CN111718438A - Preparation method of porous sodium polyacrylate super absorbent resin - Google Patents
Preparation method of porous sodium polyacrylate super absorbent resin Download PDFInfo
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- CN111718438A CN111718438A CN201910211257.4A CN201910211257A CN111718438A CN 111718438 A CN111718438 A CN 111718438A CN 201910211257 A CN201910211257 A CN 201910211257A CN 111718438 A CN111718438 A CN 111718438A
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- absorbent resin
- super absorbent
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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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/26—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
Abstract
The preparation method of the porous sodium polyacrylate super absorbent resin comprises the following steps: the invention belongs to the field of synthesis of super absorbent resin, and particularly relates to a method for synthesizing porous sodium polyacrylate. The main method of the invention is as follows: weighing acrylic acid, adding weighed CMC-Na and F127 into a 250ml three-neck flask, stirring and fully dissolving; adding the prepared sodium hydroxide solution for neutralization under the ice-water bath condition; sequentially adding NNMBA solution, KPS solution, pore-forming agent and NaHSO3Adding appropriate amount of deionized water to make monomer concentration at the end 33%, stirring for 10min, reacting at 60 deg.C for 2 hr, cutting into slender strips, heating to 105 deg.C, oven drying, pulverizing, sieving to 50-100 mesh, and testing to obtain porous superabsorbent polymerAnd (3) resin.
Description
Technical Field
The invention relates to the field of production of super absorbent resin, in particular to a preparation method of porous sodium polyacrylate.
Background
The super absorbent resin is a substance having a network molecular structure capable of absorbing several tens to several thousands of times of its own weight. The application field is wider, and the method mainly relates to the fields of physiological sanitation, agriculture, forestry, gardening, medicine slow release, construction and the like. With the annual increase of domestic demand, the research on the super absorbent resin is increasing day by day and becomes a research hotspot gradually. The acrylic super absorbent resin is a water absorbent material which is most widely used at present because of excellent water absorption, water retention and the like.
The acrylic super absorbent resin has the advantages of high water absorption, good salt resistance, good water retention property and the like, but in practical application, the problem of slow absorption speed exists, and the swelling balance can be achieved generally within hours or even days. In order to solve the problems that the swelling speed of the super absorbent resin is slow and the absorption speed is increased, the common method for increasing the absorption speed of the super absorbent resin comprises the following steps: the super absorbent resin is crushed into fine particles, holes are formed in the super absorbent resin, and the super absorbent resin is subjected to surface crosslinking and the like. The super absorbent resin particles are crushed into smaller particles, although the absorption speed can be effectively improved, the particle size is too small, the use in certain occasions is limited, and the particles are easy to agglomerate and adhere after being reduced and absorbed water. The surface modification is carried out on the super absorbent resin particles, the absorption speed of the super absorbent resin can be improved to a certain extent, the problem of high water absorption adhesion is solved, but the effective improvement of the absorption speed is limited. Through pore-forming the super absorbent resin, the specific surface area of the super absorbent resin can be effectively improved, and then the absorption speed is improved, so that the super absorbent resin can meet the requirements of practical application.
Disclosure of Invention
The invention aims to provide a preparation method of a porous sodium polyacrylate super absorbent resin, which can improve the specific surface area of the super absorbent resin and shorten the path of water molecules entering the super absorbent resin by forming a porous structure in the super absorbent resin, thereby improving the absorption speed of the super absorbent resin and further meeting the actual application requirements of the market. The technical scheme of the invention is as follows: the preparation method of the porous sodium polyacrylate super absorbent resin comprises the following main raw materials in percentage by weight: 100 percent of acrylic acid, 0.2 to 1.0 percent of thickening agent, 0.05 to 0.30 percent of surfactant, 0.1 to 1.2 percent of redox initiator, 0.01 to 0.07 percent of cross-linking agent, 3 to 12 percent of pore-foaming agent, 150 percent of deionized water and 300 percent of neutralization degree, and the polymerization temperature is 40 to 90 ℃; the preparation process comprises the following steps:
(1) weighing acrylic acid, sequentially adding a thickening agent and a nonionic surfactant into a three-neck flask, and stirring at 300r/min for full dissolution;
(2) adding sodium hydroxide solution for neutralization, sequentially adding a cross-linking agent N, N-methylene bisacrylamide solution, an oxidation system initiator potassium persulfate solution, a pore-forming agent and a reduction system initiator sodium bisulfite solution, stirring for a certain time, and placing in an oven for reaction at a certain temperature for a certain time.
(3) Shearing the super absorbent resin gel formed after the reaction into uniform strips, heating, performing pore-forming drying in a drying oven, crushing, and testing for later use.
The method is characterized in that: the thickening agent in the step (1) is sodium carboxymethylcellulose, and the nonionic surfactant is polyoxyethylene-propylene oxide. And (3) the pore-foaming agent in the step (2) is ethanol or ammonium bicarbonate. The slender strip in the step (3) is about 1cm, the thickness is not more than 1cm, and the pore-forming drying temperature is 105 ℃.
Drawings
FIG. 1 is a scanning electron micrograph of a super absorbent resin obtained in example 1 at a magnification of 30;
FIG. 2 is a scanning electron micrograph of the super absorbent resin obtained in example 2 magnified 30 times;
the specific implementation example is as follows:
the present invention is further illustrated by the following examples, which are intended to be illustrative, not limiting, and the scope of the invention is not limited thereto.
Example 1 was carried out:
the raw materials comprise the following components in parts by weight:
acrylic acid: 30
Thickening agent: 0.24
Surfactant (b): 0.03
Degree of neutralization: 90 percent of
A crosslinking agent: 0.006
Initiator: 0.21
Ethanol: 3
The preparation process comprises the following steps:
(1) weighing 30g of acrylic acid, sequentially adding 0.24g of thickening agent and 0.03g of nonionic surfactant into a three-neck flask, and stirring at 300r/min for full dissolution;
(2) adding sodium hydroxide solution until the neutralization degree is 90%, then sequentially adding a solution containing 0.006g of cross-linking agent N, N-methylene bisacrylamide, a solution containing 0.21g of oxidation system initiator potassium persulfate, 3g of pore-forming agent ethanol and a solution containing reduction system initiator sodium bisulfite, stirring for 10min, and placing in an oven to react for 2h at 60 ℃.
(3) Shearing the super absorbent resin gel formed after the reaction into strips with the width of 1cm and the thickness of no more than 1cm, raising the temperature to 105 ℃, forming holes in an oven, drying, crushing and testing for later use.
The scanning electron microscope image of the obtained super absorbent resin with the magnification of 30 times is shown in figure 1:
example 2 was carried out:
the raw materials comprise the following components in parts by weight:
acrylic acid: 30
Thickening agent: 0.24
Surfactant (b): 0.03
Degree of neutralization: 90 percent of
A crosslinking agent: 0.006
Initiator: 0.21
Ammonium bicarbonate: 3
The preparation process comprises the following steps:
(1) weighing 30g of acrylic acid, sequentially adding 0.24g of thickening agent and 0.03g of nonionic surfactant into a three-neck flask, and stirring at 300r/min for full dissolution;
(2) adding a sodium hydroxide solution until the neutralization degree is 90%, sequentially adding a crosslinking agent N, N-methylene bisacrylamide solution containing 0.006g, an oxidation system initiator potassium persulfate solution containing 0.21g, a pore-forming agent ammonium bicarbonate solution containing 3g and a reduction system initiator sodium bisulfite solution, stirring for 10min, and placing in an oven to react for 2h at 60 ℃.
(3) Shearing the super absorbent resin gel formed after the reaction into strips with the width of 1cm and the thickness of no more than 1cm, raising the temperature to 105 ℃, forming holes in an oven, drying, crushing and testing for later use.
The scanning electron microscope image of the obtained super absorbent resin with the magnification of 30 times is shown in FIG. 2.
Claims (5)
1. A preparation method of porous sodium polyacrylate super absorbent resin comprises the following main raw materials in percentage by weight: 100 percent of acrylic acid, 0.2 to 1.0 percent of thickening agent, 0.05 to 0.30 percent of surfactant, 0.1 to 1.2 percent of redox initiator, 0.01 to 0.07 percent of cross-linking agent, 3 to 12 percent of pore-foaming agent, 150 percent of deionized water and 300 percent of neutralization degree, and the polymerization temperature is 40 to 90 ℃; the preparation process comprises the following steps:
weighing acrylic acid, sequentially adding a thickening agent and a nonionic surfactant into a three-neck flask, and stirring at 300r/min for full dissolution;
adding sodium hydroxide solution for neutralization, sequentially adding a cross-linking agent N, N-methylene bisacrylamide solution, an oxidation system initiator potassium persulfate solution, a pore-forming agent and a reduction system initiator sodium bisulfite solution, stirring for a certain time, and placing in an oven for reaction at a certain temperature for a certain time.
2. Shearing the super absorbent resin gel formed after the reaction into uniform strips, heating, performing pore-forming drying in a drying oven, crushing, and testing for later use.
3. The method for preparing porous sodium polyacrylate according to claim 1, which is characterized in that:
the thickening agent in the step (1) is sodium carboxymethylcellulose, and the nonionic surfactant is polyoxyethylene-propylene oxide.
4. And (3) the pore-foaming agent in the step (2) is ethanol or ammonium bicarbonate.
5. The slender strip in the step (3) is about 1cm, the thickness is not more than 1cm, and the pore-forming drying temperature is 105 ℃.
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| CN201910211257.4A CN111718438A (en) | 2019-03-20 | 2019-03-20 | Preparation method of porous sodium polyacrylate super absorbent resin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023120907A1 (en) * | 2021-12-24 | 2023-06-29 | 주식회사 엘지화학 | Preparation method for super absorbent polymer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3083124A (en) * | 1959-03-20 | 1963-03-26 | Int Latex Corp | Cellular materials and articles and method of producing |
| CN103214616A (en) * | 2013-04-16 | 2013-07-24 | 华南理工大学 | Preparation method of porous-super-absorbent resin |
| CN106916260A (en) * | 2017-03-29 | 2017-07-04 | 中山大学惠州研究院 | A kind of preparation method of hud typed porous high water absorption microballoon |
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2019
- 2019-03-20 CN CN201910211257.4A patent/CN111718438A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3083124A (en) * | 1959-03-20 | 1963-03-26 | Int Latex Corp | Cellular materials and articles and method of producing |
| CN103214616A (en) * | 2013-04-16 | 2013-07-24 | 华南理工大学 | Preparation method of porous-super-absorbent resin |
| CN106916260A (en) * | 2017-03-29 | 2017-07-04 | 中山大学惠州研究院 | A kind of preparation method of hud typed porous high water absorption microballoon |
Non-Patent Citations (2)
| Title |
|---|
| 何领好等: "《功能高分子材料》", 31 August 2016 * |
| 孙伯平等: "聚丙烯酸钠高吸水性树脂的研究", 《工程塑料应用》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023120907A1 (en) * | 2021-12-24 | 2023-06-29 | 주식회사 엘지화학 | Preparation method for super absorbent polymer |
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Application publication date: 20200929 |