CN107011910A - One kind is containing bentonitic degradability super absorbent resin lipid microspheres and preparation method thereof - Google Patents
One kind is containing bentonitic degradability super absorbent resin lipid microspheres and preparation method thereof Download PDFInfo
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- CN107011910A CN107011910A CN201710181985.6A CN201710181985A CN107011910A CN 107011910 A CN107011910 A CN 107011910A CN 201710181985 A CN201710181985 A CN 201710181985A CN 107011910 A CN107011910 A CN 107011910A
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- absorbent resin
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/40—Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
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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
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K2101/00—Agricultural use
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
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Abstract
Contain bentonitic degradability super absorbent resin lipid microspheres the invention discloses one kind, and its preparation technology, it is characterized in that, with starch, acrylic acid, acrylamide, potassium persulfate solution, Span 80, N, N' methylene-bisacrylamides, itaconic acid, ammonium ceric nitrate, attapulgite, bentonite, humic acid, zeolite, bacillus etc. are raw material.The present invention is using potassium peroxydisulfate as initiator, with N, N' methylene-bisacrylamides are crosslinking agent, and itaconic acid is prepared for a kind of composite highly-absorbent resin with acrylic amide graft copolymerization, with good water holding capacity, the addition of attapulgite improves the salt-resistance of high hydroscopic resin.Bentonite can improve soil texture, improve water conservation drought resisting, the fertilizer conservation getting fat ability of soil;The water absorption rate, water retention property and heat endurance of high hydroscopic resin are improved simultaneously;It is combined with humic acid, zeolite, bacillus and is prepared for soil conditioner, is can adjust soil acidity or alkalinity, buffering soil value, improve crop yield.
Description
Technical field
The present invention relates to high hydroscopic resin field, and in particular to one kind is micro- containing bentonitic degradability high hydroscopic resin
Ball, and its preparation technology.
Background technology
High hydroscopic resin is a kind of high molecular polymer containing strong absorptive group of lower crosslink density, is made by being hydrated
It is in gel with substantial amounts of water is promptly absorbed, with good water absorbing properties, water retention property, and water absorption capacity is big, inhale
Water speed rate is fast, water holding capacity is strong.It is widely used in recent years agricultural, health, building etc. are multi-field.
Reverb woods et al. is in its paper《The preparation technology of micron order degradability super absorbent resin lipid microspheres》In one text, to form sediment
Powder is raw material with acrylic acid/acrylamide, using the method for graft copolymerization, is prepared in the inverse suspension system of low oil-water ratio micro-
The degradable super absorbent resin lipid microspheres of meter level, inquired into oil-water ratio, degree of neutralization, dispersant,
The influence of initiator, crosslinking agent to resin property.
The present invention is with N, and N'- methylene-bisacrylamides are crosslinking agent, using potassium peroxydisulfate as initiator, itaconic acid and propylene
Acid amide-grafted copolymerization is prepared for a kind of composite highly-absorbent resin, with good water holding capacity, and the addition of attapulgite is improved
The salt-resistance of high hydroscopic resin.Bentonite can improve the structure of soil, improve water conservation drought resisting, the fertilizer conservation getting fat ability of soil;Together
When, bentonitic addition also improves the water absorption rate, water retention property and heat endurance of high hydroscopic resin;By itself and humic acid, boiling
Stone, bacillus are compound to prepare a kind of soil conditioner, available for regulation soil acidity or alkalinity, buffering soil value, Jin Erti
High crop yield.
The content of the invention
The present invention solves the technical problem of provide it is a kind of containing bentonitic degradability super absorbent resin lipid microspheres and
Its preparation technology, the super absorbent resin lipid microspheres prepared according to the technique have good water imbibition, water-retaining property, degradable.
The technical problems to be solved by the invention are realized using following technical scheme:
Starch 20-30, acrylic acid 15-20, acrylamide 10-15, potassium persulfate solution 3-6, Span 80 4-7, N, N'- methylenes
Base bisacrylamide 2-4, itaconic acid 4-7, ammonium ceric nitrate 2-5, attapulgite 6-10, bentonite 6-9, humic acid 5-7, zeolite 3-
6, bacillus 2-5, NaOH solution, hexamethylene, ethanol, distillation appropriate amount of water.
A kind of preparation method containing bentonitic degradability super absorbent resin lipid microspheres, it is characterised in that according to the following steps
Carry out:
A. by starch 1:10-20 is dissolved in distilled water, is heated to 50-60 DEG C of gelatinization, is added potassium persulfate solution after cooling, stir
Uniform A liquid is mixed, by Span80 1:15-25 is dissolved in hexamethylene, is mixed with A liquid, under nitrogen protection, stirring and emulsifying reaction 1-
2h, heating water bath is down to room temperature, goes aqueous phase, alcohol is washed 3-5 times, be dried in vacuo, grind, treat to 50-70 DEG C of reaction 3-5h
With;
B. into itaconic acid 1:3-5:15-20 adds NaOH solution, distilled water, stirs, and adds acrylamide, cerous nitrate
After ammonium, stirring 1-2h, A liquid is obtained;Acrylic acid is placed in ice bath, 1:5-10 adds after the neutralization of NaOH solution part, is mixed with A liquid
It is even, attapulgite is added, the ultrasound 1-2h at 30-40 DEG C is passed through under nitrogen, stirring and adds N, N'- methylene-bisacrylamides,
Resulting material in a, stirring is to being completely dissolved to obtain polymerization liquid;
C. bentonite is mixed with humic acid, 1:10-15 adds distilled water, stirs, and tune pH is 8-9, adds zeolite, bud
Spore bacillus, the sonic oscillation 2-4h at 30-40 DEG C, freeze-drying is ground, and crosses 100-200 mesh sieves, stand-by;
D. resulting material in b, c is mixed, sonic oscillation 1-2h is placed in ice bath, is atomized under the effect of the pressure tiny
Drop, drop enters in 100-110 DEG C of oil-soluble solution, by slow infall process, obtains product, perseverance after reaction terminates
Warm 1-2h, thus obtained microsphere pulverizes and sieves through centrifuging after 80-90 DEG C of dry 8-12h, produces super absorbent resin lipid microspheres.
Potassium persulfate solution concentration is 10-15% in step a;Attapulgite described in step b, soaks in 60-70 DEG C of acid solution
Bubble processing 1-2h, is washed with distilled water to pH=6-7,100-110 DEG C of drying for standby;NaOH concentration of aqueous solution is described in step b
30-35%。
The reaction mechanism of the present invention is as follows:
(1)The present invention is with N, and N'- methylene-bisacrylamides are initiator, using ammonium persulfate as crosslinking agent, itaconic acid and propylene
Acid amide-grafted copolymerization is prepared for a kind of composite highly-absorbent resin, with good water holding capacity, and the addition of attapulgite is improved
The salt-resistance of high hydroscopic resin.
(2)Bentonite can improve the structure of soil, improve water conservation drought resisting, the fertilizer conservation getting fat ability of soil;Meanwhile, bentonite
Addition also improve the water absorption rate, water retention property and heat endurance of high hydroscopic resin;By itself and humic acid, zeolite, gemma bar
Bacterium is compound to prepare a kind of soil conditioner, and available for regulation soil acidity or alkalinity, buffering soil value, and then produce are made in raising
Amount.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment
One kind contains bentonitic degradability super absorbent resin lipid microspheres, is made by the raw material of following weight parts (g):
Starch 30, acrylic acid 20, acrylamide 15, potassium persulfate solution 6, Span804, N, N'- methylene-bisacrylamides 2,
Itaconic acid 7, ammonium ceric nitrate 5, attapulgite 10, bentonite 9, humic acid 7, zeolite 6, bacillus 5, NaOH solution, hexamethylene,
Ethanol, distillation appropriate amount of water.
A kind of preparation method containing bentonitic degradability super absorbent resin lipid microspheres, it is characterised in that according to the following steps
Carry out:
A. by starch 1:20 are dissolved in distilled water, are heated to 50-60 DEG C of gelatinization, and potassium persulfate solution is added after cooling, and stirring is equal
It is even to obtain A liquid, by Span80 1:15 are dissolved in hexamethylene, are mixed with A liquid, under nitrogen protection, and stirring and emulsifying reaction 1h, water-bath adds
Heat is down to room temperature, goes aqueous phase, alcohol is washed 3 times, be dried in vacuo, grind to 60-70 DEG C of reaction 3h, stand-by;
B. into itaconic acid 1:5:20 add NaOH solution, distilled water, stir, and add acrylamide, ammonium ceric nitrate, stir
Mix after 1h, obtain A liquid;Acrylic acid is placed in ice bath, 1:10 add after the neutralization of NaOH solution part, are well mixed, add recessed with A liquid
Convex rod soil, the ultrasound 1h at 30-40 DEG C is passed through nitrogen, and stirring is lower to add gains in N, N'- methylene-bisacrylamides, a
Material, stirring is to being completely dissolved to obtain polymerization liquid;
C. bentonite is mixed with humic acid, 1:15 add distilled water, stir, and tune pH is 8-9, adds zeolite, gemma bar
Bacterium, the sonic oscillation 2h at 30-40 DEG C, freeze-drying is ground, and crosses 100 mesh sieves, stand-by;
D. resulting material in b, c is mixed, sonic oscillation 2h is placed in ice bath, and tiny liquid is atomized under the effect of the pressure
Drop, drop enters in 100-110 DEG C of oil-soluble solution, by slow infall process, obtains product, and reaction terminates rear constant temperature
1h, thus obtained microsphere pulverizes and sieves through centrifuging after 80-90 DEG C of dry 10h, produces super absorbent resin lipid microspheres.
Claims (5)
1. one kind contains bentonitic degradability super absorbent resin lipid microspheres, it is characterised in that be made by the raw material of following weight parts:
Starch 20-30, acrylic acid 15-20, acrylamide 10-15, potassium persulfate solution 3-6, Span 80 4-7, N, N'- methylenes
Base bisacrylamide 2-4, itaconic acid 4-7, ammonium ceric nitrate 2-5, attapulgite 6-10, bentonite 6-9, humic acid 5-7, zeolite 3-
6, bacillus 2-5, NaOH solution, hexamethylene, ethanol, distillation appropriate amount of water.
2. a kind of preparation method containing bentonitic degradability super absorbent resin lipid microspheres according to claim 1, it is special
Levy and be, carry out according to the following steps:
A. by starch 1:10-20 is dissolved in distilled water, is heated to 50-60 DEG C of gelatinization, is added potassium persulfate solution after cooling, stir
Uniform A liquid is mixed, by Span80 1:15-25 is dissolved in hexamethylene, is mixed with A liquid, under nitrogen protection, stirring and emulsifying reaction 1-
2h, heating water bath is down to room temperature, goes aqueous phase, alcohol is washed 3-5 times, be dried in vacuo, grind, treat to 50-70 DEG C of reaction 3-5h
With;
B. into itaconic acid 1:3-5:15-20 adds NaOH solution, distilled water, stirs, and adds acrylamide, cerous nitrate
After ammonium, stirring 1-2h, A liquid is obtained;Acrylic acid is placed in ice bath, 1:5-10 adds after the neutralization of NaOH solution part, is mixed with A liquid
It is even, attapulgite is added, the ultrasound 1-2h at 30-40 DEG C is passed through under nitrogen, stirring and adds N, N'- methylene-bisacrylamides,
Resulting material in a, stirring is to being completely dissolved to obtain polymerization liquid;
C. bentonite is mixed with humic acid, 1:10-15 adds distilled water, stirs, and tune pH is 8-9, adds zeolite, bud
Spore bacillus, the sonic oscillation 2-4h at 30-40 DEG C, freeze-drying is ground, and crosses 100-200 mesh sieves, stand-by;
D. resulting material in b, c is mixed, sonic oscillation 1-2h is placed in ice bath, is atomized under the effect of the pressure tiny
Drop, drop enters in 100-110 DEG C of oil-soluble solution, by slow infall process, obtains product, perseverance after reaction terminates
Warm 1-2h, thus obtained microsphere pulverizes and sieves through centrifuging after 80-90 DEG C of dry 8-12h, produces super absorbent resin lipid microspheres.
3. a kind of preparation method containing bentonitic degradability super absorbent resin lipid microspheres according to claim 2, it is special
Levy and be, potassium persulfate solution concentration is 10-15% in step a.
4. a kind of preparation containing bentonitic degradability super absorbent resin lipid microspheres according to claim 2
Method, it is characterised in that attapulgite described in step b, the immersion treatment 1-2h in 60-70 DEG C of acid solution uses distilled water
Wash to pH=6-7,100-110 DEG C of drying for standby.
5. a kind of preparation containing bentonitic degradability super absorbent resin lipid microspheres according to claim 2
Method, it is characterised in that NaOH concentration of aqueous solution described in step b is 30-35%.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108822865A (en) * | 2018-07-11 | 2018-11-16 | 合肥达户电线电缆科技有限公司 | A kind of high-efficiency environment friendly moisturizer |
CN109429806A (en) * | 2018-12-14 | 2019-03-08 | 重庆城市管理职业学院 | A kind of water storage Gardening flowerpot |
CN110665049A (en) * | 2019-10-25 | 2020-01-10 | 石家庄亿生堂医用品有限公司 | Method for preparing hemostatic starch microspheres by ultrasonic |
CN111793169A (en) * | 2020-08-11 | 2020-10-20 | 李方 | High-salt-tolerance super absorbent resin and preparation process thereof |
CN115650671A (en) * | 2022-10-31 | 2023-01-31 | 辰龙新材料科技发展(山东)有限公司 | High-ductility white cement-based rapid closed spraying material and preparation method thereof |
WO2023173735A1 (en) * | 2022-03-17 | 2023-09-21 | 山东省林业科学研究院 | Biological water-retaining material, and preparation method therefor and use thereof |
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CN102250276A (en) * | 2011-05-10 | 2011-11-23 | 中国科学院兰州化学物理研究所 | Clay-based amphoteric hydrophobic salt-resistant and high water absorbent resin and its preparation method |
CN103694052A (en) * | 2013-12-23 | 2014-04-02 | 营口博科环保材料有限公司 | Multiple-effect super absorbent resin fertilizer and manufacturing method thereof |
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CN102250276A (en) * | 2011-05-10 | 2011-11-23 | 中国科学院兰州化学物理研究所 | Clay-based amphoteric hydrophobic salt-resistant and high water absorbent resin and its preparation method |
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108822865A (en) * | 2018-07-11 | 2018-11-16 | 合肥达户电线电缆科技有限公司 | A kind of high-efficiency environment friendly moisturizer |
CN109429806A (en) * | 2018-12-14 | 2019-03-08 | 重庆城市管理职业学院 | A kind of water storage Gardening flowerpot |
CN109429806B (en) * | 2018-12-14 | 2021-03-30 | 重庆城市管理职业学院 | Water storage gardening flowerpot |
CN110665049A (en) * | 2019-10-25 | 2020-01-10 | 石家庄亿生堂医用品有限公司 | Method for preparing hemostatic starch microspheres by ultrasonic |
CN110665049B (en) * | 2019-10-25 | 2022-02-01 | 石家庄亿生堂医用品有限公司 | Method for preparing hemostatic starch microspheres by ultrasonic |
CN111793169A (en) * | 2020-08-11 | 2020-10-20 | 李方 | High-salt-tolerance super absorbent resin and preparation process thereof |
CN111793169B (en) * | 2020-08-11 | 2021-09-17 | 乐清市川嘉电气科技有限公司 | High-salt-tolerance super absorbent resin and preparation process thereof |
WO2023173735A1 (en) * | 2022-03-17 | 2023-09-21 | 山东省林业科学研究院 | Biological water-retaining material, and preparation method therefor and use thereof |
CN115650671A (en) * | 2022-10-31 | 2023-01-31 | 辰龙新材料科技发展(山东)有限公司 | High-ductility white cement-based rapid closed spraying material and preparation method thereof |
CN115650671B (en) * | 2022-10-31 | 2023-04-14 | 辰龙新材料科技发展(山东)有限公司 | High-ductility white cement-based rapid closed spraying material and preparation method thereof |
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