CN109054265B - Method for preparing expanded polyvinyl alcohol - Google Patents
Method for preparing expanded polyvinyl alcohol Download PDFInfo
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- CN109054265B CN109054265B CN201810831454.1A CN201810831454A CN109054265B CN 109054265 B CN109054265 B CN 109054265B CN 201810831454 A CN201810831454 A CN 201810831454A CN 109054265 B CN109054265 B CN 109054265B
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- polyvinyl alcohol
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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
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/125—Water, e.g. hydrated salts
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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
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/10—Water or water-releasing compounds
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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
- C08J2329/00—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 at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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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
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a method for preparing expanded polyvinyl alcohol, which comprises the steps of performing expansion production by using a screw expander, adding a special mixed auxiliary agent of hexadecylamine polyoxyethylene ether and polyethylene glycol in the expansion process to prepare expanded polyvinyl alcohol in a fibrous shape, measuring the specific surface area of the expanded polyvinyl alcohol in the fibrous shape by using a gas adsorption BET method, wherein the specific surface area is 10-20 times that of similar industrial grade polyvinyl alcohol particles, the expanded polyvinyl alcohol in the fibrous shape is not attached to the wall and does not sink at the bottom in a dissolving device, and the expanded polyvinyl alcohol can be dissolved in water at 95 ℃ for 5-10 minutes, so that the dissolving time is greatly shortened, and the problem that a downstream customer is difficult to dissolve the polyvinyl alcohol is solved; the invention has the advantages of simple preparation process, large specific surface area of the prepared expanded polyvinyl alcohol and strong solubility.
Description
Technical Field
The invention relates to the technical field of extrusion and expansion, in particular to a method for preparing expanded polyvinyl alcohol.
Background
The conventional commercial industrial grade polyvinyl alcohol resin series products are white solids, and the shapes of the products are flocculent, granular and powdery; it is non-toxic, tasteless and pollution-free, and can be dissolved in water at 80-95 deg.C, and its aqueous solution possesses good adhesion and film-forming property, can resist most organic solvents of oil, lubricant and hydrocarbon, etc., and possesses the chemical properties of long-chain polyol esterification, etherification and acetalation, etc.
Polyvinyl alcohol is an important chemical raw material, and is mainly used for warp size, fabric finishing agent and vinylon fiber raw material in the textile industry; building decoration industry 107 glue, internal and external wall paint and adhesive; the polymer is used as a polymeric emulsifier, a dispersant and polyvinyl formal, acetal and butyral resin in the chemical industry; the paper industry is used as paper adhesives; the agricultural pesticide is used for soil conditioners, pesticide adhesion synergists and polyvinyl alcohol films; it can also be used in daily cosmetics and high frequency quenching agent.
At present, the purity of the commercial polyvinyl alcohol is 92-94%, and when the polyvinyl alcohol is used as an industrial raw material, the polyvinyl alcohol needs to be dissolved into an aqueous solution; the density of the flake, flocculent or powdery solid polyvinyl alcohol is 1.27-1.31 g/cm3(ii) a Therefore, when the water-soluble organic silicon compound is dissolved in water, the phenomena of wall adhesion and bottom precipitation can be generated in a dissolving device, the dissolving speed is low, and the dissolving time is long.
Polyvinyl alcohol is conventionally used as follows: polyvinyl alcohol resin series products can be dissolved in hot water below 95 ℃, but due to the difference of polymerization degree and alcoholysis degree, and the difference of alcoholysis modes and the like, the dissolution time and temperature have certain difference, so when polyvinyl alcohol resins of different brands are used, the dissolution method and time need to be groped; when in dissolving, the product can be slowly added into cold water with the temperature of about 20 ℃ while stirring to fully swell and disperse and escape volatile materials (the product can be directly dissolved by adding the product into water with the temperature of more than 40 ℃ to avoid the bag-shaped and skin-dissolved endogenous phenomenon, namely the phenomenon of entrainment), then the temperature is increased to about 95 ℃ to accelerate the dissolution, the temperature is kept for 2 to 2.5 hours until the solution does not contain micro particles any more, and the solution can be used for standby after impurities are filtered by 28-mesh stainless steel; the stirring speed is 70-100 r/m, and indirect heating modes such as a jacket, a water bath and the like can be adopted during temperature rise, and direct heating by water vapor can also be adopted; however, direct heating by open fire is not possible, so that the decomposition by local overheating is avoided, and the dissolution can be carried out by blowing steam in a tangential direction without a stirrer.
Disclosure of Invention
The invention aims to solve the problems that the conventional industrial polyvinyl alcohol product on the market is dissolved in water, the phenomena of wall adhesion and bottom precipitation are generated in a dissolving device, the dissolving speed is low, and the dissolving time is long.
The purpose of the invention is realized as follows: a method of making expanded polyvinyl alcohol comprising the steps of:
1) preparation of a special auxiliary agent: mixing hexadecylamine polyoxyethylene ether and polyethylene glycol to obtain a special auxiliary agent, wherein the mass ratio of the hexadecylamine polyoxyethylene ether to the polyethylene glycol is 1: 0.5-1.5;
2) preparing expanded polyvinyl alcohol: feeding a conventional industrial polyvinyl alcohol particle raw material into an extrusion cavity of a screw extruder under the action of a feeder controlled by frequency conversion, spraying the special auxiliary agent prepared in the step 1) into the extrusion cavity of the screw extruder, extruding the special auxiliary agent through the extrusion cavity to obtain expanded polyvinyl alcohol, and then cutting the expanded polyvinyl alcohol into expanded polyvinyl alcohol fibrous finished products through a cutter of the screw extruder; wherein 5-10L of special additive is added into every 1 ton of polyvinyl alcohol particles, and the mass concentration of the special additive is controlled to be 1-10%; the temperature in the extrusion cavity is 90-110 ℃, and the pressure is 3-6 MPa.
In the step 1), the mass ratio of the hexadecylamine polyoxyethylene ether to the polyethylene glycol is 1: 1.
In the step 1), 6L of special auxiliary agent is added into every 1 ton of polyvinyl alcohol particles.
In the step 1), the mass concentration of the special additive is 5%.
The invention has the following beneficial effects: the invention discloses a method for preparing expanded polyvinyl alcohol, wherein conventional industrial polyvinyl alcohol particles enter an extrusion cavity of a screw expander under the action of a feeder controlled by frequency conversion, and special additives are sprayed simultaneously, the flow area in the cavity is gradually reduced, materials are subjected to shearing, kneading and friction during movement, the temperature of the materials is suddenly increased to 90-110 ℃, the pressure is suddenly increased to 3-6 MPa, the materials become plastic colloid, after extrusion die orifices are extruded, the materials are suddenly exposed to normal temperature and normal pressure, high-temperature water in the materials is suddenly vaporized, the materials are expanded to become loose and porous expanded polyvinyl alcohol, and then the loose and porous expanded polyvinyl alcohol is cut into expanded polyvinyl alcohol fibrous finished products by a cutter arranged on the screw expander; the industrial polyvinyl alcohol particles can be expanded by 10-20 times, do not adhere to the wall and sink in a dissolving device, and can be dissolved in water at 95 ℃ within 5-10 minutes, while the conventional granular and powdery polyvinyl alcohol sold in the market is difficult to dissolve due to sticking to the wall and sinking in water at 100 ℃ within 2-3 hours, so that the expanded polyvinyl alcohol prepared by the invention can greatly shorten the dissolving time, solves the problem of difficulty in dissolving the polyvinyl alcohol by downstream customers, and has obvious superiority; measuring the specific surface area of the expanded polyvinyl alcohol by adopting a gas adsorption BET method, wherein the specific surface area is 10-20 times that of similar industrial grade polyvinyl alcohol particles; in summary, the invention has the advantages of simple preparation process, large specific surface area of the prepared expanded polyvinyl alcohol and strong solubility.
Detailed Description
The invention is further illustrated by the following examples, without restricting the invention thereto.
The screw extruder used in the present invention is a DXY 75-III screw extruder from Asahi Asia mechanical Equipment Co., Ltd.
The specification and the manufacturer of various raw materials used in the invention are as follows:
note: (1) PVA 1788: industrial polyvinyl alcohol with a designation 1788; (2) PVA 1799: industrial polyvinyl alcohol with a designation 1799; (3) PVA 2488: polyvinyl alcohol, an industrial product of the brand 2488; (4) PVA 2499: commercial product polyvinyl alcohol with a designation of 2499.
Example 1
1) Preparation of a special auxiliary agent: mixing hexadecylamine polyoxyethylene ether and polyethylene glycol to obtain a special auxiliary agent, wherein the mass ratio of the hexadecylamine polyoxyethylene ether to the polyethylene glycol is 1: 1;
2) preparing expanded polyvinyl alcohol: feeding a conventional industrial polyvinyl alcohol particle (PVA 1788) raw material into an extrusion cavity of a screw extruder under the action of a feeder controlled by frequency conversion, spraying the special auxiliary agent prepared in the step 1) into the extrusion cavity of the screw extruder, extruding the special auxiliary agent by the extrusion cavity to obtain expanded polyvinyl alcohol, and then cutting the expanded polyvinyl alcohol into expanded polyvinyl alcohol whisker-shaped finished products by a cutter of the screw extruder; wherein 6L of special additive is added into every 1 ton of polyvinyl alcohol particles, and the mass concentration of the special additive is controlled to be 5%; the temperature in the extrusion cavity is 90-110 ℃, and the pressure is 3-6 MPa;
the specific surface area of the expanded polyvinyl alcohol whisker-shaped finished product is 16 times of that of the industrial polyvinyl alcohol (PVA 1788) particles, the expanded polyvinyl alcohol whisker-shaped finished product can float on the water surface and can be dissolved in hot water at 95 ℃ for 10 minutes, and the dissolution time of the industrial polyvinyl alcohol (PVA 1788) particles in the hot water at 95 ℃ is 120 minutes, so that the phenomena of bottom sinking and wall sticking of the conventionally prepared polyvinyl alcohol in the water solution are overcome, and the dissolution speed is accelerated.
Example 2
1) Preparation of a special auxiliary agent: mixing hexadecylamine polyoxyethylene ether and polyethylene glycol to obtain a special auxiliary agent, wherein the mass ratio of the hexadecylamine polyoxyethylene ether to the polyethylene glycol is 1: 1;
2) preparing expanded polyvinyl alcohol: feeding a conventional industrial polyvinyl alcohol particle (PVA 1799) raw material into an extrusion cavity of a screw extruder under the action of a feeder controlled by frequency conversion, spraying the special auxiliary agent prepared in the step 1) into the extrusion cavity of the screw extruder, extruding the special auxiliary agent by the extrusion cavity to obtain expanded polyvinyl alcohol, and then cutting the expanded polyvinyl alcohol into expanded polyvinyl alcohol fibrous finished products by a cutter of the screw extruder; wherein 6L of special additive is added into every 1 ton of polyvinyl alcohol particles, and the mass concentration of the special additive is controlled to be 5%; the temperature in the extrusion cavity is 90-110 ℃, and the pressure is 3-6 MPa;
the specific surface area of the expanded polyvinyl alcohol whisker-shaped finished product is 14 times of that of the industrial polyvinyl alcohol (PVA 1799) particles, the expanded polyvinyl alcohol whisker-shaped finished product can float on the water surface and can be dissolved in hot water at 95 ℃ for 10 minutes, and the dissolution time of the industrial polyvinyl alcohol (PVA 1799) particles in the hot water at 95 ℃ is 120 minutes, so that the phenomena of bottom sinking and wall sticking of the conventionally prepared polyvinyl alcohol in the water solution are overcome, and the dissolution speed is accelerated.
Example 3
1) Preparation of a special auxiliary agent: mixing hexadecylamine polyoxyethylene ether and polyethylene glycol to obtain a special auxiliary agent, wherein the mass ratio of the hexadecylamine polyoxyethylene ether to the polyethylene glycol is 1: 1;
2) preparing expanded polyvinyl alcohol: feeding a conventional industrial polyvinyl alcohol particle (PVA 2488) raw material into an extrusion cavity of a screw extruder under the action of a feeder controlled by frequency conversion, spraying the special auxiliary agent prepared in the step 1) into the extrusion cavity of the screw extruder, extruding the special auxiliary agent by the extrusion cavity to obtain expanded polyvinyl alcohol, and then cutting the expanded polyvinyl alcohol into expanded polyvinyl alcohol whisker-shaped finished products by a cutter of the screw extruder; wherein 6L of special additive is added into every 1 ton of polyvinyl alcohol particles, and the mass concentration of the special additive is controlled to be 5%; the temperature in the extrusion cavity is 90-110 ℃, and the pressure is 3-6 MPa;
the specific surface area of the expanded polyvinyl alcohol whisker-shaped finished product is 13.5 times of that of the industrial polyvinyl alcohol (PVA 2488) particles, the expanded polyvinyl alcohol whisker-shaped finished product can float on the water surface and can be dissolved in hot water at 95 ℃ for 10 minutes, and the dissolution time of the industrial polyvinyl alcohol (PVA 2488) particles in the hot water at 95 ℃ is 120 minutes, so that the phenomena of bottom sinking and wall sticking of the conventionally prepared polyvinyl alcohol in the water solution are overcome, and the dissolution speed is accelerated.
Example 4
1) Preparation of a special auxiliary agent: mixing hexadecylamine polyoxyethylene ether and polyethylene glycol to obtain a special auxiliary agent, wherein the mass ratio of the hexadecylamine polyoxyethylene ether to the polyethylene glycol is 1: 1;
2) preparing expanded polyvinyl alcohol: feeding a conventional industrial polyvinyl alcohol particle (PVA 2499) raw material into an extrusion cavity of a screw extruder under the action of a feeder controlled by frequency conversion, spraying the special auxiliary agent prepared in the step 1) into the extrusion cavity of the screw extruder, extruding the special auxiliary agent by the extrusion cavity to obtain expanded polyvinyl alcohol, and then cutting the expanded polyvinyl alcohol into expanded polyvinyl alcohol whisker-shaped finished products by a cutter of the screw extruder; wherein 6L of special additive is added into every 1 ton of polyvinyl alcohol particles, and the mass concentration of the special additive is controlled to be 5%; the temperature in the extrusion cavity is 90-110 ℃, and the pressure is 3-6 MPa;
the specific surface area of the expanded polyvinyl alcohol whisker-shaped finished product is 12 times of that of the industrial polyvinyl alcohol (PVA 2499) particles, the expanded polyvinyl alcohol whisker-shaped finished product can float on the water surface and can be dissolved in hot water at 95 ℃ for 10 minutes, and the dissolution time of the industrial polyvinyl alcohol (PVA 2499) particles in the hot water at 95 ℃ is 120 minutes, so that the phenomena of bottom sinking and wall sticking of the conventionally prepared polyvinyl alcohol in the water solution are overcome, and the dissolution speed is accelerated.
The above description is only a basic description of the present invention, and any equivalent changes made according to the technical solution of the present invention should fall within the protection scope of the present invention.
Claims (4)
1. A method for preparing expanded polyvinyl alcohol is characterized in that: the method comprises the following steps:
preparation of a special auxiliary agent: mixing hexadecylamine polyoxyethylene ether and polyethylene glycol to obtain a special auxiliary agent, wherein the mass ratio of the hexadecylamine polyoxyethylene ether to the polyethylene glycol is 1: 0.5-1.5;
preparing expanded polyvinyl alcohol: feeding a conventional industrial polyvinyl alcohol particle raw material into an extrusion cavity of a screw extruder under the action of a feeder controlled by frequency conversion, spraying the special auxiliary agent prepared in the step 1) into the extrusion cavity of the screw extruder, extruding the special auxiliary agent through the extrusion cavity to obtain expanded polyvinyl alcohol, and then cutting the expanded polyvinyl alcohol into expanded polyvinyl alcohol fibrous finished products through a cutter of the screw extruder; wherein 5-10L of special additive is added into every 1 ton of polyvinyl alcohol particles, and the mass concentration of the special additive is controlled to be 1-10%; the temperature in the extrusion cavity is 90-110 ℃, and the pressure is 3-6 MPa.
2. The process of claim 1, wherein the expanded polyvinyl alcohol comprises: in the step 1), the mass ratio of the hexadecylamine polyoxyethylene ether to the polyethylene glycol is 1: 1.
3. The process of claim 1, wherein the expanded polyvinyl alcohol comprises: in the step 1), 6L of special auxiliary agent is added into every 1 ton of polyvinyl alcohol particles.
4. The process of claim 1, wherein the expanded polyvinyl alcohol comprises: in the step 1), the mass concentration of the special additive is 5%.
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| CN201810831454.1A CN109054265B (en) | 2018-07-26 | 2018-07-26 | Method for preparing expanded polyvinyl alcohol |
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| CN201810831454.1A CN109054265B (en) | 2018-07-26 | 2018-07-26 | Method for preparing expanded polyvinyl alcohol |
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| CN109054265B true CN109054265B (en) | 2021-02-05 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0965609A2 (en) * | 1998-06-16 | 1999-12-22 | National Starch and Chemical Investment Holding Corporation | Biodegradable expanded starch products and the method of preparation |
| CN103030909A (en) * | 2012-12-28 | 2013-04-10 | 上海金树树脂粉末有限公司 | Expanded polyvinyl alcohol and preparation method thereof |
| CN103483598A (en) * | 2013-09-26 | 2014-01-01 | 重庆理工大学 | Method for accelerating polyvinyl alcohol dissolution |
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- 2018-07-26 CN CN201810831454.1A patent/CN109054265B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0965609A2 (en) * | 1998-06-16 | 1999-12-22 | National Starch and Chemical Investment Holding Corporation | Biodegradable expanded starch products and the method of preparation |
| CN103030909A (en) * | 2012-12-28 | 2013-04-10 | 上海金树树脂粉末有限公司 | Expanded polyvinyl alcohol and preparation method thereof |
| CN103483598A (en) * | 2013-09-26 | 2014-01-01 | 重庆理工大学 | Method for accelerating polyvinyl alcohol dissolution |
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