CN113667369B - Preparation method of efficient anti-sticking coating agent for polyvinyl chloride suspension polymerization - Google Patents
Preparation method of efficient anti-sticking coating agent for polyvinyl chloride suspension polymerization Download PDFInfo
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- CN113667369B CN113667369B CN202110856746.2A CN202110856746A CN113667369B CN 113667369 B CN113667369 B CN 113667369B CN 202110856746 A CN202110856746 A CN 202110856746A CN 113667369 B CN113667369 B CN 113667369B
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- C—CHEMISTRY; METALLURGY
- 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
- C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
- C09D161/04—Condensation polymers of aldehydes or ketones with phenols only
- C09D161/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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- C—CHEMISTRY; METALLURGY
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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Abstract
The invention discloses a preparation method of an efficient kettle adhesion preventing coating agent for polyvinyl chloride suspension polymerization, and relates to the technical field of kettle adhesion preventing agents. The preparation method comprises the following steps: adding 1-naphthol, water and an aqueous solution of sodium hydroxide into a reactor, starting stirring, and replacing air in the reactor; heating the reactor, mixing part or all of sodium formaldehyde sulfoxylate and the formaldehyde aqueous solution, then dropwise adding the mixture into the reactor, and stirring for reaction; cooling, adding water, a benzenesulfonic acid aqueous solution, a polyvinyl alcohol aqueous solution and the balance of sodium formaldehyde sulfoxylate, adjusting the solid content, and stirring to obtain a light yellow phenolic resin aqueous solution product; and standing the obtained product to obtain a light yellow clear anti-sticking coating agent product. The preparation method is simple and easy to operate, the anti-sticking effect is good, the product appearance is a light yellow clear transparent solution, the quality of the resin product is improved, and the storage and use stability of the product is enhanced.
Description
Technical Field
The invention relates to the technical field of anti-sticking kettle agents, in particular to a method for preparing an efficient anti-sticking kettle coating agent for polyvinyl chloride suspension polymerization.
Background
In the polymerization of vinyl chloride, a part of the polymer adheres to the wall of the polymerization vessel, the stirrer and the baffle, which is called as "sticking vessel" and brings great harm to the production of PVC. After the kettle wall is bonded, the heat transfer coefficient of the kettle wall is reduced, the reaction heat cannot be removed in time, the polymerization rate is forced to be reduced, and the polymerization time is prolonged. The viscosity kettle material has low porosity and poor processing and plasticizing performance, and fish eyes are easily generated, so that PVC products are easy to age, and the quality of the products is influenced. The kettle cleaning not only prolongs the auxiliary time of production and reduces the utilization rate of the kettle, but also has bad environment and high labor intensity of manual kettle cleaning, and seriously influences the health and life safety of workers. Preventing the large-scale and continuous production of the kettle.
In order to solve the problems, manufacturers seek high-quality and low-cost anti-sticking kettle agents while improving the productivity. By coating polymerization inhibitor and adding anti-sticking agent, the surface smoothness of the polymerization kettle can be effectively improved, the surface activity of the polymerization kettle wall can be effectively purified, the graft polymerization reaction between the polymerization kettle wall and PVC resin can be prevented, and the problem of kettle sticking can be solved.
The high molecular type anti-sticking kettle coating agent is the most widely used anti-sticking kettle coating agent at present, and the anti-sticking kettle coating agent of American red, English blue, Italian yellow and similar anti-sticking kettle coating agents in China are successfully used for suspension polymerization of various kettle types of PVC, and have good effect. Wherein the anti-sticking agent having too dark color may color the resin and deteriorate the quality. Furthermore, the treatment of the dark waste water discharged during the rinsing process is complicated. Therefore, the development of "italian yellow" like light color series products has received much attention in recent years.
The invention discloses a Chinese patent application 201611151926.6, which discloses an aromatic amine-phenol copolycondensation type anti-sticking kettle agent, comprising the following components in parts by weight: 1-5.1 parts of 1-amino-4-sodium naphthalene sulfonate, 1-5.1 parts of beta-naphthol, 3-7 parts of formaldehyde solution with the concentration of 37%, 10-20 parts of sodium hydroxide solution with the concentration of 30%, 50-100 parts of distilled water, 7 parts of polyvinyl alcohol, 3 parts of sodium alginate and 10 parts of sodium sulfoxylate and hydrogen formaldehyde. The preparation method comprises the following steps: weighing 1-amino-4-sodium naphthalenesulfonate, placing in a three-neck flask, adding distilled water, heating to 50-80 ℃, and stirring to dissolve; then adding sodium hydroxide solution and beta-naphthol, dripping formaldehyde solution into the mixture, and reacting the mixture for 2 to 6 hours at the temperature of between 80 and 100 ℃; cooling to 60-80 ℃, adding polyvinyl alcohol and sodium alginate, and continuing to react for 1 h; stirring and cooling to room temperature, and adding sodium formaldehyde sulfoxylate to obtain the aromatic amine-phenol copolycondensation type anti-sticking kettle agent. The method needs more raw materials, needs to change the temperature step by step and increases the complexity of preparation.
Chinese patent application 201510068651.9 discloses a production method for producing a high impact polyvinyl chloride resin anti-sticking kettle agent, adding refined 1-naphthol, deionized water and sodium hydroxide solution into a reactor, dripping formaldehyde solution into the reactor under an alkaline condition, continuously heating and stirring reaction liquid, after fully reacting for 2 hours, adding film-forming agent polyvinyl alcohol, continuously stirring and reacting, controlling the pH value to be 12-13, cooling to room temperature, adding reductive stabilizer sodium formaldehyde sulfoxylate, and obtaining the high impact polyvinyl chloride resin special anti-sticking kettle agent. The anti-sticking agent effectively solves the problem of sticking a kettle during the suspension emulsion polymerization reaction of the high impact polyvinyl chloride resin. The method also needs the processes of first heating and then cooling, thereby increasing the complexity of preparation.
In view of the above, the present invention provides a method for preparing an anti-sticking coating agent, which has a simple preparation process, and does not require repeated temperature adjustment, and the prepared product has good anti-sticking effect and good appearance, and is beneficial to improving the quality of resin products.
Disclosure of Invention
The invention aims to provide a preparation method of an anti-sticking kettle coating agent, which is simple and easy to operate, the prepared anti-sticking kettle coating agent has good anti-sticking kettle effect on suspension polymerization of polyvinyl chloride, the appearance of the product is light yellow clear transparent solution, the influence of deep color falling objects is effectively avoided, the quality of a resin product is favorably improved, and the storage and use stability of the product is enhanced.
In order to achieve the aim, the invention provides a preparation method of an efficient anti-sticking kettle coating agent for polyvinyl chloride suspension polymerization,
the anti-sticking kettle coating agent comprises the following raw materials in parts by weight:
8-12 parts of sodium formaldehyde sulfoxylate
7-9 parts of 1-naphthol
4-11 parts of formaldehyde solution
8-22 parts of sodium hydroxide solution
45-210 parts of water
Polyvinyl alcohol solution 8-12 parts
8-12 parts of a benzenesulfonic acid solution;
the manufacturing steps are as follows:
(1) adding 1-naphthol, water and a sodium hydroxide solution with the formula dosage into a reactor, starting stirring, and replacing air in the reactor;
(2) heating the reactor, mixing the formaldehyde solution with all or part of sodium formaldehyde sulfoxylate in the formula amount, then dropwise adding the mixture into the reactor, and stirring for reaction;
(3) and cooling, adding water, a benzenesulfonic acid solution, a polyvinyl alcohol solution and the residual sodium formaldehyde sulfoxylate, adjusting the solid content, and stirring to obtain a light yellow phenolic resin aqueous solution product.
(4) And (4) standing the product obtained in the step (3) to obtain a light yellow clear anti-sticking kettle coating agent product.
Wherein the content of the first and second substances,
preferably, the raw materials of the anti-sticking kettle coating agent comprise the following components in parts by weight:
preferably, the 1-naphthol is 99% purified 1-naphthol.
Preferably, the formaldehyde solution is a 37% technical grade formaldehyde aqueous solution.
Preferably, the sodium hydroxide solution is a 32% technical grade aqueous sodium hydroxide solution.
Preferably, the water is one or more of deionized water, drinking water, purified water and distilled water, and is further preferably deionized water.
Preferably, the polyvinyl alcohol solution is a 4.5% polyvinyl alcohol aqueous solution.
Preferably, the benzenesulfonic acid solution is a 30% strength by mass benzenesulfonic acid aqueous solution.
Preferably, in the step (1), the replacement of the air in the reactor means replacement of the air in the reactor with nitrogen or argon.
Preferably, in the step (2), the heating temperature is 80-100 DEG C
Preferably, in step (2), the reactor is maintained in an alkaline environment, and more preferably, the pH is 11 to 13.
Preferably, in the step (2), the dropping time is 1-3 h.
Preferably, in the step (2), the stirring reaction time is 4-12 h.
Preferably, in step (3), the cooling is cooling to room temperature.
Preferably, in the step (3), the adjusted solid content is 5 to 6%.
Preferably, in the step (3), the stirring time is 20-40 min.
Preferably, in the step (4), the standing time is 10 to 15 days.
Compared with the prior art, the invention has the following advantages:
(1) the method has the advantages of simple process flow, easily achieved reaction conditions and easy control.
(2) The obtained anti-sticking kettle coating agent has good appearance clarity and transparency, is similar to the color of polyvinyl chloride resin, effectively avoids the influence of deep-color falling objects, and is beneficial to improving the quality of resin products.
(3) Sodium formaldehyde sulfoxylate which does not participate in the reaction can enhance the oxidation resistance of the product, thereby enhancing the storage and use stability of the product.
Detailed Description
The present invention will be further explained with reference to specific examples in order to make the technical means, the technical features, the technical objectives and the effects of the present invention easier to understand, but the following examples are only preferred embodiments of the present invention, and not all embodiments of the present invention. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative efforts belong to the protection scope of the present invention.
In the following examples, unless otherwise specified, all the procedures and equipment used were conventional equipment.
In the following examples, a 37% industrial-grade formaldehyde solution was purchased from national pharmaceutical products chemical Co., Ltd under the product number 100100620; 32% technical grade sodium hydroxide solution was purchased from alcalid corporation; the polyvinyl alcohol is a polyvinyl alcohol aqueous solution with the mass concentration of 4.5%; the benzenesulfonic acid is a 30% benzenesulfonic acid aqueous solution; the water used was deionized water.
Example 1
Adding 8 parts of 99% refined 1-naphthol, 50 parts of water and 10 parts of 32% sodium hydroxide solution into a reactor, starting stirring, and introducing nitrogen to replace air in the reactor; heating the reactor until the reaction temperature is stabilized at 95 ℃, slowly dropwise adding a mixed solution of 10 parts of sodium formaldehyde sulfoxylate and 10 parts of formaldehyde aqueous solution into the reactor for 2 hours to ensure that the interior of the reactor is in an alkaline environment and the pH value is 11-13; and (3) continuously reacting for 4 hours under the stirring condition, cooling to room temperature, adding 100 parts of water, 10 parts of benzenesulfonic acid aqueous solution and 10 parts of polyvinyl alcohol aqueous solution, stirring for 30min, and standing for 10 days to obtain a transparent light yellow anti-sticking kettle coating agent product with the water-soluble phenolic resin of which the specific gravity is 5-6%.
Example 2
Adding 8 parts of 99% refined 1-naphthol, 50 parts of water and 15 parts of 32% sodium hydroxide solution into a reactor, starting stirring, and introducing argon to replace air in the reactor; heating the reactor until the reaction temperature is stabilized at 97 ℃, slowly dripping the mixed solution of 10 parts of sodium formaldehyde sulfoxylate and 10 parts of formaldehyde aqueous solution into the reactor for 2 hours to ensure that the inside of the reactor is in an alkaline environment and the pH value is 11-13; and (3) continuously reacting for 8 hours under the condition of stirring, cooling to room temperature, adding 100 parts of water, 10 parts of benzenesulfonic acid aqueous solution and 10 parts of polyvinyl alcohol aqueous solution, stirring for 30min, and standing for 12 days to obtain a transparent light yellow anti-sticking kettle coating agent product with the water-soluble phenolic resin of which the specific gravity is 5-6%.
Example 3
Adding 8 parts of 99% refined 1-naphthol, 50 parts of water and 15 parts of 32% sodium hydroxide solution into a reactor, starting stirring, and introducing nitrogen to replace air in the reactor; heating the reactor until the reaction temperature is stabilized at 100 ℃, slowly dropwise adding a mixed solution of 5 parts of sodium formaldehyde sulfoxylate and 10 parts of formaldehyde aqueous solution into the reactor for 1h to ensure that the interior of the reactor is in an alkaline environment and the pH value is 11-13; and (3) continuously reacting for 8 hours under the stirring condition, cooling to room temperature, adding 100 parts of water, 10 parts of benzenesulfonic acid aqueous solution, 10 parts of polyvinyl alcohol aqueous solution and 5 parts of sodium formaldehyde sulfoxylate, stirring for 20min, and standing for 13 days to obtain a transparent light yellow anti-sticking kettle coating agent product with the water-soluble phenolic resin of which the specific gravity is 5-6%.
Example 4
Adding 8 parts of 99% refined 1-naphthol, 50 parts of water and 20 parts of 32% sodium hydroxide solution into a reactor, starting stirring, and introducing nitrogen to replace air in the reactor; heating the reactor until the reaction temperature is stabilized at 90 ℃, slowly dropwise adding a mixed solution of 10 parts of sodium formaldehyde sulfoxylate and 10 parts of formaldehyde aqueous solution into the reactor for 3 hours to ensure that the interior of the reactor is in an alkaline environment and the pH value is 11-13; and (3) continuously reacting for 12h under the stirring condition, cooling to room temperature, adding 100 parts of water, 10 parts of benzenesulfonic acid aqueous solution and 10 parts of polyvinyl alcohol aqueous solution, stirring for 40min, and standing for 15 days to obtain a transparent light yellow anti-sticking kettle coating agent product with the water-soluble phenolic resin of which the specific gravity is 5-6%.
Example 5
Adding 7 parts of 99% refined 1-naphthol, 15 parts of water and 8 parts of 32% sodium hydroxide solution into a reactor, starting stirring, and introducing argon to replace air in the reactor; heating the reactor until the reaction temperature is stabilized at 97 ℃, slowly dropwise adding a mixed solution of 8 parts of sodium formaldehyde sulfoxylate and 4 parts of formaldehyde aqueous solution into the reactor for 2 hours to ensure that the interior of the reactor is in an alkaline environment and the pH value is 11-13; and (3) continuously reacting for 8 hours under the condition of stirring, cooling to room temperature, adding 30 parts of water, 8 parts of benzenesulfonic acid aqueous solution and 8 parts of polyvinyl alcohol aqueous solution, stirring for 30min, and standing for 12 days to obtain a transparent light yellow anti-sticking kettle coating agent product with the water-soluble phenolic resin of which the specific gravity is 5-6%.
Example 6
Adding 9 parts of 99% refined 1-naphthol, 60 parts of water and 22 parts of 32% sodium hydroxide solution into a reactor, starting stirring, and introducing argon to replace air in the reactor; heating the reactor until the reaction temperature is stabilized at 97 ℃, slowly dropwise adding a mixed solution of 12 parts of sodium formaldehyde sulfoxylate and 11 parts of formaldehyde aqueous solution into the reactor for 2 hours to ensure that the interior of the reactor is in an alkaline environment and the pH value is 11-13; and (3) continuously reacting for 8 hours under the condition of stirring, cooling to room temperature, adding 150 parts of water, 12 parts of benzenesulfonic acid aqueous solution and 12 parts of polyvinyl alcohol aqueous solution, stirring for 30min, and standing for 12 days to obtain a transparent light yellow anti-sticking kettle coating agent product with the water-soluble phenolic resin of which the specific gravity is 5-6%.
Comparative example 1
The difference from example 2 is that comparative example 1 was identical to example 1 except that no benzenesulfonic acid aqueous solution was added.
Comparative example 2
In contrast to example 2, sodium formaldehyde sulfoxylate was cooled to room temperature and then added together with water, an aqueous solution of benzenesulfonic acid, and an aqueous solution of polyvinyl alcohol, with the remainder being the same.
Comparative example 3
The difference from example 2 is that 15 parts of sodium formaldehyde sulfoxylate are used, and the rest is the same.
Comparative example 4
The difference from example 2 is that 5 parts of sodium formaldehyde sulfoxylate are used, and the rest is the same.
The pot release effect and the properties of the obtained resin were measured for examples and comparative examples.
Table 1.
| Resin type SG-5 | Coating amount | Amount of sticking to the kettle | Storage time | Whiteness of resin |
| Example 1 | 12Kg | 56g | 152 days | 83.76％ |
| Example 2 | 12Kg | 21g | 281 days | 84.32％ |
| Example 3 | 12Kg | 89g | 163 days | 80.70％ |
| Example 4 | 12Kg | 102g | 129 days | 78.64％ |
| Example 5 | 12Kg | 62g | 194 days | 81.35％ |
| Example 6 | 12Kg | 73g | 207 days | 81.16％ |
| Comparative example 1 | 12Kg | 1002g | 7 days | 76.21％ |
| Comparative example 2 | 12Kg | 287g | 188 days | 79.64％ |
| Comparative example 3 | 12Kg | 39g | 288 days | 75.32％ |
| Comparative example 4 | 12Kg | 26g | Day 116 | 82.87％ |
It can be seen that the anti-sticking kettle coating agent product of the embodiment of the application has the effects of kettle sticking prevention, long storage time and good resin appearance performance, and the comparative example 1 shows that when no benzenesulfonic acid is added, the kettle sticking amount is the highest, the storage time is the shortest and the resin whiteness is poor. Comparative example 2 shows that the timing of the addition of sodium formaldehyde sulfoxylate has a great influence on the final properties.
The present invention is not limited to the above-described preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The preparation method of the efficient anti-sticking kettle coating agent for polyvinyl chloride suspension polymerization is characterized in that the anti-sticking kettle coating agent comprises the following raw materials in parts by weight:
8-12 parts of sodium formaldehyde sulfoxylate
7-9 parts of 1-naphthol
4-11 parts of formaldehyde solution
8-22 parts of sodium hydroxide solution
45-210 parts of water
Polyvinyl alcohol solution 8-12 parts
8-12 parts of a benzenesulfonic acid solution;
the preparation method comprises the following steps:
(1) adding 1-naphthol, water and a sodium hydroxide solution into a reactor, starting stirring, and replacing air in the reactor;
(2) heating the reactor, mixing the formaldehyde solution with all or part of sodium formaldehyde sulfoxylate in the formula amount, then dropwise adding the mixture into the reactor, and stirring for reaction;
(3) cooling, adding water, a benzenesulfonic acid solution, a polyvinyl alcohol solution and the residual sodium formaldehyde sulfoxylate, adjusting the solid content, and stirring to obtain a light yellow phenolic resin aqueous solution product;
(4) and (4) standing the product obtained in the step (3) to obtain a light yellow clear anti-sticking coating agent product.
2. The preparation method of claim 1, wherein the raw materials of the anti-sticking kettle coating agent comprise the following components in parts by weight:
3. the method according to claim 1, wherein the step (1) of replacing the air in the reactor comprises replacing the air in the reactor with nitrogen or argon.
4. The method according to claim 1, wherein the heating temperature in the step (2) is 80 to 100 ℃.
5. The method according to claim 1, wherein in the step (2), an alkaline environment is maintained in the reactor.
6. The method according to claim 5, wherein in the step (2), the pH of the alkaline environment is 11 to 13.
7. The production method according to claim 1, wherein in the step (2), the dropping time is 1 to 3 hours.
8. The method according to claim 1, wherein in the step (2), the stirring reaction time is 4 to 12 hours.
9. The method according to claim 1, wherein in the step (3), the stirring time is 20 to 40 min.
10. The method according to claim 1, wherein the standing time in the step (4) is 10 to 15 days.
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