CN108219056A - A kind of method that can be continuously produced super absorbent resin - Google Patents
A kind of method that can be continuously produced super absorbent resin Download PDFInfo
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- CN108219056A CN108219056A CN201611222293.3A CN201611222293A CN108219056A CN 108219056 A CN108219056 A CN 108219056A CN 201611222293 A CN201611222293 A CN 201611222293A CN 108219056 A CN108219056 A CN 108219056A
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- absorbent resin
- super absorbent
- continuously produced
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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
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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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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Abstract
The invention belongs to synthesizing high-hydroscopicity production of resins technical field more particularly to a kind of preparation process for the super absorbent resin that can be continuously produced.The process is characterized in including neutralizing, polymerization, pelletizing, wherein it is polymerizeing with using substep viscosity reduction method in pelletizing process, viscosity reduction component is introduced respectively in this two procedures, so as to solve the biggest problem --- the adhesion problems in granulation process of puzzlement synthesizing high-hydroscopicity resin continuous production.The method that the present invention uses improves the production efficiency of synthesis hydroscopic high-molecular resin while production cost is not increased, while solves the problems, such as the dust pollution easily generated in drying process.
Description
Technical field
The present invention relates to a kind of super absorbent resin preparation methods that can be continuously produced, and belong to functional high molecule material neck
Domain.
Background technology
Hydroscopic high-molecular resin is a kind of new functional macromolecule material with tridimensional network, with conventional water suction
Material is different, has stronger water absorbing capacity hydroscopic high-molecular resin under stress, other than having high-hydroscopicity energy,
Also there is the features such as production cost is low, simple for process, product quality is stablized, and long-time storage undergoes no deterioration, and acrylic acid is former
Material also has non-toxic and environmental protection advantage.In opening system, the super absorbent resin using acrylic acid as principal monomer is completed
Later stage building-up process, extruded granulation by fluidized bed drying, after pulverizing and sieving, obtains product, realizes continuous operation.
Since the principal monomer of synthesis water-absorbing resin is acrylic acid, the gel after polymerizeing is rich in a large amount of carboxyls, makes its adhesiveness extremely strong,
It easily sticks together, is also easy under head high shear forces puffing in cavity and between particle during extrusion is broken
Foaming, it is broken to influence gel solution.The presence of carboxyl also results in product in drying process and hardened phenomenon occurs, greatly reduces fluidisation
Bed drying efficiency even will appear the phenomenon that a large amount of outer dry interior wet aggregates block fluid bed when serious.Traditional solution is done
Method one is to increase the degree of neutralization and the degree of cross linking of monomeric acrylic, second is that adding in the dispersants such as lauryl sodium sulfate when squeezing out.
Although the former, which can partly ensure, squeezes out broken progress, the hardened phenomenon in drying process, and degree of neutralization can not be eliminated
Raising with the degree of cross linking can greatly reduce the water absorption rate and salt absorbing rate of final products；The latter is when a large amount of add in and document
Report is consistent, water absorbent gel solution can be made to be broken into smaller particle substantially, but still have caking phenomenon, and in powder in dryer section
During broken screening, tiny dispersant is flown upward everywhere, causes dust pollution, is influenced production and is normally carried out.
The purpose of the present invention is being directed to defect present in above-mentioned continuous production technology, a kind of new mode substep is provided
Solve bonding and carry out viscosity reduction, it will not reduce the water absorption rate and salt absorbing rate of product, and improve be granulated property with can drying property, improve production
Efficiency, reduces production cost, it has the characteristics that simple and easy to do, is suitble in synthesizing high-hydroscopicity Resin Industry continuous production
Using.
Technique proposed by the present invention for synthesizing high-hydroscopicity resin continuous production for substep solution bonding, be by with
Lower method is to realize, acrylic acid is neutralized with lye, adds in crosslinking agent mixing, adds carboxy protective agent, continues to introduce oxygen
Change reduction initiating system, polymerize, cross-linking reaction, generate high water absorbent resin gel not soluble in water.It will react what is formed
In gel merging extruder, compounding dispersion liquid is added in, extruding pelletization is dried by fluid bed, subsequently enters crushing, screening
Process is packed through examining.
Invention content
For the adhesion problems in existing method granulation process.The present invention seeks to be that providing one kind can be continuously produced
Super absorbent resin preparation method, while production cost is not increased, improve synthesis hydroscopic high-molecular resin production
Efficiency, while solve the problems, such as the dust pollution generated in drying process.Include the following steps：
(1) raw material propylene acid, acrylamide, water, neutralizer, crosslinking agent are weighed by proportioning, neutralizer first is dissolved in water matches
Into lye, after by other all raw materials input lye, be sufficiently mixed and stir, complete neutralization step.Wherein weight percent contains
Measure acrylic acid 20-45%, acrylamide 0-20%, water 55-70%, neutralizer 7-23%, crosslinking agent 0.02-0.2%, neutralizer
For sodium carbonate, sodium hydroxide, sodium bicarbonate, potassium hydroxide, ammonium hydroxide etc., one or more mixing, crosslinking agent N, N ' methylene
Double methacrylate, polyethyleneglycol diacrylate etc..
(2) temperature is adjusted to 20-50 DEG C, by lauryl sodium sulfate, odium stearate, neopelex in
It is mixed with liquid, after it is completely dissolved, successively adds in initiator and reducing agent, stirring is allowed to be sufficiently mixed, is polymerize, handed over
Connection.Wherein lauryl sodium sulfate: odium stearate: neopelex 0-1: 0-1.5: 0-1.5, initiator weight account for
The 0.05-1% of monomer, reducing agent weight account for the 20-70% of initiator, and initiator is ammonium persulfate or potassium peroxydisulfate etc., is restored
Agent is received for sodium thiosulfate, sodium sulfite or bisulfite.
(3) it treats that temperature is cooled to room temperature, jello is placed in extruder, it is continuous in an extruder that dispersion is added dropwise
Liquid, speed 2ml/s, dispersion liquid composition is solid dispersion, liquid dispersant and water, and weight ratio is：2-10: 1-4: 86-97,
Drying is with spare.Solid dispersion is for lauryl sodium sulfate, odium stearate or neopelex etc., liquid dispersant
For span 80, this disk 60, Tween 80, polysorbate60 or Op-10 etc., one or more mixing.
Embodiment 1：
It is acrylic acid 60kg to choose raw material weight proportioning of soup processed, sodium hydroxide 20kg, crosslinking agent N, N ' methylene bisacrylamide acid esters
0.4kg, water 160kg, wherein 100kg water are first used to dissolve sodium hydroxide proportionaling alkali-forming liquid.All raw materials are put into lye, are completed
Neutralization step.
Temperature is adjusted to 35 DEG C, addition 1kg lauryl sodium sulfate, 1.5kg odium stearate, after it is completely dissolved,
Initiation system, ammonium persulfate 1kg, sodium thiosulfate 0.7kg are added in, stirring is allowed to be sufficiently mixed, is polymerize, be crosslinked.
It treats that temperature is cooled to room temperature, jello is placed in extruder, dispersion liquid, speed are continuously added dropwise in an extruder
It spends for 2ml/s, dispersion liquid composition is (weight ratio)：95% water, 2% span 80,1%op-10,1% odium stearate, 1% 12
Sodium alkyl sulfate.
It is extruded to be granulated, is dry, obtaining final products after crushing.
It is generated in production process without dust, actual measurement water absorption rate 560g/g.
Embodiment 2：
It is acrylic acid 60kg to choose raw material weight proportioning of soup processed, sodium hydroxide 25kg, crosslinking agent N, N ' methylene bisacrylamide acid esters
0.4kg, water 150kg, wherein 100kg water are first used to dissolve sodium hydroxide proportionaling alkali-forming liquid.All raw materials are put into lye, are completed
Neutralization step.
Temperature is adjusted to 35 DEG C, adds in 0.5kg lauryl sodium sulfate, 1kg neopelexes treat it completely
After dissolving, initiation system, ammonium persulfate 1kg, sodium hydrogensulfite 0.7kg are added in, stirring is allowed to be sufficiently mixed, is polymerize, handed over
Connection.
It treats that temperature is cooled to room temperature, jello is placed in extruder, dispersion liquid, speed are continuously added dropwise in an extruder
It spends for 2ml/s, dispersion liquid composition is (weight ratio)：93% water, 2% this disk 60,2%op-10,1% odium stearate, 2% 12
Sodium alkyl sulfate.
It is extruded to be granulated, is dry, obtaining final products after crushing.
It is generated in production process without dust, actual measurement water absorption rate 460g/g.
Embodiment 3：
It is acrylic acid 60kg to choose raw material weight proportioning of soup processed, potassium hydroxide 20kg, crosslinking agent polyethyleneglycol diacrylate
0.4kg, water 160kg, wherein 100kg water are first used to dissolve sodium hydroxide proportionaling alkali-forming liquid.All raw materials are put into lye, are completed
Neutralization step.
Temperature is adjusted to 40 DEG C, addition 1kg lauryl sodium sulfate, 1.5kg odium stearate, after it is completely dissolved,
Initiation system, ammonium persulfate 1kg, sodium thiosulfate 0.6kg are added in, stirring is allowed to be sufficiently mixed, is polymerize, be crosslinked.
It treats that temperature is cooled to room temperature, jello is placed in extruder, dispersion liquid, speed are continuously added dropwise in an extruder
It spends for 2ml/s, dispersion liquid composition is (weight ratio)：94.5% water, 2% polysorbate60,1%op-10,1% lauryl sodium sulfate,
1.5% odium stearate.
It is extruded to be granulated, is dry, obtaining final products after crushing.
It is generated in production process without dust, actual measurement water absorption rate 570g/g.
Embodiment 4：
It is acrylic acid 65kg to choose raw material weight proportioning of soup processed, potassium hydroxide 30kg, crosslinking agent polyethyleneglycol diacrylate
0.6kg, water 180kg, wherein 100kg water are first used to dissolve sodium hydroxide proportionaling alkali-forming liquid.All raw materials are put into lye, are completed
Neutralization step.
Temperature is adjusted to 35 DEG C, adds in 2kg odium stearate, after it is completely dissolved, adds in initiation system, ammonium persulfate
1kg, sodium thiosulfate 0.5kg, stirring are allowed to be sufficiently mixed, are polymerize, be crosslinked.
It treats that temperature is cooled to room temperature, jello is placed in extruder, dispersion liquid, speed are continuously added dropwise in an extruder
It spends for 2ml/s, dispersion liquid composition is (weight ratio)：93% water, 2% this disk 60,1% polysorbate60,3% odium stearate, 1% 12
Sodium alkyl sulfate.
It is extruded to be granulated, is dry, obtaining final products after crushing.
It is generated in production process without dust, actual measurement water absorption rate 570g/g.
Embodiment 5：
It is acrylic acid 60kg to choose raw material weight proportioning of soup processed, sodium hydroxide 20kg, acrylamide 10kg, and crosslinking agent N, N ' are sub-
Methyl double methacrylate 0.4kg, water 180kg, wherein 100kg water are first used to dissolve sodium hydroxide proportionaling alkali-forming liquid.By all raw materials
It puts into lye, completes neutralization step.
Temperature is adjusted to 35 DEG C, 1kg lauryl sodium sulfate is added in after it is completely dissolved, adds in initiation system, mistake
Ammonium sulfate 1kg, sodium thiosulfate 0.7kg, stirring are allowed to be sufficiently mixed, are polymerize, be crosslinked.
It treats that temperature is cooled to room temperature, jello is placed in extruder, dispersion liquid, speed are continuously added dropwise in an extruder
It spends for 2ml/s, dispersion liquid composition is (weight ratio)：95% water, 2%Op-10,1% odium stearate, 2% lauryl sodium sulfate.
It is extruded to be granulated, is dry, obtaining final products after crushing.
It is generated in production process without dust, actual measurement water absorption rate 540g/g.
Claims (7)
1. a kind of super absorbent resin preparation method that can be continuously produced, which is characterized in that include the following steps：
(1) raw material propylene acid, acrylamide, water, neutralizer, crosslinking agent are weighed by proportioning, neutralizer is first dissolved in water proportionaling alkali-forming
Liquid, after by other all raw materials input lye, be sufficiently mixed and stir, complete neutralization step.Wherein weight percentage third
Olefin(e) acid 20-45%, acrylamide 0-20%, water 55-70%, neutralizer 7-23%, crosslinking agent 0.02-0.2%.
(2) temperature is adjusted to 20-50 DEG C, by lauryl sodium sulfate, odium stearate, neopelex and neutralizer
Mixing after it is completely dissolved, successively adds in initiator and reducing agent, and stirring is allowed to be sufficiently mixed, is polymerize, be crosslinked.Its
Middle lauryl sodium sulfate: odium stearate: neopelex 0-1: 0-1.5: 0-1.5, initiator weight account for monomer
0.05-1%, reducing agent weight accounts for the 20-70% of initiator,
(3) it treats that temperature is cooled to room temperature, jello is placed in extruder, dispersion liquid, speed are continuously added dropwise in an extruder
It spends for 2ml/s, dispersion liquid composition is solid dispersion, liquid dispersant and water, and weight ratio is：2-10: 1-4: 86-97, it is dry
With spare.
A kind of 2. super absorbent resin preparation method that can be continuously produced described in accordance with the claim 1, which is characterized in that institute
Neutralizer is stated as sodium carbonate, sodium hydroxide, sodium bicarbonate, potassium hydroxide, ammonium hydroxide etc., one or more mixing.
A kind of 3. super absorbent resin preparation method that can be continuously produced described in accordance with the claim 1, which is characterized in that institute
Crosslinking agent is stated as N, N ' methylene bisacrylamides acid esters, polyethyleneglycol diacrylate etc..
A kind of 4. super absorbent resin preparation method that can be continuously produced described in accordance with the claim 1, which is characterized in that institute
Initiator is stated as ammonium persulfate or potassium peroxydisulfate etc..
A kind of 5. super absorbent resin preparation method that can be continuously produced described in accordance with the claim 1, which is characterized in that institute
Reducing agent is stated to receive for sodium thiosulfate, sodium sulfite or bisulfite.
A kind of 6. super absorbent resin preparation method that can be continuously produced described in accordance with the claim 1, which is characterized in that institute
Solid dispersion is stated as lauryl sodium sulfate, odium stearate or neopelex etc..
A kind of 7. super absorbent resin preparation method that can be continuously produced described in accordance with the claim 1, which is characterized in that institute
Liquid dispersant is stated as span 80, this disk 60, Tween 80, polysorbate60 or Op-10 etc., one or more mixing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611222293.3A CN108219056A (en) | 2016-12-22 | 2016-12-22 | A kind of method that can be continuously produced super absorbent resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611222293.3A CN108219056A (en) | 2016-12-22 | 2016-12-22 | A kind of method that can be continuously produced super absorbent resin |
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| CN108219056A true CN108219056A (en) | 2018-06-29 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201611222293.3A Pending CN108219056A (en) | 2016-12-22 | 2016-12-22 | A kind of method that can be continuously produced super absorbent resin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112300322A (en) * | 2020-10-29 | 2021-02-02 | 甘肃恒石公路检测科技有限公司 | Super absorbent resin suitable for concrete alkaline environment and preparation method thereof |
| CN114316107A (en) * | 2022-01-07 | 2022-04-12 | 安徽富瑞雪化工科技股份有限公司 | Novel production method of super absorbent resin |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475692A (en) * | 2009-01-12 | 2009-07-08 | 上海华谊丙烯酸有限公司 | Prilling process for high hydroscopicity resin hydrogel polymer |
| CN103910896A (en) * | 2014-04-08 | 2014-07-09 | 万华化学集团股份有限公司 | Preparation method of macromolecular water-absorbent resin with low reverse osmosis |
| CN104744711A (en) * | 2015-03-25 | 2015-07-01 | 华南理工大学 | High-brightness crylic acid super absorbent resin and preparation method thereof |
| CN105294920A (en) * | 2015-12-10 | 2016-02-03 | 湖北乾峰新材料科技有限公司 | Preparation method of high-water-absorption polymer |
-
2016
- 2016-12-22 CN CN201611222293.3A patent/CN108219056A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475692A (en) * | 2009-01-12 | 2009-07-08 | 上海华谊丙烯酸有限公司 | Prilling process for high hydroscopicity resin hydrogel polymer |
| CN103910896A (en) * | 2014-04-08 | 2014-07-09 | 万华化学集团股份有限公司 | Preparation method of macromolecular water-absorbent resin with low reverse osmosis |
| CN104744711A (en) * | 2015-03-25 | 2015-07-01 | 华南理工大学 | High-brightness crylic acid super absorbent resin and preparation method thereof |
| CN105294920A (en) * | 2015-12-10 | 2016-02-03 | 湖北乾峰新材料科技有限公司 | Preparation method of high-water-absorption polymer |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112300322A (en) * | 2020-10-29 | 2021-02-02 | 甘肃恒石公路检测科技有限公司 | Super absorbent resin suitable for concrete alkaline environment and preparation method thereof |
| CN114316107A (en) * | 2022-01-07 | 2022-04-12 | 安徽富瑞雪化工科技股份有限公司 | Novel production method of super absorbent resin |
| CN114316107B (en) * | 2022-01-07 | 2023-08-18 | 安徽富瑞雪化工科技股份有限公司 | Novel production method of super absorbent resin |
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