CN105859948A - Preparing method for composite high water absorbent material - Google Patents
Preparing method for composite high water absorbent material Download PDFInfo
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- CN105859948A CN105859948A CN201610431288.7A CN201610431288A CN105859948A CN 105859948 A CN105859948 A CN 105859948A CN 201610431288 A CN201610431288 A CN 201610431288A CN 105859948 A CN105859948 A CN 105859948A
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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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
Abstract
The invention provides a preparing method for a composite high water absorbent material. The preparing method includes the steps that acrylic acid is added into water, the pH value is adjusted to 8.0-9.0, acrylamide, maleic anhydride and dimethylbenzene are added and heated, octadecanol, p-toluenesulfonic acid, n-butyl alcohol and ethyl acetate are added under the stirring condition, heated for reaction and cooled to the room temperature to obtain a mixture I; bentonite is added into water to be dispersed, acidic silica sol is added, a hydrochloric acid solution is added, the temperature is raised to 50-60 DEG C and kept for 2-6 h, and the product is cooled to the room temperature and washed with water to obtain a mixture II; the mixture I, the mixture II, N,N-methylene bisacrylamide, benzotriazole, 2,6-tertiary butyl p-cresol and ethyl alcohol are mixed and stirred for reaction, and then ammonium persulfate, azobis(isobutylamidine hydrochloride) and sodium hydrogen sulfite are added and stirred to obtain the composite high water absorbent material. The modified bentonite is applied to the high water absorbent material, the crosslinking degree of the bentonite in a polymer network, grafting reaction is more complete, and the water absorbent effect of the composite material is better.
Description
Technical field
The invention belongs to absorbent material technical field, be specifically related to the preparation method of a kind of composite high-water uptake material.
Background technology
High-absorbent material, also known as High hydrophilous resin, water-retaining agent, is a kind of merit that can absorb the deadweight hundred times extremely thousand of times of water yields
Energy macromolecular material, is the important component part of Water-saving agricultural technology.High-absorbent material mixes in soil and can the most effectively deposit
Moisture, then slowly releases water, supply root system of plant or neutron absorption by the root draft of evaporation or plant.It can increase
The water retention property of strong soil, raising efficiency of water application, improvement Soil structure, to promoting crop growth, improving germination
Rate has preferably effect, has preferably in fields such as industrial crops cultivation, desertification treatment, forestation in mountain area, urban landscapings
Application prospect.
The high-absorbent material of current more than 95% is used for physiological hygiene product, and agricultural horticultural use proportion is less than 5%, higher
Cost price be to hinder the key factor promoted at agriculture field of high-absorbent material.The high-absorbent material per kilogram of virgin resin class
Price is more than 20 yuan, and every mu of ground increase cost is more than 100 yuan, and this is difficult to accept for low value-added plantation industry.
Then research worker considers to prepare composite high-water uptake material by the cheap inorganic mineral of interpolation, wants ensureing that product reaches to use
Cost is reduced while asking.
At present, the research to mineral base composite high-water uptake material also exists following weak point: 1, mineral addition is few, to fall
The cost of low high-absorbent material has little significance；2, many to water absorbing properties research, what water-retaining property and salt tolerance considered lacks；3、
The influence factor of composite Minerals and study on mechanism are weak；, Product Process formula and actual production disconnect, grind the work that makes internal disorder or usurp
Do not fully take into account cost factor and producing feasibility.It is therefore desirable to for mineralogical character, carry out high addition, low
The mineral base composite high-water uptake material preparation of cost and performance are ground and are made internal disorder or usurp, and promote high-absorbent material pushing away in agriculture and forestry water-saving technology
Wide application, also the high value added utilization for raw mineral materials provides developing thought.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art to provide the preparation method of a kind of composite high-water uptake material, by modification
Bentonite is applied in high-absorbent material, and the soaking effect making composite is more preferable.
The preparation method of a kind of composite high-water uptake material, comprises the following steps:
Step 1, in parts by weight, adds to acrylic acid 5～12 parts in water 20～30 parts, regulates pH to 8.0～9.0,
Add acrylamide 3～9 parts, maleic anhydride 1～4 parts, dimethylbenzene 2～5 parts, heating, add 18 under agitation
Alcohol 1～5 parts, p-methyl benzenesulfonic acid 2～5 parts, n-butyl alcohol 3～7 parts, ethyl acetate 2～6 parts, be warming up to 140～150 DEG C
Reaction 8～12h, is cooled to room temperature, obtains mixture I；
Step 2, in parts by weight, bentonite 4～10 parts are added in water 15～25 parts disperse, add acidic silicasol 2～
7 parts, dripping mass concentration under the conditions of 30～40 DEG C is 1～the hydrochloric acid solution 3 of 5%～9 parts, is warming up to 50～60 DEG C of insulations
2～6 hours, let cool to room temperature, wash with water, obtain mixtures II；
Step 3, in parts by weight, by mixture I 5～10 parts, mixtures II 4～8 parts, N,N methylene bis acrylamide
3～6 parts, BTA 1～6 parts, 2,6-Butylated Hydroxytoluene 3～6 parts, ethanol 8～15 parts of mixing, 50～70
DEG C stirring reaction 1～3h, lets cool to room temperature, add Ammonium persulfate. 2～6 parts, azo-bis-isobutyrate hydrochloride 1～4 parts,
Sodium sulfite sodium 3～5 parts, stirring,.
Further, in step 1, heating-up temperature is 45～70 DEG C.
Further, in step 1, mixing speed is 300～500rpm.
Further, in step 2 bentonitic particle diameter in 10～30 μm.
Further, in step 2, rate of dispersion is 3000～5000rpm.
Further, in step 3, mixed process need to be passed through CO2。
Modified alta-mud is applied in high-absorbent material by the present invention, improves bentonite crosslinking degree in polymer network,
Making graft reaction carry out more complete, the soaking effect making composite is more preferable.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of composite high-water uptake material, comprises the following steps:
Step 1, in parts by weight, adds to 5 parts of acrylic acid in 20 parts of water, regulates pH to 8.0, adds acrylamide 3
Part, maleic anhydride 1 part, dimethylbenzene 2 parts, heating, under agitation add octadecanol 1 part, p-methyl benzenesulfonic acid 2 parts,
N-butyl alcohol 3 parts, ethyl acetate 2 parts, be warming up to 140 DEG C of reaction 12h, be cooled to room temperature, obtain mixture I；
Step 2, in parts by weight, adds to bentonite 4 parts disperse in 15 parts of water, adds acidic silicasol 2 parts, 30
Drip the hydrochloric acid solution 3 parts that mass concentration is 1% under the conditions of DEG C, be warming up to 50 DEG C and be incubated 6 hours, let cool to room temperature, use water
Washing, obtains mixtures II；
Step 3, in parts by weight, by mixture I 5 parts, mixtures II 4 parts, N,N methylene bis acrylamide 3 parts,
BTA 1 part, 2,6-Butylated Hydroxytoluene 3 parts, ethanol 8 parts mixing, 50 DEG C stirring reaction 3h, let cool to room
Temperature, adds Ammonium persulfate. 2 parts, azo-bis-isobutyrate hydrochloride 1 part, 3 parts of sodium sulfite sodium, stirring,.
Wherein, in step 1, heating-up temperature is 45 DEG C, and mixing speed is 300rpm；In step 2, bentonitic particle diameter is in 10 μm,
Rate of dispersion is 3000rpm；In step 3, mixed process need to be passed through CO2。
The water absorbent rate of gained high-absorbent material is 1430g/g, and inhaling 0.9% saline multiplying power is 132g/g.
Embodiment 2
The preparation method of a kind of composite high-water uptake material, comprises the following steps:
Step 1, in parts by weight, adds to 7 parts of acrylic acid in 23 parts of water, regulates pH to 8.5, adds acrylamide 7
Part, maleic anhydride 2 parts, dimethylbenzene 4 parts, heating, under agitation add octadecanol 3 parts, p-methyl benzenesulfonic acid 4 parts,
N-butyl alcohol 5 parts, ethyl acetate 3 parts, be warming up to 140 DEG C of reaction 10h, be cooled to room temperature, obtain mixture I；
Step 2, in parts by weight, adds to bentonite 7 parts disperse in 18 parts of water, adds acidic silicasol 5 parts, 35
Drip the hydrochloric acid solution 6 parts that mass concentration is 2% under the conditions of DEG C, be warming up to 55 DEG C and be incubated 4 hours, let cool to room temperature, use water
Washing, obtains mixtures II；
Step 3, in parts by weight, by mixture I 6 parts, mixtures II 7 parts, N,N methylene bis acrylamide 5 parts,
BTA 2 parts, 2,6-Butylated Hydroxytoluene 5 parts, ethanol 11 parts mixing, 60 DEG C stirring reaction 2h, let cool to room
Temperature, adds Ammonium persulfate. 4 parts, azo-bis-isobutyrate hydrochloride 3 parts, 4 parts of sodium sulfite sodium, stirring,.
Wherein, in step 1, heating-up temperature is 65 DEG C, and mixing speed is 400rpm；In step 2, bentonitic particle diameter is in 20 μm,
Rate of dispersion is 4000rpm；In step 3, mixed process need to be passed through CO2。
The water absorbent rate of gained high-absorbent material is 1390g/g, and inhaling 0.9% saline multiplying power is 141g/g.
Embodiment 3
The preparation method of a kind of composite high-water uptake material, comprises the following steps:
Step 1, in parts by weight, adds to 9 parts of acrylic acid in 27 parts of water, regulates pH to 8.0, adds acrylamide 5
Part, maleic anhydride 1 part, dimethylbenzene 2 parts, heating, under agitation add octadecanol 1 part, p-methyl benzenesulfonic acid 2 parts,
N-butyl alcohol 6 parts, ethyl acetate 5 parts, be warming up to 145 DEG C of reaction 9h, be cooled to room temperature, obtain mixture I；
Step 2, in parts by weight, adds to bentonite 8 parts disperse in 22 parts of water, adds acidic silicasol 5 parts, 35
Drip the hydrochloric acid solution 8 parts that mass concentration is 4% under the conditions of DEG C, be warming up to 55 DEG C and be incubated 3 hours, let cool to room temperature, use water
Washing, obtains mixtures II；
Step 3, in parts by weight, by mixture I 7 parts, mixtures II 5 parts, N,N methylene bis acrylamide 4 parts,
BTA 3 parts, 2,6-Butylated Hydroxytoluene 5 parts, ethanol 13 parts mixing, 60 DEG C stirring reaction 2h, let cool to room
Temperature, adds Ammonium persulfate. 5 parts, azo-bis-isobutyrate hydrochloride 3 parts, 4 parts of sodium sulfite sodium, stirring,.
Wherein, in step 1, heating-up temperature is 65 DEG C, and mixing speed is 400rpm；In step 2, bentonitic particle diameter is in 20 μm,
Rate of dispersion is 3500rpm；In step 3, mixed process need to be passed through CO2。
The water absorbent rate of gained high-absorbent material is 1455g/g, and inhaling 0.9% saline multiplying power is 128g/g.
Embodiment 4
The preparation method of a kind of composite high-water uptake material, comprises the following steps:
Step 1, in parts by weight, adds to 12 parts of acrylic acid in 30 parts of water, regulates pH to 9.0, adds acrylamide 9
Part, maleic anhydride 4 parts, dimethylbenzene 5 parts, heating, under agitation add octadecanol 5 parts, p-methyl benzenesulfonic acid 5 parts,
N-butyl alcohol 7 parts, ethyl acetate 6 parts, be warming up to 150 DEG C of reaction 8h, be cooled to room temperature, obtain mixture I；
Step 2, in parts by weight, adds to bentonite 10 parts disperse in 25 parts of water, adds acidic silicasol 7 parts,
Drip the hydrochloric acid solution 9 parts that mass concentration is 5% under the conditions of 40 DEG C, be warming up to 60 DEG C and be incubated 2 hours, let cool to room temperature, use
Water washs, and obtains mixtures II；
Step 3, in parts by weight, by mixture I 10 parts, mixtures II 8 parts, N,N methylene bis acrylamide 6 parts,
BTA 6 parts, 2,6-Butylated Hydroxytoluene 6 parts, ethanol 15 parts mixing, 70 DEG C stirring reaction 1h, let cool to room
Temperature, adds Ammonium persulfate. 6 parts, azo-bis-isobutyrate hydrochloride 4 parts, 5 parts of sodium sulfite sodium, stirring,.
Wherein, in step 1, heating-up temperature is 70 DEG C, and mixing speed is 500rpm；In step 2, bentonitic particle diameter is in 30 μm,
Rate of dispersion is 5000rpm；In step 3, mixed process need to be passed through CO2。
The water absorbent rate of gained high-absorbent material is 1510g/g, and inhaling 0.9% saline multiplying power is 148g/g.
Claims (6)
1. the preparation method of a composite high-water uptake material, it is characterised in that: comprise the following steps:
Step 1, in parts by weight, adds to acrylic acid 5～12 parts in water 20～30 parts, regulates pH to 8.0～9.0,
Add acrylamide 3～9 parts, maleic anhydride 1～4 parts, dimethylbenzene 2～5 parts, heating, add 18 under agitation
Alcohol 1～5 parts, p-methyl benzenesulfonic acid 2～5 parts, n-butyl alcohol 3～7 parts, ethyl acetate 2～6 parts, be warming up to 140～150 DEG C
Reaction 8～12h, is cooled to room temperature, obtains mixture I；
Step 2, in parts by weight, bentonite 4～10 parts are added in water 15～25 parts disperse, add acidic silicasol 2～
7 parts, dripping mass concentration under the conditions of 30～40 DEG C is 1～the hydrochloric acid solution 3 of 5%～9 parts, is warming up to 50～60 DEG C of insulations
2～6 hours, let cool to room temperature, wash with water, obtain mixtures II；
Step 3, in parts by weight, by mixture I 5～10 parts, mixtures II 4～8 parts, N,N methylene bis acrylamide
3～6 parts, BTA 1～6 parts, 2,6-Butylated Hydroxytoluene 3～6 parts, ethanol 8～15 parts of mixing, 50～70
DEG C stirring reaction 1～3h, lets cool to room temperature, add Ammonium persulfate. 2～6 parts, azo-bis-isobutyrate hydrochloride 1～4 parts,
Sodium sulfite sodium 3～5 parts, stirring,.
The preparation method of composite high-water uptake material the most according to claim 1, it is characterised in that: heating temperature in step 1
Degree is 45～70 DEG C.
The preparation method of composite high-water uptake material the most according to claim 1, it is characterised in that: stirring speed in step 1
Degree is 300～500rpm.
The preparation method of composite high-water uptake material the most according to claim 1, it is characterised in that: bentonite in step 2
Particle diameter in 10～30 μm.
The preparation method of composite high-water uptake material the most according to claim 1, it is characterised in that: dispersion speed in step 2
Degree is 3000～5000rpm.
The preparation method of composite high-water uptake material the most according to claim 1, it is characterised in that: step 3 mixed
Journey need to be passed through CO2。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610431288.7A CN105859948A (en) | 2016-06-16 | 2016-06-16 | Preparing method for composite high water absorbent material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108852633A (en) * | 2018-07-11 | 2018-11-23 | 合肥尚涵装饰工程有限公司 | A kind of environmental protection blotting paper |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999021897A1 (en) * | 1997-10-23 | 1999-05-06 | Innoval Management Limited | Method of preparation of products which absorb water intermolecularly |
| CN1224028A (en) * | 1998-01-18 | 1999-07-28 | 郑可省 | High hydroscopicity material of graft bentonite and its producing process |
| CN102464585A (en) * | 2010-11-01 | 2012-05-23 | 袁俊海 | Novel method for preparing hydrophobic monomer of composite water absorbing material |
-
2016
- 2016-06-16 CN CN201610431288.7A patent/CN105859948A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999021897A1 (en) * | 1997-10-23 | 1999-05-06 | Innoval Management Limited | Method of preparation of products which absorb water intermolecularly |
| CN1224028A (en) * | 1998-01-18 | 1999-07-28 | 郑可省 | High hydroscopicity material of graft bentonite and its producing process |
| CN102464585A (en) * | 2010-11-01 | 2012-05-23 | 袁俊海 | Novel method for preparing hydrophobic monomer of composite water absorbing material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108852633A (en) * | 2018-07-11 | 2018-11-23 | 合肥尚涵装饰工程有限公司 | A kind of environmental protection blotting paper |
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