CN116178597A - Production method of extinction polyvinyl chloride paste resin - Google Patents
Production method of extinction polyvinyl chloride paste resin Download PDFInfo
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- CN116178597A CN116178597A CN202111434217.XA CN202111434217A CN116178597A CN 116178597 A CN116178597 A CN 116178597A CN 202111434217 A CN202111434217 A CN 202111434217A CN 116178597 A CN116178597 A CN 116178597A
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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
- C08F114/00—Homopolymers 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
- C08F114/02—Monomers containing chlorine
- C08F114/04—Monomers containing two carbon atoms
- C08F114/06—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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
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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
Abstract
The production process of extinction polyvinyl chloride paste resin includes a) curing desalted water, copper chloride solution, sodium metabisulfite, buffering agent, catalyst and emulsifier, adding vinyl chloride, cross-linking agent, emulsifier and catalyst successively, and adding dodecyl alcohol in 6-10 weight portions to obtain seed when the reaction pressure is reduced to 40% of initial pressure; b) Adding desalted water, the seeds, the copper chloride solution, sodium metabisulfite, a buffer, a catalyst and a part of emulsifying agent for reaction, continuously adding vinyl chloride, the emulsifying agent and the catalyst in the reaction until the designed feeding amount is reached, ending the reaction when the reaction pressure is reduced to 40% of the initial pressure, and drying to obtain the product.
Description
Technical Field
The invention relates to a production method of extinction polyvinyl chloride paste resin.
Background
Along with the improvement of the living standard of people and the change of aesthetic ideas, in different occasions, people need different gloss plastic products, and the existing extinction modes mainly comprise physical extinction and chemical extinction, and the specific mechanism is as follows: the surface of the product is formed with very small concave-convex or very small wrinkles by using a physical or chemical method, and the concave-convex or the wrinkles can generate diffuse reflection and scattering effects on light rays, so that the glossiness of the surface of the product is reduced.
Li Sheng et al, "study of matting properties of gel-containing matt PVC resins" ("chemical production and technique", volume 10, phase 4, 2003) describe the properties of matt PVC resins and study of the effect of crosslinking agents on matting properties. When the influence of the cross-linking agent is studied, the method adopted comprises cross-linking and copolymerizing the cross-linking agent and vinyl chloride, then blending the obtained copolymer with common PVC resin, and measuring the extinction property after processing the copolymer into sheets. The results show that when the gel content and the swelling degree are substantially the same, the kind of the crosslinking agent has little influence on the matting property, which is mainly influenced by the gel content of the resin and the crosslinking density of the gel.
Although the "study of matting properties of gel-containing matt PVC resins" of Li Sheng et al gives a method for producing matt PVC resins using a crosslinking agent, the method of blending two PVC has room for improvement in both mixing uniformity and processing difficulty.
Seed emulsion polymerization is a typical method of preparing core-shell emulsions, and the polymers formed are generally homopolymers or copolymers, so the method of preparation is essentially the same as the usual emulsion polymerization process. The shell monomer may be added according to the manner of addition, and may be divided into batch process, swelling process, semi-continuous process, and continuous process. The batch process is to add seed emulsion, water, initiator, emulsifier and shell monomer into a reactor at one time according to the formula, and heat the mixture to the reaction temperature for polymerization. Seed emulsions are typically used in amounts of only 1% of the finished emulsion and thus have essentially no effect on the properties of the emulsion film, unlike the effect of checking the properties of emulsion films in contemporary popular core-shell emulsion polymerizations.
In view of the state of the art, there is still a need in the art to find a method for producing matt polyvinyl chloride, which not only has the advantages of simple processing and uniform and consistent properties of the obtained matt resin, but also has good processability.
Disclosure of Invention
The invention aims to provide a production method of extinction polyvinyl chloride, which has the advantages of simple processing and uniform and consistent performance of the obtained extinction resin, and the obtained extinction resin has good processing performance.
Accordingly, the present invention relates to a process for preparing a matted polyvinyl chloride resin by a seed polymerization process, comprising:
a) Adding desalted water, copper chloride solution, sodium metabisulfite, buffer, catalyst and emulsifier into a seed polymerization kettle for curing for 0.5-1.5h, then reacting, continuously adding vinyl chloride, cross-linking agent, emulsifier and catalyst in the reaction, and adding 6-10 parts by weight of dodecanol when the reaction pressure is reduced to 40% of the initial pressure to obtain seeds;
b) Adding desalted water, the seeds, the copper chloride solution, sodium metabisulfite, a buffer, a catalyst and part of emulsifier into a seed polymerization kettle for reaction, continuously adding vinyl chloride, the emulsifier and the catalyst in the reaction until the feeding amount is designed, ending the reaction when the reaction pressure is reduced to 40% of the initial pressure, and drying to obtain the product.
The invention also relates to another method for preparing extinction polyvinyl chloride resin by using a seed polymerization method, which comprises the following steps:
a) Adding desalted water, copper chloride solution, sodium metabisulfite, buffer, catalyst, cross-linking agent and emulsifier into a seed polymerization kettle for curing for 0.5-1.5h, then reacting, continuously adding vinyl chloride, emulsifier and catalyst in the reaction, and adding 6-10 parts by weight of dodecanol when the reaction pressure is reduced to 40% of the initial pressure, thus obtaining seeds;
b) Adding desalted water, the seeds, the copper chloride solution, sodium metabisulfite, a buffer, a catalyst and part of emulsifier into a seed polymerization kettle for reaction, continuously adding vinyl chloride, the emulsifier and the catalyst in the reaction until the feeding amount is designed, ending the reaction when the reaction pressure is reduced to 40% of the initial pressure, and drying to obtain the product.
Detailed Description
The method for preparing extinction polyvinyl chloride resin by using seed polymerization method of the invention comprises a seed preparation step and a polymer preparation step, and is characterized in that a cross-linking agent is added in the seed preparation step to form gel with extinction effect, and then the final polyvinyl chloride polymer is formed by using the seed, so that the final product has gel content required by extinction, more importantly, the polyvinyl chloride polymer formed in the way has good processing property and improved gel uniformity, and the property of the product prepared by using the extinction resin is improved.
Seed production
The desalted water suitable for use in the process of the present invention may be conventional deionized water, and in one example of the present invention, the desalted water is used in total amount of 10000 to 14000 parts by weight, preferably 10500 to 13500 parts by weight.
In one embodiment of the present invention, the concentration of the copper chloride solution is 0.1 to 1kg/L, preferably 0.3 to 1.8kg/L, more preferably 0.5 to 1.5kg/L. The copper chloride solution is used in an amount of 0.2 to 1.3 parts by weight, preferably 0.4 to 1.2 parts by weight, more preferably 0.6 to 1.1 parts by weight, based on 10000 parts by weight of desalted water.
In one embodiment of the present invention, the sodium metabisulfite is added in an amount of 10 to 15 parts by weight, preferably 11 to 14 parts by weight, based on 10000 parts by weight of desalted water.
In one example of the invention, the buffer is selected from one or more of sodium bicarbonate, ammonium bicarbonate, or sodium hydroxide. The buffer is added in an amount of 3 to 8 parts by weight, preferably 3.5 to 7.5 parts by weight, based on 10000 parts by weight of desalted water.
In one example of the invention, the catalyst is selected from persulfate catalysts, such as potassium persulfate or ammonium persulfate or mixtures thereof, and the like. The catalyst is added in an amount of 1.0 to 3.0 parts by weight, preferably 1.2 to 2.8 parts by weight, more preferably 1.5 to 2.5 parts by weight, based on 10000 parts by weight of desalted water.
In one embodiment of the present invention, the total amount of the vinyl chloride monomer is 10000 to 14000 parts by weight, preferably 10500 to 13500 parts by weight, more preferably 11000 to 13000 parts by weight, based on 10000 parts by weight of desalted water.
In one example of the invention, the emulsifier is selected from sodium dodecyl sulfate, potassium dodecyl sulfate, or mixtures thereof. The emulsifier is added in an amount of 50 to 80 parts by weight, preferably 55 to 75 parts by weight, more preferably 58 to 72 parts by weight, based on 10000 parts by weight of desalted water.
In one embodiment of the invention, the cross-linking agent is a diene or polyene monomer such as diallyl phthalate, diallyl maleate, ethylene glycol dimethacrylate, polyethylene glycol diacrylate and the like, preferably one or a mixture of two of diallyl phthalate, diallyl maleate or polyethylene glycol diacrylate. The crosslinking agent is added in an amount of 6 to 15 parts by weight, preferably 7 to 14 parts by weight, more preferably 8 to 12 parts by weight, based on 10000 parts by weight of desalted water.
Preferably, the desalted water is fed for one time before polymerization and heating; the copper chloride solution is fed in the mode of feeding before polymerization and heating; the sodium metabisulfite feeding mode is one-time feeding before polymerization temperature rise; the buffer feeding mode is feeding once before polymerization temperature rising.
In one embodiment of the invention, the catalyst is added in such a manner that 0.3 to 1.0 parts by weight is added before the polymerization temperature rises, and the remaining parts by weight are continuously added after the reaction temperature is reached.
In one embodiment of the invention, the vinyl chloride monomer is fed at a rate of 1500 to 3500 parts by weight/h, preferably 1800 to 3200 parts by weight/h, after the reaction temperature is reached, until the formulation is fed
In one embodiment of the invention, the emulsifier is added by adding 6 to 10 parts by weight, preferably 7 to 9 parts by weight, before the temperature is raised, and continuously adding the remaining emulsifier after the reaction has started.
In one embodiment of the invention, after mixing the crosslinking agent with 20 to 30 parts by weight of the emulsifier, the mixture is homogenized at high speed for 10 to 20 minutes and then added to the reaction system. In one embodiment of the invention, the cross-linking agent mixed with the emulsifier is added continuously after the reaction is timed for 20min-30min, and the adding time is controlled to be 30min-40min.
Polymer production
The polymer preparation step of the invention comprises adding desalted water, the seeds obtained above, copper chloride solution, sodium metabisulfite, buffer, catalyst and partial emulsifier into a seed polymerization kettle for reaction, continuously adding vinyl chloride, emulsifier and catalyst in the reaction until the designed feeding amount, ending the reaction when the reaction pressure is reduced to 40% of the initial pressure, and entering a drying section to obtain the product.
In one embodiment of the present invention, the desalted water may be conventional deionized water in a total amount of 10000 to 14000 parts by weight, preferably 10500 to 13500 parts by weight.
The seeds are obtained in the above step, and the seed is added in an amount of 350 to 650 parts by weight, preferably 400 to 600 parts by weight, based on 10000 parts by weight of desalted water.
In one embodiment of the present invention, the concentration of the copper chloride solution is 0.1 to 1kg/L, preferably 0.2 to 0.9kg/L, more preferably 0.3 to 0.8kg/L; the copper chloride solution is added in an amount of 0.3 to 0.9 parts by weight, preferably 0.4 to 0.8 parts by weight, based on 10000 parts by weight of desalted water.
In one embodiment of the present invention, the sodium metabisulfite is added in an amount of 5 to 9 parts by weight, preferably 6 to 8 parts by weight.
In one example of the invention, the buffer is selected from sodium bicarbonate, ammonium bicarbonate, sodium hydroxide, or a mixture thereof; the buffer is added in an amount of 3 to 8 parts by weight, preferably 4 to 7 parts by weight, based on 10000 parts by weight of desalted water.
In one embodiment of the present invention, the catalyst may be the same as or different from the catalyst used in seed production, and is selected from potassium persulfate, ammonium persulfate, a mixture thereof, and the like, and the catalyst is added in an amount of 0.8 to 1.5 parts by weight, preferably 0.9 to 1.4 parts by weight, based on 10000 parts by weight of desalted water.
In one embodiment of the present invention, the total amount of the vinyl chloride monomer is 10000 to 14000 parts by weight, preferably 10500 to 13500 parts by weight, based on 10000 parts by weight of desalted water.
In one embodiment of the present invention, the emulsifier is selected from sodium dodecyl sulfate or potassium dodecyl sulfate, and is added in an amount of 70 to 100 parts by weight, preferably 80 to 95 parts by weight, based on 10000 parts by weight of desalted water.
In one example of the invention, the desalted water is fed for the first time before the polymerization temperature rises; the seed feeding mode is feeding for the first time before polymerization and heating; the copper chloride solution is fed in the mode of one time before polymerization and heating; the sodium metabisulfite is fed for the first time before polymerization temperature rise; the buffer feeding mode is one feeding before polymerization temperature rising.
In one embodiment of the invention, the catalyst is added in such a manner that 0.1 to 0.5 parts by weight, preferably 0.2 to 0.4 parts by weight, is added before the temperature is raised in the polymerization; continuously adding the rest parts by weight after the reaction temperature is reached;
in one embodiment of the invention, the vinyl chloride monomer is fed at a rate of 2000 to 3500 parts by weight/h, preferably 2400 to 3200 parts by weight/h, after reaching the reaction temperature, until the formulation is fed.
In one example of the invention, the emulsifier is added in such a way that 20-30 parts by weight of the emulsifier is added before the temperature is raised, and the rest of the emulsifier is continuously added after the reaction starts;
the extinction polyvinyl chloride paste resin prepared by the method has high gel content and low surface glossiness, can meet the matte demand of the product and has good processability.
The invention is further illustrated below with reference to examples.
Example 1
Preparation of emulsion seeds:
14000 parts by weight of desalted water, 0.7 part by weight of copper chloride solution with a concentration of 0.3kg/L, 12 parts by weight of sodium metabisulfite, 5 parts by weight of sodium bicarbonate, 0.7 part by weight of potassium persulfate and 7 parts by weight of emulsifier are mixed, cured at 48 ℃ for 30min,8 parts by weight of diallyl maleate is mixed with 20 parts by weight of sodium dodecyl sulfate, and the mixture is homogenized at high speed for 15min. After curing, continuously adding vinyl chloride monomer into a polymerization kettle, controlling the reaction temperature to be 48+/-1 ℃, controlling the adding speed of the vinyl chloride monomer to be 2000 parts by weight/h, simultaneously continuously adding 2 parts by weight of catalyst potassium persulfate and 50 parts by weight of emulsifier sodium dodecyl sulfate, adding diallyl maleate mixed solution after 20 minutes of reaction timing, and controlling the adding time to be 30 minutes. Stopping adding vinyl chloride when the vinyl chloride is added to the total feeding amount, continuously reducing the reaction pressure to 40% of the initial pressure, and adding 8 parts by weight of dodecanol to obtain seed latex with the average particle diameter of 0.46 mu m and the solid content of 38%;
vinyl chloride monomer is added in a total of 10000 parts by weight;
preparation of extinction polyvinyl chloride paste resin:
14000 parts by weight of desalted water, 0.6 part by weight of copper chloride solution with the concentration of 0.3kg/L, 7 parts by weight of sodium metabisulfite, 500 parts by weight of seed latex, 3 parts by weight of sodium bicarbonate, 0.2 part by weight of ammonium persulfate and 20 parts of sodium dodecyl sulfate are uniformly mixed in a polymerization kettle, when the temperature reaches 47+/-1 ℃, vinyl chloride monomer is added, the adding speed of vinyl chloride is 3000 parts by weight/h, simultaneously, 1.0 part by weight of catalyst ammonium persulfate and 60 parts by weight of emulsifier sodium dodecyl sulfate are continuously added, when the vinyl chloride is added to the total amount of the materials, the adding of the vinyl chloride is stopped, when the reaction pressure is continuously reduced to 40% of the initial pressure, the reaction is ended, and the extinction polyvinyl chloride paste resin is obtained through spray drying.
The total amount of vinyl chloride monomer added is 11000 parts by weight;
the index results of the obtained resin product were as follows: b viscosity 4350 (10-3 Pa.S), gel content 25%, average degree of polymerization of soluble fraction 1280.
Example 2
Seed preparation:
adding 13000 parts by weight of desalted water, 0.4 part by weight of copper chloride solution with the concentration of 0.5kg/L, 9 parts by weight of sodium metabisulfite, 4 parts by weight of sodium bicarbonate, 0.6 part by weight of potassium persulfate, 15 parts by weight of sodium dodecyl sulfate and 20 parts by weight of polyethylene glycol diacrylate into a polymerization kettle, curing for 0.5 hour at 48+/-1 ℃, then adding vinyl chloride monomer, controlling the reaction temperature to be 48+/-1 ℃, controlling the adding speed of the vinyl chloride monomer to 3000 parts by weight/h, simultaneously continuously adding 2 parts by weight of potassium persulfate and 50 parts by weight of sodium dodecyl sulfate, stopping adding vinyl chloride when the vinyl chloride is added to the total feeding amount, continuously adding 8 parts by weight of dodecanol when the reaction pressure is reduced to 40% of the initial pressure, and obtaining seed latex with the average particle size of 0.43 mu m and the solid content of 36%;
the total amount of vinyl chloride monomer added is 11000 parts by weight;
preparation of extinction polyvinyl chloride paste resin:
14000 parts by weight of desalted water, 0.5 part by weight of copper chloride solution with the concentration of 0.5kg/L, 8 parts by weight of sodium metabisulfite and 650 parts by weight of seed latex, 5 parts by weight of sodium bicarbonate, 0.3 part by weight of ammonium persulfate and 25 parts of sodium dodecyl sulfate are uniformly mixed in a polymerization kettle, when the temperature of the polymerization kettle reaches 48+/-1 ℃, vinyl chloride monomer is added, the adding speed is 2000 parts by weight/h, simultaneously, 1.2 parts by weight of catalyst ammonium persulfate and 70 parts by weight of sodium dodecyl sulfate are continuously added, the reaction temperature is controlled to be stable, when the vinyl chloride is added to the total amount of the materials, the adding of the vinyl chloride is stopped, the reaction is stopped, and when the reaction pressure is reduced to 40% of the initial pressure, the reaction is ended, and the extinction polyvinyl chloride paste resin is obtained through spray drying.
A total of 12000 parts by weight of vinyl chloride monomer was added;
the index results of the obtained resin product were as follows: the viscosity of B was 4420 (10-3 Pa.S), the gel content was 21%, and the average degree of polymerization of the soluble fraction was 1320.
Claims (8)
1. A method for preparing extinction polyvinyl chloride resin by a seed polymerization method, comprising the following steps:
a) Adding desalted water, copper chloride solution, sodium metabisulfite, buffer, catalyst and emulsifier into a seed polymerization kettle for curing for 0.5-1.5h, then reacting, continuously adding vinyl chloride, cross-linking agent, emulsifier and catalyst in the reaction, and adding 6-10 parts by weight of dodecanol when the reaction pressure is reduced to 40% of the initial pressure to obtain seeds;
b) Adding desalted water, the seeds, the copper chloride solution, sodium metabisulfite, a buffer, a catalyst and part of emulsifier into a seed polymerization kettle for reaction, continuously adding vinyl chloride, the emulsifier and the catalyst in the reaction until the feeding amount is designed, ending the reaction when the reaction pressure is reduced to 40% of the initial pressure, and drying to obtain the product.
2. A method for preparing extinction polyvinyl chloride resin by a seed polymerization method, comprising the following steps:
a) Adding desalted water, copper chloride solution, sodium metabisulfite, buffer, catalyst, cross-linking agent and emulsifier into a seed polymerization kettle for curing for 0.5-1.5h, then reacting, continuously adding vinyl chloride, emulsifier and catalyst in the reaction, and adding 6-10 parts by weight of dodecanol when the reaction pressure is reduced to 40% of the initial pressure, thus obtaining seeds;
b) Adding desalted water, the seeds, the copper chloride solution, sodium metabisulfite, a buffer, a catalyst and part of emulsifier into a seed polymerization kettle for reaction, continuously adding vinyl chloride, the emulsifier and the catalyst in the reaction until the feeding amount is designed, ending the reaction when the reaction pressure is reduced to 40% of the initial pressure, and drying to obtain the product.
3. The method of claim 1 or 2, wherein the cross-linking agent is selected from the group consisting of diallyl phthalate, diallyl maleate, ethylene glycol dimethacrylate, polyethylene glycol diacrylate, and mixtures of both.
4. The method according to claim 1 or 2, wherein the crosslinking agent is added in an amount of 6 to 15 parts by weight, preferably 7 to 14 parts by weight, more preferably 8 to 12 parts by weight, based on 10000 parts by weight of desalted water.
5. The method according to claim 1 or 2, wherein in step (a),
the concentration of the copper chloride solution is 0.1 to 1kg/L, preferably 0.3 to 1.8kg/L, more preferably 0.5 to 1.5kg/L. The copper chloride solution is used in an amount of 0.2 to 1.3 parts by weight, preferably 0.4 to 1.2 parts by weight, more preferably 0.6 to 1.1 parts by weight, based on 10000 parts by weight of desalted water;
the sodium metabisulfite is added in an amount of 10-15 parts by weight, preferably 11-14 parts by weight, based on 10000 parts by weight of desalted water;
the buffer is added in an amount of 3 to 8 parts by weight, preferably 3.5 to 7.5 parts by weight, based on 10000 parts by weight of desalted water.
6. A method according to claim 1 or 2, characterized in that the buffer is selected from one or more of sodium bicarbonate, ammonium bicarbonate or sodium hydroxide; the emulsifier is selected from sodium dodecyl sulfate, potassium dodecyl sulfate or a mixture thereof.
7. A method according to claim 1 or 2, characterized in that in step (b) the seeds are added in an amount of 350-650 parts by weight, preferably 400-600 parts by weight, per 10000 parts by weight of desalted water.
8. The method according to claim 1 or 2, wherein in step (b),
the concentration of the copper chloride solution is 0.1 to 1kg/L, preferably 0.2 to 0.9kg/L, more preferably 0.3 to 0.8kg/L; the addition amount of the copper chloride solution is 0.3 to 0.9 part by weight, preferably 0.4 to 0.8 part by weight, based on 10000 parts by weight of desalted water;
the sodium metabisulfite is added in an amount of 5 to 9 parts by weight, preferably 6 to 8 parts by weight, and the buffer is added in an amount of 3 to 8 parts by weight, preferably 4 to 7 parts by weight, based on 10000 parts by weight of desalted water.
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