CN106188404A - The formula of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting and preparation technology - Google Patents
The formula of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting and preparation technology Download PDFInfo
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- CN106188404A CN106188404A CN201610587536.7A CN201610587536A CN106188404A CN 106188404 A CN106188404 A CN 106188404A CN 201610587536 A CN201610587536 A CN 201610587536A CN 106188404 A CN106188404 A CN 106188404A
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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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Abstract
The invention discloses formula and the preparation technology of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting, it is made up of following raw material according to parts by weight: useless 25 30 parts of acrylic acid, starch 50 60 parts, potassium hydroxide solution 15 20 parts, dehydrated alcohol 30 40 parts, potassium peroxydisulfate 10 15 parts, cross-linking agent 5 10 parts, appropriate distilled water is added in soluble starch, stir into suspension, after stirring gelatinizing cooling, adding appropriate potassium peroxydisulfate, constant temperature stirs；Then being neutralized by acrylic acid potassium hydroxide solution, liquid to be neutralized is down to during room temperature add N N,Methylene-bisacrylamide, stirs；Then neutralizer is poured in gelatinized starch, stir and be passed through nitrogen and be cooled to room temperature reaction to reaction completely, obtain graft copolymer；Again copolymer is filtered, utilize absolute ethanol washing 23 times；After carrying out drying and crushing after washing and sieving, obtain light yellow crystalline super absorbent resin.The water-absorbing resins water absorption that the present invention produces, good water-retaining property of pressurizeing, and shorten technological process.
Description
Technical field
The present invention relates to water-absorbing resins preparation technology field, be specifically related to a kind of starch graft acrylic acid high-hydroscopicity tree
The formula of fat and preparation technology.
Background technology
Super absorbent resin is a kind of novel functional high molecule material, has the feature such as high-hydroscopicity, high-moisture-retention, extensively
General for industries such as agricultural gardening, physiological hygiene articles for use, building, medicine and cosmetics.Through the effort of numerous researcheres, by height
The fluid sealant that water-absorbing resins and other materials are composited, has been used for the caulking sealings such as building jointing, steel sheet pile and pipe joint,
With replacement seal and adhesives.The main chain backbone of starch grafting type esters of acrylic acid super absorbent resin is starch, its main chain
Or containing hydrophilic radical-OH-COOH and-CONH on graft side chain2Deng, through lightly crosslinked formation one, there is main chain, side chain
Three-dimensional net structure with low crosslinking degree；Owing to starch source is abundant, cheap, safety and sanitation and there is good biological fall
Solve performance it is considered to be a kind of environmental friendliness shaped material, can be widely used for agricultural gardening, physiological hygiene articles for use, building, medicine and
The fields such as cosmetics；But there is the shortcomings such as rate of water absorption is slow, salt tolerance is poor in this resinoid, thus its range of application is restricted.
Summary of the invention
For problem above, the invention provides formula and the preparation work of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting
Skill, substantially reduces technological process, and the water-absorbing resin water absorption that generates, pressurization water-retaining property are superior to be synthesized by conventional method
Product；Both remained starch itself such as cheap, wide material sources, environmental friendliness, biodegradable characteristic simultaneously, there is again synthesis
High molecular characteristic, so that starch-based product has more preferable serviceability, can effectively solve the problem in background technology.
To achieve these goals, the technical solution used in the present invention is as follows: a kind of starch graft acrylic acid high-hydroscopicity
The formula of resin, is made up of following raw material according to parts by weight:
Acrylic acid 25-30 part, starch 50-60 part, potassium hydroxide solution 15-20 part, dehydrated alcohol 30-40 part, potassium peroxydisulfate 10-
15 parts, cross-linking agent 5-10 part.
According to technique scheme, described acrylic acid is chemical pure, and potassium hydroxide, potassium peroxydisulfate are analytical pure.
According to technique scheme, described potassium hydroxide solution concentration is 25-30%.
According to technique scheme, described cross-linking agent selects N-N,Methylene-bis-acrylamide.
According to technique scheme, described starch selects soluble starch.
Additionally the present invention have also been devised the preparation technology of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting, including walking as follows
Rapid:
(1) in soluble starch, add appropriate distilled water, stir into suspension, after stirring gelatinizing cooling, add appropriate over cure
Acid potassium, constant temperature stirs；
(2) being neutralized by acrylic acid potassium hydroxide solution, control degree of neutralization is 75%-85%, and liquid to be neutralized is down to during room temperature add
N-N,Methylene-bis-acrylamide, stirs；
(3) neutralizer in step (2) is poured in gelatinized starch, stir and be passed through nitrogen and be cooled to room temperature to reaction completely
Reaction, obtains graft copolymer；
(4) graft copolymer obtained is filtered, utilize absolute ethanol washing 2-3 time；
(5), after the graft copolymer after washing being dried pulverizing and sieves, light yellow crystalline super absorbent resin is obtained.
According to technique scheme, in described step (1), gelatinization point controls at 80 DEG C, and chilling temperature controls at 45 DEG C,
Gelatinization time 1h.
According to technique scheme, in described step (3), control polymer production temperature, at 45 DEG C, is passed through nitrogen gas stirring
Time meta 2h.
According to technique scheme, controlling baking temperature in described (5) is constant temperature 80 DEG C, and dried polymer powder crosses 80
Mesh sieve.
Beneficial effects of the present invention:
The present invention is with soluble starch as primary raw material, and acrylic acid is modified monomer, and potassium peroxydisulfate is initiator and enters N-N,Sub-
Methyl-bisacrylamide is cross-linking agent, uses grafting copolymerization process to prepare starch graft acrylic acid type super absorbent resin, can save
The steps such as saponification, substantially reduce technological process, and the water-absorbing resin water absorption, the pressurization water-retaining property that generate are superior to by routine side
The product of method synthesis；Both remained starch itself such as cheap, wide material sources, environmental friendliness, biodegradable characteristic, again simultaneously
There is the high molecular characteristic of synthesis, so that starch-based product has more preferable serviceability.
Accompanying drawing explanation
Fig. 1 is the graph of relation of gelatinization point of the present invention and hydroscopicity resin energy.
Fig. 2 is the graph of relation of gelatinization time of the present invention and hydroscopicity resin energy.
Fig. 3 is the graph of relation of graft reaction temperature of the present invention and hydroscopicity resin energy.
Fig. 4 is the graph of relation of graft reaction time of the present invention and hydroscopicity resin energy.
Fig. 5 is preparation technology flow chart of the present invention.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, to the present invention
It is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not used to
Limit the present invention.
Embodiment 1:
The formula of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting, is made up of following raw material according to parts by weight:
25 parts of acrylic acid, starch 50 parts, potassium hydroxide solution 15 parts, dehydrated alcohol 30, potassium peroxydisulfate 10 parts, cross-linking agent 5 parts.
Described acrylic acid is chemical pure, and potassium hydroxide, potassium peroxydisulfate are analytical pure；Described potassium hydroxide solution concentration is
25%；Described cross-linking agent selects N-N,Methylene-bis-acrylamide；Described starch selects soluble starch.
Its preparation technology, comprises the steps:
(1) in soluble starch, add appropriate distilled water, stir into suspension, after stirring gelatinizing cooling, add appropriate over cure
Acid potassium, constant temperature stirs, and gelatinization point controls at 80 DEG C, and chilling temperature controls at 45 DEG C, gelatinization time 1h；
(2) being neutralized by acrylic acid potassium hydroxide solution, controlling degree of neutralization is 75%, and liquid to be neutralized is down to during room temperature add N-N,
Methylene-bis-acrylamide, stirs；
(3) neutralizer in step (2) is poured in gelatinized starch, stir and be passed through nitrogen and be cooled to room temperature to reaction completely
Reaction, obtains graft copolymer, controls polymer production temperature at 45 DEG C, meta 2h when being passed through nitrogen gas stirring；
(4) graft copolymer obtained is filtered, utilize absolute ethanol washing 3 times；
(5), after the graft copolymer after washing being dried pulverizing and sieves, light yellow crystalline super absorbent resin is obtained, dry
Dry temperature is constant temperature 80 DEG C, and dried polymer powder crosses 80 mesh sieves.
Embodiment 2:
The formula of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting, is made up of following raw material according to parts by weight:
27 parts of acrylic acid, starch 55 parts, potassium hydroxide solution 17 parts, dehydrated alcohol 35 parts, potassium peroxydisulfate 13 parts, cross-linking agent 8 parts.
Described acrylic acid is chemical pure, and potassium hydroxide, potassium peroxydisulfate are analytical pure；Described potassium hydroxide solution concentration is
27%；Described cross-linking agent selects N-N,Methylene-bis-acrylamide；Described starch selects soluble starch.
Its preparation technology, comprises the steps:
(1) in soluble starch, add appropriate distilled water, stir into suspension, after stirring gelatinizing cooling, add appropriate over cure
Acid potassium, constant temperature stirs, and gelatinization point controls at 85 DEG C, and chilling temperature controls at 50 DEG C, gelatinization time 0.8；
(2) being neutralized by acrylic acid potassium hydroxide solution, controlling degree of neutralization is 80%, and liquid to be neutralized is down to during room temperature add N-N,
Methylene-bis-acrylamide, stirs；
(3) neutralizer in step (2) is poured in gelatinized starch, stir and be passed through nitrogen and be cooled to room temperature to reaction completely
Reaction, obtains graft copolymer, controls polymer production temperature at 50 DEG C, meta 1.5h when being passed through nitrogen gas stirring；
(4) graft copolymer obtained is filtered, utilize absolute ethanol washing 2 times；
(5), after the graft copolymer after washing being dried pulverizing and sieves, light yellow crystalline super absorbent resin is obtained, dry
Dry temperature is constant temperature 85 DEG C, and dried polymer powder crosses 80 mesh sieves.
Embodiment 3:
The formula of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting, is made up of following raw material according to parts by weight:
30 parts of acrylic acid, starch 60 parts, potassium hydroxide solution 20 parts, dehydrated alcohol 40 parts, potassium peroxydisulfate 15 parts, cross-linking agent 10
Part.
Described acrylic acid is chemical pure, and potassium hydroxide, potassium peroxydisulfate are analytical pure；Described potassium hydroxide solution concentration is
30%；Described cross-linking agent selects N-N,Methylene-bis-acrylamide；Described starch selects soluble starch.
Its preparation technology, comprises the steps:
(1) in soluble starch, add appropriate distilled water, stir into suspension, after stirring gelatinizing cooling, add appropriate over cure
Acid potassium, constant temperature stirs, and gelatinization point controls at 75 DEG C, and chilling temperature controls at 40 DEG C, gelatinization time 1.5h；
(2) being neutralized by acrylic acid potassium hydroxide solution, controlling degree of neutralization is 85%, and liquid to be neutralized is down to during room temperature add N-N,
Methylene-bis-acrylamide, stirs；
(3) neutralizer in step (2) is poured in gelatinized starch, stir and be passed through nitrogen and be cooled to room temperature to reaction completely
Reaction, obtains graft copolymer, controls polymer production temperature at 40 DEG C, meta 2.5h when being passed through nitrogen gas stirring；
(4) graft copolymer obtained is filtered, utilize absolute ethanol washing 3 times；
(5), after the graft copolymer after washing being dried pulverizing and sieves, light yellow crystalline super absorbent resin is obtained, dry
Dry temperature is constant temperature 75 DEG C, and dried polymer powder crosses 80 mesh sieves.
By following Study on Test Method, gelatinization point, gelatinization time, graft reaction temperature and response time etc. are to tree
The impact of fat water absorbing properties.
(1) gelatinization point impact (as shown in Figure 1) on hydroscopicity resin energy
Weigh the powder super absorbent resin that 0.1g difference gelatinization point is made, put in plane ware, add 200mL distilled water
Stand 3h, after filtering quiet device dewatering 1.5h with 100 mesh nylon, water absorbent gel is placed in 5min on filter paper, takes surface moisture, weigh
It is calculated as follows water absorbent rate: m=(m1-m0)/m0.
As shown in Figure 1, the water absorption rate of resin raising in the trend fallen after rising along with starch gelatinization temperature.When gelatinizing temperature
When degree is 85 DEG C, the water absorbing capacity of resin is optimal, and this is owing to starch is in gelatinization process, when temperature is less than 85 DEG C, along with temperature
The rising of degree, the glucose molecule chain of original distortion is prone to stretch, and starch is also easy to water absorption and swelling, and after starch water absorption and swelling, structure is subject to
To destroying, increase with monomer contact area, thus the carrying out of beneficially graft reaction；When temperature is 85 DEG C, starch is fully stuck with paste
Change graft reaction and reach optimum；But, when temperature is too high, the phenomenons such as the most aging may be caused, cause graft reaction not
Good, thus affect the water absorbing capacity of resin.
(2) gelatinization time impact (as shown in Figure 2) on hydroscopicity resin energy
Weigh the powder super absorbent resin made under 0.1g difference gelatinization time, put in plane ware, add 200mL distillation
Water stands 3h, after filtering quiet device dewatering 1.5h with 100 mesh nylon, water absorbent gel is placed in 5min on filter paper, takes surface moisture, claims
Heavily it is calculated as follows water absorbent rate: m=(m1-m0)/m0.
As seen from Figure 2, the water absorption rate of resin increases in becoming of falling after rising along with the starch gelatinization time, works as gelatinizing
When time is 1h, the water absorbing capacity of resin is optimal, and this is owing to when gelatinization time is less than 1h, gelatinization time is the longest, gelatinized corn starch
Change degree is the biggest, and the activity of starch is the highest, is more conducive to the carrying out of graft polymerization reaction, and the copolymer of generation is the most, table
It it is now the water absorbing capacity increase of resin；When gelatinization time is higher than 1h, easily causes the generation of side reaction, thus destroy starch
Structure, accelerate the aging of starch, therefore water absorption rate also can reduce.
(3) the graft reaction temperature impact (as shown in Figure 3) on hydroscopicity resin energy
The powder super absorbent resin made at a temperature of weighing 0.1g difference graft reaction, puts in plane ware, adds 200mL
Distilled water stands 3h, after filtering quiet device dewatering 1.5h with 100 mesh nylon, water absorbent gel is placed in 5min on filter paper, takes surface water
Point, weigh and be calculated as follows water absorbent rate: m=(m1-m0)/m0.
As seen from Figure 3, the water absorption rate of resin raises in the trend fallen after rising along with polymerization temperature, when grafting is anti-
When to answer temperature be 60 DEG C, this is owing to when reaction temperature is relatively low, decomposition of initiator speed is relatively slow, draws to the water absorption rate of resin
Send out induction time longer, therefore the slower water absorption rate of reaction rate is relatively low；Along with the continuous rising of temperature, the decomposition rate of initiator carries
Height, chain initiation reaction and graft reaction are accelerated, and the beneficially polyreaction of monomer, grafting degree significantly improves；But, when grafting temperature
When spending high, chain transfer reaction speed and chain termination reaction speed increase, and cause local product self-crosslinking to cause percent grafting to decline,
The water absorption rate of resin reduces.
(4) the graft reaction time impact (as shown in Figure 4) on hydroscopicity resin energy
Weigh the powder super absorbent resin made under the 0.1g difference graft reaction time, put in plane ware, add 200mL
Distilled water stands 3h, after filtering quiet device dewatering 1.5h with 100 mesh nylon, water absorbent gel is placed in 5min on filter paper, takes surface water
Point, weigh and be calculated as follows water absorbent rate: m=(m1-m0)/m0.
As seen from Figure 4, the water absorption rate of resin extending in the trend fallen after rising, when reacted along with the response time
Between when being 4h, the water absorption rate of resin reaches maximum.This is due to time between when reacted less than 4h, starch and acrylic acid grafting
Copolyreaction is the slowest；Along with the prolongation in response time, graft copolymer increases, and water absorption rate increases；Between when reacted
During more than 4h, along with the further prolongation in response time, the follow-up crosslinking produced in course of reaction makes the space networks cross winding of resin
Connection excessively, thus have impact on the water absorption rate of resin.
Based on above-mentioned, it is an advantage of the current invention that the present invention with soluble starch as primary raw material, acrylic acid is modified single
Body, potassium peroxydisulfate is initiator and enters N-N,Methylene-bis-acrylamide is cross-linking agent, uses grafting copolymerization process to prepare starch and connects
Branch high absorptive resin in acrylic acid type, can save the steps such as saponification, substantially reduces technological process, and the water-absorbing resin generated is inhaled
Aqueous, pressurization water-retaining property are superior to the product synthesized by conventional method；Both remained starch such as cheap, source itself extensively simultaneously
General, environmental friendliness, biodegradable characteristic, have again the high molecular characteristic of synthesis, so that starch-based product has preferably
Serviceability.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.
Claims (9)
1. the formula of a Technologies of Water-absorbing Resin: Corn Starch Grafting, it is characterised in that according to parts by weight by following raw material
Composition:
Acrylic acid 25-30 part, starch 50-60 part, potassium hydroxide solution 15-20 part, dehydrated alcohol 30-40 part, potassium peroxydisulfate 10-
15 parts, cross-linking agent 5-10 part.
The formula of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting the most according to claim 1, it is characterised in that described
Acrylic acid is chemical pure, and potassium hydroxide, potassium peroxydisulfate are analytical pure.
The formula of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting the most according to claim 1, it is characterised in that described
Potassium hydroxide solution concentration is 25-30%.
The formula of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting the most according to claim 1, it is characterised in that described
Cross-linking agent selects N-N,Methylene-bis-acrylamide.
The formula of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting the most according to claim 1, it is characterised in that described
Starch selects soluble starch.
6. the preparation technology of a Technologies of Water-absorbing Resin: Corn Starch Grafting, it is characterised in that comprise the steps:
(1) in soluble starch, add appropriate distilled water, stir into suspension, after stirring gelatinizing cooling, add appropriate over cure
Acid potassium, constant temperature stirs；
(2) being neutralized by acrylic acid potassium hydroxide solution, control degree of neutralization is 75%-85%, and liquid to be neutralized is down to during room temperature add
N-N,Methylene-bis-acrylamide, stirs；
(3) neutralizer in step (2) is poured in gelatinized starch, stir and be passed through nitrogen and be cooled to room temperature to reaction completely
Reaction, obtains graft copolymer；
(4) graft copolymer obtained is filtered, utilize absolute ethanol washing 2-3 time；
(5), after the graft copolymer after washing being dried pulverizing and sieves, light yellow crystalline super absorbent resin is obtained.
The preparation technology of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting the most according to claim 6, it is characterised in that
In described step (1), gelatinization point controls at 80 DEG C, and chilling temperature controls at 45 DEG C, gelatinization time 1h.
The preparation technology of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting the most according to claim 6, it is characterised in that
In described step (3), control polymer production temperature at 45 DEG C, meta 2h when being passed through nitrogen gas stirring.
The preparation technology of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting the most according to claim 6, it is characterised in that
Controlling baking temperature in described (5) is constant temperature 80 DEG C, and dried polymer powder crosses 80 mesh sieves.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106883350A (en) * | 2017-03-07 | 2017-06-23 | 吴肖颜 | A kind of preparation method of degradable high-efficiency water-absorbing resin |
| CN109337015A (en) * | 2018-10-25 | 2019-02-15 | 南京财经大学 | A kind of rice starch water absorbing agent |
| 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 |
| CN110078940A (en) * | 2019-04-26 | 2019-08-02 | 池州学院 | A kind of preparation method of BIOLOGICAL CALCIUM composite high-water-absorptivresin resin |
| CN113480692A (en) * | 2021-06-28 | 2021-10-08 | 武汉海翎化学工业有限公司 | High-water-absorptivity polyacrylic resin and preparation method thereof |
| CN115710142A (en) * | 2022-11-17 | 2023-02-24 | 沈阳化工大学 | Controllable slow-release moisturizing fertilizer and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109337015A (en) * | 2018-10-25 | 2019-02-15 | 南京财经大学 | A kind of rice starch water absorbing agent |
| 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 |
| CN110078940A (en) * | 2019-04-26 | 2019-08-02 | 池州学院 | A kind of preparation method of BIOLOGICAL CALCIUM composite high-water-absorptivresin resin |
| CN113480692A (en) * | 2021-06-28 | 2021-10-08 | 武汉海翎化学工业有限公司 | High-water-absorptivity polyacrylic resin and preparation method thereof |
| CN115710142A (en) * | 2022-11-17 | 2023-02-24 | 沈阳化工大学 | Controllable slow-release moisturizing fertilizer and preparation method thereof |
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Application publication date: 20161207 |
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| RJ01 | Rejection of invention patent application after publication |