described as the new bio based high molecular material of " green " article by people.As water-absorbing material, require it to have higher relative molecular weight, be generally 8000-200000, the SAP 73 in this molecular weight ranges has the water absorbent rate height, and rate of water absorption is fast, and degraded product does not produce characteristics such as detrimentally affect to environment and body.People such as Tan Tianwei utilize the thermal condensation of L-aspartic acid to prepare intermediate product polysuccinimide (PSI) in Preparation and Water Absorbent Behavior of Superabsorbent Polyaspartic Acid Resin one literary composition; Hydrolysis PSI under alkaline condition then; Neutralization; Hydrolyzed solution slowly poured in saturated methyl alcohol-sodium chloride solution precipitate; Filter, dry under vacuum tightness 0.095MPa, 40 ℃ of conditions, obtain the SAP 73 powder of molecular weight in the 1000-200000 scope.Narrated a kind of preparation method of high molecular weight polyasparagic acid among the CN1869100A.It is to be raw material with the aspartic acid, adds catalyzer, and at a certain temperature, the vacuum polycondensation generates SAP 73, and it is pulverized, and repolymerization repeats this process, can make the high molecular weight polyasparagic acid of weight-average molecular weight at 20000-200000.The SAP 73 purposes very extensively relates to industries such as Treatment of Industrial Water, agricultural, medicine, household chemicals and petroleum drilling, has been the focus of present polymkeric substance research field.But it is poor, frangible that its polymkeric substance often has anti-pressure ability, and shortcomings such as water-retaining capacity decline under the load-bearing situation and suction electrolyte solution ability have had a strong impact on its application in every respect.
Polynite (Montmorillonite is called for short MMT) mining deposits is very abundant, cheap, and excellent property can be used for multiple industries such as light industry, oil, metallurgy, desertification control, WWT, medicine, is described as by people " universal material ".Nano imvite has good dispersing property; Can widespread use macromolecular material industry as the additive of nanometer polymer macromolecular material; Improve shock resistance, antifatigue, dimensional stability and gas barrier property etc.; Thereby play the effect that strengthens the comprehensive physicals of polymkeric substance, improve the material processing characteristics simultaneously.
If SAP 73 is become matrix material with nano imvite through in-situ polymerization or physical blending, can improve the over-all properties of SAP 73 water-absorbing material to a great extent, make the SAP 73 composite absorbent material obtain more fully with widely using.
Summary of the invention
The objective of the invention is to above-mentioned deficiency, a kind of organic and inorganic composite absorbent material based on SAP 73 and nano imvite is provided to prior art.This composite absorbent material is to utilize nano imvite that the super-strong water-absorbing material SAP 73 is carried out modification to obtain; Have that preparation is convenient, water absorbing properties is excellent, rate of water absorption is high, water retention property is excellent, characteristics such as good salt tolerance and impact resistance height, it obtained more fully in each fields such as macromolecule water absorbent material, sand-fixation agents and use widely.
Another object of the present invention provides the preparation method of this composite absorbent material.
The object of the invention can be realized through following technical scheme:
A kind of preparation method of the organic and inorganic composite absorbent material based on SAP 73 and the polynite of sodium rice utilizes nano imvite through in-situ polymerization or physical blending method the SAP 73 water-absorbing material to be carried out modification.
Described nano imvite is a sodium-based montmorillonite, purity＞90%, particle diameter＜2 μ m (Zhejiang Feng Hong clay chemical industry ltd).
The described method for preparing SAP 73-nano imvite composite absorbent material through in-situ polymerization is:
(1) 2-10 weight part nano imvite is scattered in the deionized water of 20 times of quality, high-speed stirring 0.5-4h forms stable suspension, adds the H of L-aspartic acid 100 weight parts, 15-30ml 85% successively to nano imvite suspension-s
3PO
4Solution, 0.1-0.2 weight part linking agent N,N methylene bis acrylamide (being called for short crosslinking agent B is), ultra-sonic dispersion, logical N
2Protection, then behind the temperature reaction 1-5h, cooling, methyl alcohol is washed, is washed to neutrality, drying get final product intermediate product.
(2) above-mentioned intermediate product is pulverized hydrolysis 0.5-2h under the alkaline condition, neutralization; Hydrolyzed solution after will neutralizing is then slowly poured in the saturated solution of sodium-chlor-methyl alcohol of vigorous stirring and is precipitated, and filters, and methyl alcohol is washed repeatedly; Drying gets SAP 73/nano imvite composite absorbent material.
Wherein, described 85% H
3PO
4The preferred 25ml of solution add-on.
Preferred 0.1 weight part of described crosslinking agent B is consumption.
Described temperature of reaction is 180-220 ℃, preferred 200 ℃, and preferred 2h of reaction times.
Described alkaline condition hydrolysis is at NaOH (2mol/L) solution hydrolysis 0.5-2h, preferred 1-1.5h, and the NaOH consumption remains between the 10-12 final hydrolyzed solution pH.
Described neutralization is to utilize the neutralization of HCl solution, and degree of neutralization is 70-80%.
The described method for preparing SAP 73-nano imvite composite absorbent material through the physical blending method is: in there-necked flask, 2-15 weight part nano imvite is scattered in the deionized water of 20 times of quality; Form steady suspension with ultrasonication 0.5h; Slowly drip the aqueous solution that contains SAP 73 100 weight parts then while stirring; Back adding 0.05-0.3 weight part promotor cobalt octoate stirs; Continue to stir 12h, rotate 20-30min in the rotary evaporation in vacuo appearance under temperature 50-55 ℃, under vacuum condition, naturally cooling to room temperature behind the baking 48h under 60 ℃ of vacuum conditions at last.
Wherein, described SAP 73 relative molecular mass is between 100000-200000.Multiple compound method capable of using prepares voluntarily, screens the SAP 73 of suitable molecular weight then, also can buy corresponding commercially available SAP 73 product.
The preferred 0.1g of described promotor add-on.
A kind of SAP 73-nano imvite composite absorbent material that utilizes described in-situ polymerization to prepare.
A kind of SAP 73-nano imvite composite absorbent material that utilizes described physical blending method to prepare.
Beneficial effect:
The present invention utilizes nano imvite that SAP 73 is carried out modification, not only can improve the gel-strength of SAP 73 water-absorbing material, makes its compressive property, dimensional stability etc. obtain effective improvement.Simultaneously, improved the salt resistant character of SAP 73 water-absorbing material.
SAP 73 water absorbing properties through modification is excellent, rate of water absorption is high, water retention property is excellent, and especially salt tolerance and gel-strength are greatly improved, and makes the polyaspartic acid composite absorbent material obtain more fully with widely using.
The performance test mode is following:
The mensuration of suction multiple: the 1g dry sample is put into the beaker of 500mL, add deionized water or w
NaCl=0.009 salt solution makes the abundant imbibition of sample, and till no longer increasing to quality, this moment, sample reached the imbibition balance, with 100 order stainless steel sifts filtrations, weighing, was calculated as follows the balance imbibition multiple (Q) of water-absorbent composite material:
Q＝(G
2-G
1)/G
1
In the formula: G
1---dry sample quality (g); G
2---suction back sample quality (g).
The test of water retention property: its water regain C is surveyed in the saturated back of 1g sample suction
1, water absorbent gel is placed the centrifugal 10min of whizzer (rotating speed 2800r/min, centrifugal acceleration 8589m/s
2) after survey its residue water regain C again
2, try to achieve material water retention (R).
R＝(C
2/C
1)×100％
Gel-strength: utilize falling-ball viscometer to estimate gel-strength.Judge 25 ℃ of lower sphere landing times in gel.
Prepared SAP 73-nano imvite composite absorbent material water absorbing properties is excellent, rate of water absorption is high, water retention property is excellent, and salt tolerance and gel-strength are greatly improved.
Embodiment
Below in conjunction with specific examples the present invention being prepared SAP 73-nano imvite composite absorbent material specifically specifies.
Situ aggregation method prepares SAP 73-nano imvite composite absorbent material
Embodiment 1
The 2g nano imvite is scattered in the deionized water of 20 times of quality, high-speed stirring 0.5h forms stable suspension, adds the H of L-aspartic acid 100g, 25ml 85% successively to MMT suspension-s
3PO
4Solution, 0.1g crosslinking agent B is, ultra-sonic dispersion, logical N
2The protection, be warming up to then 200 ℃ the reaction 2h after, the cooling, methyl alcohol is washed, is washed to neutrality, drying get final product intermediate product.
Above-mentioned intermediate product is pulverized, and at 50 ℃ of left and right sides hydrolysis 1-1.5h, the NaOH consumption remains between the 10-12 final hydrolyzed solution pH with NaOH (2mol/L) solution.With HCl neutralization, degree of neutralization is 70-80% then, the hydrolyzed solution after the neutralization is poured in the saturated solution of sodium-chlor-methyl alcohol of vigorous stirring to precipitate; Filter; Methyl alcohol is washed repeatedly, under 40 ℃ of air blast conditions of temperature, dries, and gets SAP 73-nano imvite composite absorbent material.
Embodiment 2
The 5g nano imvite is scattered in the deionized water of 20 times of quality, high-speed stirring 0.5h forms stable suspension, adds the H of L-aspartic acid 100g, 25ml 85% successively to MMT suspension-s
3PO
4Solution, 0.1g crosslinking agent B is, ultra-sonic dispersion, logical N
2The protection, be warming up to then 200 ℃ the reaction 2h after, the cooling, methyl alcohol is washed, is washed to neutrality, drying get final product intermediate product.
Above-mentioned intermediate product is pulverized, and at 50 ℃ of left and right sides hydrolysis 1-1.5h, the NaOH consumption remains between the 10-12 final hydrolyzed solution pH with NaOH (2mol/L) solution.With HCl neutralization, degree of neutralization is 70-80% then, the hydrolyzed solution after the neutralization is poured in the saturated solution of sodium-chlor-methyl alcohol of vigorous stirring to precipitate; Filter; Methyl alcohol is washed repeatedly, under 40 ℃ of air blast conditions of temperature, dries, and gets SAP 73-nano imvite composite absorbent material.
Embodiment 3
The 8g nano imvite is scattered in the deionized water of 20 times of quality, high-speed stirring 0.5h forms stable suspension, adds the H of L-aspartic acid 100g, 25ml 85% successively to MMT suspension-s
3PO
4Solution, 0.1g crosslinking agent B is, ultra-sonic dispersion, logical N
2The protection, be warming up to then 200 ℃ the reaction 2h after, the cooling, methyl alcohol is washed, is washed to neutrality, drying get final product intermediate product.
Above-mentioned intermediate product is pulverized, and at 50 ℃ of left and right sides hydrolysis 1-1.5h, the NaOH consumption remains between the 10-12 final hydrolyzed solution pH with NaOH (2mol/L) solution.With HCl neutralization, degree of neutralization is 70-80% then, the hydrolyzed solution after the neutralization is poured in the saturated solution of sodium-chlor-methyl alcohol of vigorous stirring to precipitate; Filter; Methyl alcohol is washed repeatedly, under 40 ℃ of air blast conditions of temperature, dries, and gets SAP 73-nano imvite composite absorbent material.
Embodiment 4
The 10g nano imvite is scattered in the deionized water of 20 times of quality, high-speed stirring 0.5h forms stable suspension, adds the H of L-aspartic acid 100g, 25ml 85% successively to MMT suspension-s
3PO
4Solution, 0.1g crosslinking agent B is, ultra-sonic dispersion, logical N
2The protection, be warming up to then 200 ℃ the reaction 2h after, the cooling, methyl alcohol is washed, is washed to neutrality, drying get final product intermediate product.
Above-mentioned intermediate product is pulverized, and at 50 ℃ of left and right sides hydrolysis 1-1.5h, the NaOH consumption remains between the 10-12 final hydrolyzed solution pH with NaOH (2mol/L) solution.With HCl neutralization, degree of neutralization is 70-80% then, the hydrolyzed solution after the neutralization is poured in the saturated solution of sodium-chlor-methyl alcohol of vigorous stirring to precipitate; Filter; Methyl alcohol is washed repeatedly, under 40 ℃ of air blast conditions of temperature, dries, and gets SAP 73-nano imvite composite absorbent material.
Embodiment 5
The 12g nano imvite is scattered in the deionized water of 20 times of quality, high-speed stirring 0.5h forms stable suspension, adds the H of L-aspartic acid 100g, 25ml 85% successively to MMT suspension-s
3PO
4Solution, 0.1g crosslinking agent B is, ultra-sonic dispersion, logical N
2The protection, be warming up to then 200 ℃ the reaction 2h after, the cooling, methyl alcohol is washed, is washed to neutrality, drying get final product intermediate product.
Above-mentioned intermediate product is pulverized, and at 50 ℃ of left and right sides hydrolysis 1-1.5h, the NaOH consumption remains between the 10-12 final hydrolyzed solution pH with NaOH (2mol/L) solution.With HCl neutralization, degree of neutralization is 70-80% then, the hydrolyzed solution after the neutralization is poured in the saturated solution of sodium-chlor-methyl alcohol of vigorous stirring to precipitate; Filter; Methyl alcohol is washed repeatedly, under 40 ℃ of air blast conditions of temperature, dries, and gets SAP 73-nano imvite composite absorbent material.
The physical blending legal system is equipped with SAP 73/nano imvite composite absorbent material
The preparation of SAP 73:
SAP 73 multiple compound method capable of using prepares voluntarily, screens the SAP 73 of suitable molecular weight then, also can buy corresponding SAP 73.The present invention adopts commercially available SAP 73, and relative molecular mass is (Luoyang Cai Run environment-friendly materials ltd) between 100000-200000.
Embodiment 6
In there-necked flask, 2 weight part nano imvites are scattered in the deionized water of 20 times of quality; Form steady suspension with ultrasonication 0.5h; Slowly drip the aqueous solution that contains SAP 73 100 weight parts then while stirring, the back that stirs adds 0.1g weight part promotor cobalt octoate, continues to stir 12h; Rotate 20-30min in the rotary evaporation in vacuo appearance under temperature 50-55 ℃, under vacuum condition, naturally cooling to room temperature behind the baking 48h under 60 ℃ of vacuum conditions at last.Last pulverization process obtains the organic and inorganic composite absorbent material.
Embodiment 7
In there-necked flask, 5 weight part nano imvites are scattered in the deionized water of 20 times of quality; Form steady suspension with ultrasonication 0.5h; Slowly drip the aqueous solution that contains SAP 73 100 weight parts then while stirring, the back that stirs adds 0.1g weight part promotor cobalt octoate, continues to stir 12h; Rotate 20-30min in the rotary evaporation in vacuo appearance under temperature 50-55 ℃, under vacuum condition, naturally cooling to room temperature behind the baking 48h under 60 ℃ of vacuum conditions at last.Last pulverization process obtains the organic and inorganic composite absorbent material.
Embodiment 8
In there-necked flask, 10 weight part nano imvites are scattered in the deionized water of 20 times of quality; Form steady suspension with ultrasonication 0.5h; Slowly drip the aqueous solution that contains SAP 73 100 weight parts then while stirring, the back that stirs adds 0.1g weight part promotor cobalt octoate, continues to stir 12h; Rotate 20-30min in the rotary evaporation in vacuo appearance under temperature 50-55 ℃, under vacuum condition, naturally cooling to room temperature behind the baking 48h under 60 ℃ of vacuum conditions at last.Last pulverization process obtains the organic and inorganic composite absorbent material.
Embodiment 9
In there-necked flask, 15 weight part nano imvites are scattered in the deionized water of 20 times of quality; Form steady suspension with ultrasonication 0.5h; Slowly drip the aqueous solution that contains SAP 73 100 weight parts then while stirring, the back that stirs adds 0.1g weight part promotor cobalt octoate, continues to stir 12h; Rotate 20-30min in the rotary evaporation in vacuo appearance under temperature 50-55 ℃, under vacuum condition, naturally cooling to room temperature behind the baking 48h under 60 ℃ of vacuum conditions at last.Last pulverization process obtains the organic and inorganic composite absorbent material.
Embodiment 10
In there-necked flask, 18 weight part nano imvites are scattered in the deionized water of 20 times of quality; Form steady suspension with ultrasonication 0.5h; Slowly drip the aqueous solution that contains SAP 73 100 weight parts then while stirring, the back that stirs adds 0.1g weight part promotor cobalt octoate, continues to stir 12h; Rotate 20-30min in the rotary evaporation in vacuo appearance under temperature 50-55 ℃, under vacuum condition, naturally cooling to room temperature behind the baking 48h under 60 ℃ of vacuum conditions at last.Last pulverization process obtains the organic and inorganic composite absorbent material.
Experimental example 11
The performance test of material:
With commercially available SAP 73 (PASP) is contrast, measures the water absorbing properties and the mechanical property of the matrix material of each embodiment preparation of the present invention according to national standard, and interpretation of result is as shown in table 1.
Performance relatively before and after the modification of table 1 SAP 73
Annotate: commercially available SAP 73 relative molecular mass (Luoyang Cai Run environment-friendly materials ltd) between 100000-200000 in the table.
We can find out no matter be in-situ polymerization or blending and modifying from table 1, and when polynite add-on less (5%), the water-retaining capacity of material changes very little; But surpass 5g; Water-intake rate descends very fast, and for guaranteeing the higher water-intake rate of material, the polynite addition preferably remains in the said scope.Along with the increase of polynite add-on, water retention property and suction salt solution multiplying power descend to some extent, and this is because the content step-down of hydrophilic radical causes in the material.In sum, in said polynite add-on scope, the adding of polynite has not only improved gel-strength, and saturated absorbent time is descended to some extent, and suction salt ability also has bigger improvement.
Claims (9)
1. the organic and inorganic composite absorbent material based on SAP 73 and nano imvite is characterized in that through in-situ polymerization or blending modification method preparation.
2. a kind of organic and inorganic composite absorbent material based on SAP 73 and nano imvite according to claim 1 is characterized in that described nano imvite is a sodium-based montmorillonite, purity＞90%, particle diameter＜2 μ m.
3. a kind of organic and inorganic composite absorbent material based on SAP 73 and nano imvite according to claim 1 is characterized in that described concrete steps through the in-situ polymerization preparation are:
(1) 2-10 weight part nano imvite is scattered in the deionized water of 20 times of quality, high-speed stirring 0.5-4h forms stable suspension, adds the H of L-asparagus fern ammonia 100 weight parts, 20-30ml 85% successively to nano imvite suspension-s
3PO
4Solution, 0.1-0.2 weight part linking agent N,N methylene bis acrylamide (being called for short crosslinking agent B is), ultra-sonic dispersion, logical N
2The protection, be warming up to then 180-220 ℃ the reaction 1-5h after, the cooling, methyl alcohol is washed, is washed to neutrality, drying get final product intermediate product.
(2) above-mentioned intermediate product is pulverized hydrolysis 0.5-2h under the alkaline condition, neutralization; Hydrolyzed solution after will neutralizing is then slowly poured in the saturated solution of sodium-chlor-methyl alcohol of vigorous stirring and is precipitated, and filters, and methyl alcohol is washed repeatedly; Drying gets SAP 73/nano imvite composite absorbent material.
4. a kind of organic and inorganic composite absorbent material according to claim 3 based on SAP 73 and nano imvite; It is characterized in that described alkaline condition hydrolysis is that the NaOH consumption remains between the 10-12 final hydrolyzed solution pH at NaOH (2mol/L) solution hydrolysis 1-1.5h.
5. a kind of organic and inorganic composite absorbent material based on SAP 73 and nano imvite according to claim 3 is characterized in that described neutralization is to utilize the neutralization of HCl solution, and degree of neutralization is 70-80%.
6. a kind of organic and inorganic composite absorbent material according to claim 1 based on SAP 73 and nano imvite; It is characterized in that described concrete steps through the preparation of physical blending method are: in there-necked flask, 2-15 weight part nano imvite is scattered in the deionized water of 20 times of quality; Form steady suspension with ultrasonication 0.5h; Slowly drip the aqueous solution that contains SAP 73 100 weight parts then while stirring; Back adding 0.05-0.3 weight part promotor cobalt octoate stirs; Continue to stir 12h, rotate 20-30min in the rotary evaporation in vacuo appearance under temperature 50-55 ℃, under vacuum condition, naturally cooling to room temperature behind the baking 48h under 60 ℃ of vacuum conditions at last.
7. a kind of organic and inorganic composite absorbent material based on SAP 73 and nano imvite according to claim 9 is characterized in that described SAP 73 relative molecular mass is between 100000-200000.
8. one kind is utilized the organic and inorganic composite absorbent material that each described situ aggregation method prepares among the claim 3-5.
9. one kind is utilized the organic and inorganic composite absorbent material that each described physical blending method of modifying prepares among the claim 6-7.
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