CN106317333A - Preparation method of semi-interpenetrating water-absorbing resin granules - Google Patents
Preparation method of semi-interpenetrating water-absorbing resin granules Download PDFInfo
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- CN106317333A CN106317333A CN201610704767.1A CN201610704767A CN106317333A CN 106317333 A CN106317333 A CN 106317333A CN 201610704767 A CN201610704767 A CN 201610704767A CN 106317333 A CN106317333 A CN 106317333A
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- absorbing resin
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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
- C08F251/02—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
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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
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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Abstract
The invention discloses a preparation method of semi-interpenetrating water-absorbing resin granules. The method comprises the following steps: S1. preparing the following experiment raw materials: acrylic acid, potassium hydroxide, deionized water, hydroxymethyl cellulose, sodium bisulfite, an initiator and a crosslinking agent; S2. dissolving the potassium hydroxide in the deionized water to prepare a potassium hydroxide solution, and neutralizing the acrylic acid with the prepared potassium hydroxide solution to prepare a potassium acrylate; S3. adding the hydroxymethyl cellulose and crosslinking agent into the potassium acrylate solution, stirring uniformly, heating, adding the initiator and sodium bisulfite, and keeping the temperature to react; and S4. transferring the reaction product into a drying cabinet, drying, adding into a pulverizer, pulverizing and screening. The preparation method is simple to operate, and has the advantages of high safety, environment friendliness, accessible experiment raw materials and low cost. The prepared semi-interpenetrating water-absorbing resin granules have the advantages of no toxicity, no odor and superhigh water-absorbing capacity.
Description
Technical field
The present invention relates to the preparation field of High hydrophilous resin granule, particularly relate to a kind of Semi-IPN type water absorbing resin particle
Preparation method.
Background technology
Super absorbent resin, also known as super strength water absorbent, is a kind of novel functional high molecule material, and Water absorption is up to certainly
Hundreds of or even thousands of times of body quality, and water retention property is excellent, are the special functions of the class developed rapidly in recent years
Macromolecular material.It is widely used in the fields such as agricultural, gardens, health, medicine and building.Super absorbent resin the earliest is 1974
The hydrolysate of the starch-grafted acrylonitrile copolymer of year U.S. school work portion north Research Institute, but early 1980s be
The super absorbent resin development technique of Japan occupies leading position.Although the development time of super absorbent resin is shorter, but respectively
Aspect development is very fast, if nineteen eighty-three Gross World Product is 6000 tons, has just reached 36000 to 1987 yield being only Japan
Ton；The producer of produced worldwide super absorbent resin reaches 30～40 at present, is mainly distributed on Japan, the U.S. and Europe；Product
From starch-grafted acrylonitrile develop into starch graft acrylic acid, cross-linked cellulose class, polyacrylate, copolymer hydrolysis, polyethers,
The classes such as polyurethane；The water absorption rate of super absorbent resin brings up to current four or five thousand times from the Radix Achyranthis Bidentatae of the eighties.China carries out height
The time shorter (early 1980s starts) that water-absorbing resins is developed, although research, production unit have reached tens of family, high suction
The patent of water-base resin has reached tens of kinds.But still the uneven problem of water absorbing properties, product water absorbing properties has much room for improvement.Based on
The problems referred to above, the present invention proposes the preparation method of a kind of Semi-IPN type water absorbing resin particle.
Summary of the invention
The invention aims to solve shortcoming present in prior art, and the one Semi-IPN type water suction proposed is set
The preparation method of fat granule.
The preparation method of a kind of Semi-IPN type water absorbing resin particle, comprises the following steps:
S1, preparing experiment raw material: acrylic acid, potassium hydroxide, deionized water, hydroxymethyl cellulose, sodium sulfite, initiation
Agent, cross-linking agent；
S2, being dissolved in deionized water by potassium hydroxide, compound concentration is the potassium hydroxide solution of 8～15%, with preparation
In potassium hydroxide solution and acrylic acid, preparation degree of neutralization is the potassium acrylate solution of 65～80%；
S3, add in the potassium acrylate solution that hydroxymethyl cellulose and cross-linking agent prepares to step S2, stir 10～
20min, rises to 70～90 DEG C after stirring by system temperature, adds initiator and sodium sulfite, continue stirring 15～
30min, insulation reaction 2～2.5h；
S4, transferring in drying oven by the product in step S3, high temperature 90～110 DEG C are dried 50～80min, so
After dried product is put in pulverizer, pulverize 0.8～1.2h, the product grain after pulverizing crosses 60～100 mesh sieves, i.e.
?.
Preferably, in described step S1 addition is acrylic acid addition the 24～48% of hydroxymethyl cellulose.
Preferably, in described step S1 addition is acrylic acid addition the 5～10% of cross-linking agent.
Preferably, the initiator in described step S1 is 5～8: 1 with the mass ratio of cross-linking agent.
Preferably, the initiator in described step S1 is Ammonium persulfate..
Preferably, the cross-linking agent in described step S1 is N,N methylene bis acrylamide.
The preparation method of a kind of Semi-IPN type water absorbing resin particle that the present invention proposes, with Ammonium persulfate. as initiator, N,
N-methylene-bisacrylamide is cross-linking agent, causes solution polymerization, prepares Semi-IPN type by the method being dried, pulverize and inhales
Water-resin granule, the preparation method that the present invention proposes is simple to operate, and safety and environmental protection, experimental raw is easy to get, and low cost is prepared
Semi-IPN type water absorbing resin particle is nontoxic, tasteless, and water absorbing capacity is extremely strong.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is explained orally further.
Embodiment one
The preparation method of a kind of Semi-IPN type water absorbing resin particle that the present invention proposes, comprises the following steps:
S1, preparing experiment raw material: acrylic acid, potassium hydroxide, deionized water, hydroxymethyl cellulose, sodium sulfite, initiation
Agent, cross-linking agent；
S2, being dissolved in deionized water by potassium hydroxide, compound concentration is the potassium hydroxide solution of 12%, with the hydrogen-oxygen of preparation
Changing in potassium solution and acrylic acid, preparation degree of neutralization is the potassium acrylate solution of 72%；
S3, add hydroxymethyl cellulose and N, N-that consumption is acrylic acid consumption 8% that consumption is acrylic acid consumption 28%
In the potassium acrylate solution that methylene-bisacrylamide is prepared to step S2, stir 15min, by system temperature liter after stirring
To 80 DEG C, add Ammonium persulfate. and sodium sulfite that consumption is 5 times of consumptions of N,N methylene bis acrylamide, continue stirring
22min, insulation reaction 2.3h；
S4, the product in step S3 is transferred in drying oven, 100 DEG C of dry 65min of high temperature, then will be dried
After product put in pulverizer, pulverize 1h, the product grain after pulverizing crosses 80 mesh sieves, to obtain final product.
Embodiment two
The preparation method of a kind of Semi-IPN type water absorbing resin particle that the present invention proposes, comprises the following steps:
S1, preparing experiment raw material: acrylic acid, potassium hydroxide, deionized water, hydroxymethyl cellulose, sodium sulfite, initiation
Agent, cross-linking agent；
S2, being dissolved in deionized water by potassium hydroxide, compound concentration is the potassium hydroxide solution of 10%, with the hydrogen-oxygen of preparation
Changing in potassium solution and acrylic acid, preparation degree of neutralization is the potassium acrylate solution of 68%；
S3, add hydroxymethyl cellulose and N, N-that consumption is acrylic acid consumption 5% that consumption is acrylic acid consumption 45%
In the potassium acrylate solution that methylene-bisacrylamide is prepared to step S2, stir 10min, by system temperature liter after stirring
To 70 DEG C, add Ammonium persulfate. and sodium sulfite that consumption is 7 times of consumptions of N,N methylene bis acrylamide, continue stirring
15min, insulation reaction 2h；
S4, the product in step S3 is transferred in drying oven, 95 DEG C of dry 60min of high temperature, then will be dried
After product put in pulverizer, pulverize 0.9h, the product grain after pulverizing crosses 70 mesh sieves, to obtain final product.
Embodiment three
The preparation method of a kind of Semi-IPN type water absorbing resin particle that the present invention proposes, comprises the following steps:
S1, preparing experiment raw material: acrylic acid, potassium hydroxide, deionized water, hydroxymethyl cellulose, sodium sulfite, initiation
Agent, cross-linking agent；
S2, being dissolved in deionized water by potassium hydroxide, compound concentration is the potassium hydroxide solution of 15%, with the hydrogen-oxygen of preparation
Changing in potassium solution and acrylic acid, preparation degree of neutralization is the potassium acrylate solution of 80%；
S3, add hydroxymethyl cellulose and N, N-that consumption is acrylic acid consumption 6% that consumption is acrylic acid consumption 35%
In the potassium acrylate solution that methylene-bisacrylamide is prepared to step S2, stir 20min, by system temperature liter after stirring
To 90 DEG C, add Ammonium persulfate. and sodium sulfite that consumption is 6 times of consumptions of N,N methylene bis acrylamide, continue stirring
30min, insulation reaction 2.5h；
S4, the product in step S3 is transferred in drying oven, 90 DEG C of dry 55min of high temperature, then will be dried
After product put in pulverizer, pulverize 0.8h, the product grain after pulverizing crosses 60 mesh sieves, to obtain final product.
Embodiment four
The preparation method of a kind of Semi-IPN type water absorbing resin particle that the present invention proposes, comprises the following steps:
S1, preparing experiment raw material: acrylic acid, potassium hydroxide, deionized water, hydroxymethyl cellulose, sodium sulfite, initiation
Agent, cross-linking agent；
S2, being dissolved in deionized water by potassium hydroxide, compound concentration is the potassium hydroxide solution of 14%, with the hydrogen-oxygen of preparation
Changing in potassium solution and acrylic acid, preparation degree of neutralization is the potassium acrylate solution of 75%；
S3, add hydroxymethyl cellulose and N, N-that consumption is acrylic acid consumption 10% that consumption is acrylic acid consumption 40%
In the potassium acrylate solution that methylene-bisacrylamide is prepared to step S2, stir 12min, by system temperature liter after stirring
To 75 DEG C, add Ammonium persulfate. and sodium sulfite that consumption is 8 times of consumptions of N,N methylene bis acrylamide, continue stirring
18min, insulation reaction 2.2h；
S4, the product in step S3 is transferred in drying oven, 110 DEG C of dry 75min of high temperature, then will be dried
After product put in pulverizer, pulverize 1.2h, the product grain after pulverizing crosses 100 mesh sieves, to obtain final product.
Embodiment five
The preparation method of a kind of Semi-IPN type water absorbing resin particle that the present invention proposes, comprises the following steps:
S1, preparing experiment raw material: acrylic acid, potassium hydroxide, deionized water, hydroxymethyl cellulose, sodium sulfite, initiation
Agent, cross-linking agent；
S2, being dissolved in deionized water by potassium hydroxide, compound concentration is the potassium hydroxide solution of 8%, with the hydrogen-oxygen of preparation
Changing in potassium solution and acrylic acid, preparation degree of neutralization is the potassium acrylate solution of 65%；
S3, add hydroxymethyl cellulose and N, N-that consumption is acrylic acid consumption 7% that consumption is acrylic acid consumption 25%
In the potassium acrylate solution that methylene-bisacrylamide is prepared to step S2, stir 18min, by system temperature liter after stirring
To 85 DEG C, add Ammonium persulfate. and sodium sulfite that consumption is 6.5 times of consumptions of N,N methylene bis acrylamide, continue stirring
26min, insulation reaction 2.4h；
S4, the product in step S3 is transferred in drying oven, 105 DEG C of dry 70min of high temperature, then will be dried
After product put in pulverizer, pulverize 1.1h, the product grain after pulverizing crosses 90 mesh sieves, to obtain final product.
One～five preparation methoies proposed, has manufactured experimently out five groups of Semi-IPN type water-absorbing resins according to embodiments of the present invention
Grain, the water absorbing properties of the Semi-IPN type water absorbing resin particle prepared five groups of embodiments respectively according to following methods is surveyed
Examination: at that same temperature, weigh the dry granule two parts taking 0.1g in the balance, be respectively placed in the filter cloth of 200 mesh, tether bag
Wrap up in, obtain experimental subject A and experimental subject B；Being placed in the distilled water of determined volume by experimental subject A, it is fixed to be placed in by experimental subject B
In the normal saline of amount volume, after standing 5min, experimental subject A and experimental subject B is carried, hung 5min, then weigh also
Record (is inhaled the distillation water yield and is denoted as water absorption A；Inhale saline volume and be denoted as water absorption B), result is as follows:
| Embodiment | Embodiment one | Embodiment two | Embodiment three | Embodiment four | Embodiment five |
| Water absorption A | 225g | 221g | 232g | 228g | 219g |
| Water absorption B | 16.8g | 16.2g | 18.5g | 17.3g | 15.7g |
From above table: the Semi-IPN type water absorbing resin particle water suction that five groups of embodiments that the present invention proposes are prepared
Property is splendid, and the water absorption of embodiment three is the strongest.The preparation method of a kind of Semi-IPN type water absorbing resin particle that the present invention proposes,
With Ammonium persulfate. as initiator, N,N methylene bis acrylamide is cross-linking agent, causes solution polymerization, by dry, powder
Broken method prepares Semi-IPN type water absorbing resin particle, and the preparation method that the present invention proposes is simple to operate, and safety and environmental protection is tested former
Material is easy to get, low cost, and the Semi-IPN type water absorbing resin particle prepared is nontoxic, tasteless, and water absorbing capacity is extremely strong.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope that the invention discloses, according to technical scheme and
Inventive concept equivalent or change in addition, all should contain within protection scope of the present invention.
Claims (6)
1. the preparation method of a Semi-IPN type water absorbing resin particle, it is characterised in that comprise the following steps:
S1, preparing experiment raw material: acrylic acid, potassium hydroxide, deionized water, hydroxymethyl cellulose, sodium sulfite, initiator,
Cross-linking agent；
S2, being dissolved in deionized water by potassium hydroxide, compound concentration is the potassium hydroxide solution of 8～15%, with the hydrogen-oxygen of preparation
Changing in potassium solution and acrylic acid, preparation degree of neutralization is the potassium acrylate solution of 65～80%；
S3, add in the potassium acrylate solution that hydroxymethyl cellulose and cross-linking agent prepares to step S2, stirring 10～20min, stir
After mixing uniformly, system temperature is risen to 70～90 DEG C, add initiator and sodium sulfite, continue stirring 15～30min, insulation
Reaction 2～2.5h；
S4, transferring in drying oven by the product in step S3, high temperature 90～110 DEG C are dried 50～80min, then will
Dried product puts in pulverizer, pulverizes 0.8～1.2h, and the product grain after pulverizing crosses 60～100 mesh sieves, to obtain final product.
The preparation method of a kind of Semi-IPN type water absorbing resin particle the most according to claim 1, it is characterised in that described step
In rapid S1 addition is acrylic acid addition the 24～48% of hydroxymethyl cellulose.
The preparation method of a kind of Semi-IPN type water absorbing resin particle the most according to claim 1, it is characterised in that described step
In rapid S1 addition is acrylic acid addition the 5～10% of cross-linking agent.
The preparation method of a kind of Semi-IPN type water absorbing resin particle the most according to claim 1, it is characterised in that described step
Initiator in rapid S1 is 5～8: 1 with the mass ratio of cross-linking agent.
The preparation method of a kind of Semi-IPN type water absorbing resin particle the most according to claim 1, it is characterised in that described step
Initiator in rapid S1 is Ammonium persulfate..
The preparation method of a kind of Semi-IPN type water absorbing resin particle the most according to claim 1, it is characterised in that described step
Cross-linking agent in rapid S1 is N,N methylene bis acrylamide.
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| CN201610704767.1A CN106317333A (en) | 2016-08-22 | 2016-08-22 | Preparation method of semi-interpenetrating water-absorbing resin granules |
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| CN201610704767.1A CN106317333A (en) | 2016-08-22 | 2016-08-22 | Preparation method of semi-interpenetrating water-absorbing resin granules |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107778368A (en) * | 2017-10-07 | 2018-03-09 | 浙江理工大学 | A kind of method that cellulose base profile-controlling and plugging agent is prepared using Modified by Carboxymethyl Cellulose |
| CN109126008A (en) * | 2018-06-28 | 2019-01-04 | 南京理工大学 | Macromolecule water uptake resin and preparation method thereof suitable for extinguishing chemical |
| CN110423308A (en) * | 2019-03-12 | 2019-11-08 | 北京市政建设集团有限责任公司 | The preparation method of a kind of super absorbent resin and in the application for reducing dregs moisture content |
| CN110819356A (en) * | 2019-09-30 | 2020-02-21 | 北京市政建设集团有限责任公司 | Preparation method of high-compression-resistance cellulose graft copolymerization sand fixation material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554388A (en) * | 2013-11-19 | 2014-02-05 | 宜兴丹森科技有限公司 | Preparation method of biodegradable super absorbent resin |
| CN105348444A (en) * | 2015-12-09 | 2016-02-24 | 中国-阿拉伯化肥有限公司 | High-water-absorptivity resin and preparation method thereof |
-
2016
- 2016-08-22 CN CN201610704767.1A patent/CN106317333A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554388A (en) * | 2013-11-19 | 2014-02-05 | 宜兴丹森科技有限公司 | Preparation method of biodegradable super absorbent resin |
| CN105348444A (en) * | 2015-12-09 | 2016-02-24 | 中国-阿拉伯化肥有限公司 | High-water-absorptivity resin and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107778368A (en) * | 2017-10-07 | 2018-03-09 | 浙江理工大学 | A kind of method that cellulose base profile-controlling and plugging agent is prepared using Modified by Carboxymethyl Cellulose |
| CN109126008A (en) * | 2018-06-28 | 2019-01-04 | 南京理工大学 | Macromolecule water uptake resin and preparation method thereof suitable for extinguishing chemical |
| CN110423308A (en) * | 2019-03-12 | 2019-11-08 | 北京市政建设集团有限责任公司 | The preparation method of a kind of super absorbent resin and in the application for reducing dregs moisture content |
| CN110819356A (en) * | 2019-09-30 | 2020-02-21 | 北京市政建设集团有限责任公司 | Preparation method of high-compression-resistance cellulose graft copolymerization sand fixation material |
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