CN111592726A - Preparation method of special material for chlorination of coating-grade perchloroethylene resin - Google Patents
Preparation method of special material for chlorination of coating-grade perchloroethylene resin Download PDFInfo
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- CN111592726A CN111592726A CN202010489410.2A CN202010489410A CN111592726A CN 111592726 A CN111592726 A CN 111592726A CN 202010489410 A CN202010489410 A CN 202010489410A CN 111592726 A CN111592726 A CN 111592726A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions 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 a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions 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 a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions 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 a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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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
- C08F8/00—Chemical modification by after-treatment
- C08F8/18—Introducing halogen atoms or halogen-containing groups
- C08F8/20—Halogenation
- C08F8/22—Halogenation by reaction with free halogens
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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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/18—Plasticising macromolecular 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
- C08J2327/00—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 a halogen; Derivatives of such polymers
- C08J2327/02—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 a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—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 a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
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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
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/26—Cellulose ethers
- C08J2401/28—Alkyl ethers
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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
- C08J2429/00—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
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D127/00—Coating compositions based on 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 a halogen; Coating compositions based on derivatives of such polymers
- C09D127/22—Coating compositions based on 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 a halogen; Coating compositions based on derivatives of such polymers modified by chemical after-treatment
- C09D127/24—Coating compositions based on 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 a halogen; Coating compositions based on derivatives of such polymers modified by chemical after-treatment halogenated
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Abstract
The invention provides a preparation method of a special material for chlorination of coating-grade perchloroethylene resin, which comprises the steps of preheating polyvinyl chloride resin in a vacuum oscillator with an electromagnetic heating function, keeping the temperature, adding other raw materials in batches, and cooling to obtain a finished product. The invention has the advantages of less equipment investment, large material molecular gap, bulking and drying, good swelling and dispersing effects, capability of obtaining the special raw material for chlorination of the coating grade perchloroethylene resin with the required chlorine passing amount of more than 63 percent, no need of researching and developing a production formula and improving large-scale equipment, extremely easy control of process, extremely high efficiency and very obvious economic benefit.
Description
Technical Field
The invention relates to the field of polyvinyl chloride resin, in particular to a preparation method of a material special for chlorination of coating-grade perchloroethylene resin.
Background
Polyvinyl chloride is a thermoplastic high molecular polymer polymerized from vinyl chloride monomer, and white powder with the particle size of 50-250um plays an important role in the structural characteristics of suspended polyvinyl chloride resin, in addition to the control factors such as molecular weight and distribution thereof, crystallinity and branching. The polyvinyl chloride resin is used as a raw material of the coating grade perchloroethylene resin, and the particle structure of the PVC resin has important influence on the quality and the chlorination process performance of the coating grade perchloroethylene resin product. Therefore, it is necessary to prepare a raw material for chlorination of coating grade perchloroethylene resin which requires large molecular pores, bulky and uniform particles, low polymerization degree, large specific surface area and a chlorine passing amount of more than 63%.
The processes of the currently disclosed patents CN 102443085A, CN 101195671A, CN101717459B, CN104277169A and CN108192001A are mainly characterized in that after polyvinyl alcohol with low alcoholysis degree and vinyl chloride monomer are premixed uniformly in a polymerization kettle in advance, materials such as deionized water, composite dispersant copolymer, pH regulator, heat stabilizer, chain transfer agent, initiator and the like are added into the polymerization kettle for polymerization reaction. The disadvantages are: the process is complicated, the equipment is complex, the process requirement is high, and the obtained special material particles for chlorination are looser than common polyvinyl chloride resin, have little or no surface skin, regular resin particle shape and loose structure. However, the high-chlorine-content raw material used as the coating-grade perchloroethylene resin cannot be used as a process for expanding and bulking inner holes, capillaries and gaps of particles and easily realizing high chlorination, and the chlorination speed and the chlorination uniformity cannot maximize the diffusion of chlorine in polyvinyl chloride particles, so that the special raw material for chlorination of the coating-grade perchloroethylene resin with the required chlorine passing amount of more than 63 percent is obtained.
Disclosure of Invention
The invention mainly aims to provide a preparation method of a special material for chlorination of coating-grade perchloroethylene resin, which solves the problem that the chlorine passing amount of common polyvinyl chloride resin or the special material resin for chlorination can not reach more than 63 percent in the chlorination process of an aqueous phase suspension method, and also solves the problem that the special resin for chlorination meeting the chlorine passing requirement of the coating-grade perchloroethylene resin can be obtained only by using the elimination processes such as a full solvent method or a semi-solvent method and the like due to the raw material problem.
The invention provides a preparation method of a special material for chlorination of coating-grade perchloroethylene resin, which comprises the following steps:
heating polyvinyl chloride resin to 80-100 ℃ in a vacuum shaking machine with an electromagnetic heating function, preheating, shaking and overturning, keeping the temperature, adding bentonite plasticizing oil, shaking and overturning, continuing to keep the temperature, adding an emulsifier and a dispersant, shaking and overturning, stopping heating, continuing to stir, introducing nitrogen, and cooling to normal temperature to obtain the special material for chlorination of coating-grade perchloroethylene resin.
The polymerization degree of the polyvinyl chloride resin is 650-1150.
The swelling plasticizing oil is phthalate swelling plasticizing oil, and the using amount of the swelling plasticizing oil is 15-20% of the mass of the polyvinyl chloride resin. Further, the phthalate ester swelling plasticizing oil is dibutyl phthalate.
The emulsifier is at least one of sorbitan monolaurate, sorbitan palmitate, sorbitan monostearate, sorbitan monooleate and sodium dodecyl benzene sulfonate, and the using amount of the emulsifier is 1-3% of the mass of the polyvinyl chloride resin.
The dispersing agent is polyvinyl alcohol PVA and hydroxypropyl methyl cellulose HPMC (hereinafter referred to as polyvinyl alcohol composite dispersing agent) with the mass ratio of 1:1, and the dosage is 1-3% of the mass of the polyvinyl chloride resin.
According to the invention, the swelling plasticizer, the emulsifier and the dispersant are added after the PVC resin is preheated to the vitrification temperature, so that the swelling plasticizer oil is absorbed into molecular pores between primary particles and aggregates of the PVC resin and quickly fills inner holes and gaps of resin particles, thereby obtaining the bulk dried raw material special for chlorination of the coating-grade perchloroethylene resin which is easy to meet the high chlorination technological requirements.
Advantageous effects
The invention has the advantages of less equipment investment, large material molecular gap, bulking and drying, good swelling and dispersing effects, capability of obtaining the special raw material for chlorination of the coating grade perchloroethylene resin with the required chlorine passing amount of more than 63 percent, no need of researching and developing a production formula and improving large-scale equipment, extremely easy control of process, extremely high efficiency and very obvious economic benefit.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
In order to make those skilled in the art better understand the technical solution of the present invention, the following will clearly and completely describe the technical solution of the present invention in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, shall fall within the scope of the present invention.
It is noted that the terms first, second and the like in the description and in the claims of the present invention are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those described herein. Furthermore, the terms "comprising" and "having," as well as any variations thereof, are intended to cover non-exclusive inclusions.
The properties of commercially available SG-5, SG-6 and SG-8 polyvinyl chloride resins are shown as follows:
from the above table, it can be known that the lower the viscosity of the model resin, the higher the polymerization temperature, the deeper the coalescence degree of the primary particles in the particles, the lower the porosity, and the lower the oil absorption rate, so when selecting the model resin with higher viscosity, the larger the particles, the larger the porosity, and the more desirable the high porosity of the oil absorption rate, but the higher the viscosity of the prepared perchloroethylene resin is inevitably, and the perchloroethylene resin cannot be sprayed as a coating, so the raw material selection of the polyvinyl chloride resin needs to be adjusted according to the actual requirements.
Example 1
Adding 1000 kg of SG-5 polyvinyl chloride resin into a vacuum shaking machine with the volume of 3000L and the electromagnetic heating function, starting heating to 80 ℃, keeping the temperature for 10 minutes under shaking and overturning, then adding 190 kg of dibutyl phthalate, keeping the temperature for 5 minutes, then adding 20 kg of sorbitan monolaurate and 30 kg of polyvinyl alcohol composite dispersant, keeping the temperature for 7 minutes, stopping heating, continuing shaking and overturning, introducing nitrogen, and cooling to normal temperature to obtain a finished product.
Comparative example 1
1000 kg of SG-5 polyvinyl chloride resin is added into a mixing stirrer with the volume of 3000L, and 190 kg of dibutyl phthalate, 20 kg of sorbitan monolaurate and 30 kg of polyvinyl alcohol composite dispersant are added in sequence under the condition of stirring and stirred for 30 minutes to obtain a finished product.
Example 2
Adding 1000 kg of SG-6 polyvinyl chloride resin into a vacuum shaking machine with the volume of 3000L and the electromagnetic heating function, starting heating to 80 ℃, keeping the temperature for 10 minutes under shaking and overturning, then adding 160 kg of dibutyl phthalate, keeping the temperature for 5 minutes, then adding 20 kg of sorbitan monolaurate and 30 kg of polyvinyl alcohol composite dispersant, keeping the temperature for 7 minutes, stopping heating, continuing shaking and overturning, introducing nitrogen, and cooling to normal temperature to obtain a finished product.
Comparative example 2
1000 kg of SG-6 polyvinyl chloride resin is added into a mixing stirrer with the volume of 3000L, 160 kg of dibutyl phthalate, 20 kg of sorbitan monolaurate and 30 kg of polyvinyl alcohol composite dispersant are added in sequence under the condition of stirring, and the mixture is stirred for 30 minutes to obtain a finished product.
Example 3
Adding 1000 kg of SG-8 polyvinyl chloride resin into a vacuum shaking machine with the volume of 3000L and an electromagnetic heating function, starting heating to 80 ℃, keeping the temperature for 10 minutes under shaking and overturning, then adding 140 kg of dibutyl phthalate, keeping the temperature for 5 minutes, then adding 20 kg of sorbitan monolaurate and 30 kg of polyvinyl alcohol composite dispersant, keeping the temperature for 7 minutes, stopping heating, continuing shaking and overturning, introducing nitrogen, and cooling to normal temperature to obtain a finished product.
Comparative example 3
1000 kg of SG-8 polyvinyl chloride resin is added into a mixing stirrer with the volume of 3000L, 140 kg of dibutyl phthalate, 20 kg of sorbitan monolaurate and 30 kg of polyvinyl alcohol composite dispersant are added in sequence under the condition of stirring, and the mixture is stirred for 30 minutes to obtain a finished product.
Table of parameters of different raw material examples
| Parameter(s) | Example 1 | Comparative example 1 | Example 2 | Comparative example 2 | Example 3 | Comparative example 3 |
| Number of meshes | 60 | 80 | 60 | 80 | 60 | 80 |
| Apparent appearance | Drying and bulking | Increased oil leakage | Drying and bulking | Increased oil leakage | Drying and bulking | Increased oil leakage |
As can be seen from the above table, examples 1, 2 and 3, after heating, had larger particle sizes and were dry and bulky than the unheated comparative examples 1, 2 and 3.
250 kg of the PVC chlorination special material (produced in batches, not shown) obtained in the examples 1 to 3 and the comparative examples 1 to 3, 3500 kg of water, an initiator, a surfactant and a proper amount of a dispersing agent are filled in an enamel reactor with the volume of 5000L, after the temperature reaches 80 ℃, the temperature is kept and chlorine is introduced after the air is replaced by nitrogen, and then the temperature is reduced, and the perchloroethylene resin is obtained after the procedures of water washing, neutralization, centrifugation and drying.
Chlorination parameter tables for different raw materials
| Parameter(s) | Example 1 | Comparative example 1 | Example 2 | Comparative example 2 | Example 3 | Comparative example 3 |
| Chlorine flux | 64% | 55% | 63% | 52% | 63% | 52% |
| Viscosity (10% xylene solution, paint 4) | 18 seconds | Swelling and dissolving | 16 seconds | Swelling and dissolving | 12 seconds | Swelling and dissolving |
As can be seen from the above table, the coating materials of examples 1 and 2 meet the standards of the perchloroethylene resin for HG/T2002-.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A preparation method of a coating-grade perchloroethylene resin chlorination special material comprises the following steps:
heating polyvinyl chloride resin to 80-100 ℃ in a vacuum shaking machine with an electromagnetic heating function, preheating, shaking and overturning, keeping the temperature, adding bentonite plasticizing oil, shaking and overturning, continuing to keep the temperature, adding an emulsifier and a dispersant, shaking and overturning, stopping heating, continuing to stir, introducing nitrogen, and cooling to normal temperature to obtain the special material for chlorination of coating-grade perchloroethylene resin.
2. The method of claim 1, wherein: the polymerization degree of the polyvinyl chloride resin is 650-1150.
3. The method of claim 1, wherein: the swelling plasticizing oil is phthalate swelling plasticizing oil, and the using amount of the swelling plasticizing oil is 15-20% of the mass of the polyvinyl chloride resin.
4. The method of claim 1, wherein: the emulsifier is at least one of sorbitan monolaurate, sorbitan palmitate, sorbitan monostearate, sorbitan monooleate and sodium dodecyl benzene sulfonate, and the using amount of the emulsifier is 1-3% of the mass of the polyvinyl chloride resin.
5. The method of claim 1, wherein: the dispersing agent is polyvinyl alcohol PVA and hydroxypropyl methyl cellulose HPMC in a mass ratio of 1:1, and the dosage of the dispersing agent is 1-3% of the mass of the polyvinyl chloride resin.
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| CN202010489410.2A CN111592726A (en) | 2020-06-02 | 2020-06-02 | Preparation method of special material for chlorination of coating-grade perchloroethylene resin |
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| CN202010489410.2A CN111592726A (en) | 2020-06-02 | 2020-06-02 | Preparation method of special material for chlorination of coating-grade perchloroethylene resin |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2996489A (en) * | 1958-01-08 | 1961-08-15 | Goodrich Co B F | Resin compositions of improved tolerance for high temperatures and process of producing same |
| CN85106427A (en) * | 1985-08-28 | 1987-03-18 | 湖北省化学研究所 | The solid-phase chlorination method of chloride coatings polyvinyl chloride |
| CN109071706A (en) * | 2016-03-08 | 2018-12-21 | 氧乙烯有限合伙公司 | The method of chliorinated polyvinyl chloride |
-
2020
- 2020-06-02 CN CN202010489410.2A patent/CN111592726A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2996489A (en) * | 1958-01-08 | 1961-08-15 | Goodrich Co B F | Resin compositions of improved tolerance for high temperatures and process of producing same |
| CN85106427A (en) * | 1985-08-28 | 1987-03-18 | 湖北省化学研究所 | The solid-phase chlorination method of chloride coatings polyvinyl chloride |
| CN109071706A (en) * | 2016-03-08 | 2018-12-21 | 氧乙烯有限合伙公司 | The method of chliorinated polyvinyl chloride |
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Address after: Room 101, No.12, Lane 1661, Jialuo Road, Jiading District, Shanghai, 201800 j89 Applicant after: Shanghai Baoqian New Material Technology Co.,Ltd. Address before: Room 101, No.12, Lane 1661, Jialuo Road, Jiading District, Shanghai, 201800 j89 Applicant before: Shanghai Baoqian Chemical Co.,Ltd. |
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