CN111704686B - Preparation method of high chlorinated polyethylene - Google Patents
Preparation method of high chlorinated polyethylene Download PDFInfo
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- CN111704686B CN111704686B CN202010717829.9A CN202010717829A CN111704686B CN 111704686 B CN111704686 B CN 111704686B CN 202010717829 A CN202010717829 A CN 202010717829A CN 111704686 B CN111704686 B CN 111704686B
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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
- 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
- C09D123/00—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers
- C09D123/26—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers modified by chemical after-treatment
- C09D123/28—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers modified by chemical after-treatment by reaction with halogens or compounds containing halogen
- C09D123/286—Chlorinated polyethylene
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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Abstract
The invention provides a preparation method of high chlorinated polyethylene, which comprises the steps of adding deionized water, low molecular weight polyethylene powder, an emulsifier and a dispersant into a reaction kettle for pre-dispersion and suspension, adding an initiator when a preset temperature is reached, then starting heating up and introducing chlorine, controlling the chlorine introducing speed and the heating up speed, and finally carrying out post-treatment to obtain the high chlorinated polyethylene.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to a preparation method of high chlorinated polyethylene.
Background
The high chlorinated polyethylene is a high molecular material for heavy corrosion prevention and replacing traditional solvent method chlorinated rubber on ship paint, and is obtained by chlorination reaction of low molecular weight polyethylene in water suspension medium, the product is white or yellowish particles, can be dissolved in solvents such as benzene, esters, chlorohydrocarbons and the like at normal temperature, has high chlorine content, high drying speed and excellent corrosion resistance, and can be applied to places such as steel structures, machinery, pipelines, bridges, ships and the like, and has corrosion resistance, rust prevention and salt mist resistance.
At present, the preparation method of high chlorinated polyethylene mainly comprises a solution method, a solid phase method and a water phase suspension method, the domestic process mainly adopts the water phase suspension method, and the method has been specially used for CN 1125734A, CN 1230550A, CN 1394887A, CN 1394884A, CN 101608001A, CN 101704911A and the like. The method is a water phase suspension method except CN 1125734A which is a gas-solid phase method, and the method described in CN 101704911A is applied to a high-viscosity and high-chlorinated polyethylene process for adhesives, and the main defects of other processes are as follows: 1. the initiator causes two types of high and low temperature to be matched for initiating reaction, so that the materials are easy to cohere in the kettle when the reaction is initiated when the reaction is converted to a certain temperature; 2. the multi-element multi-group reaction requires grafting treatment on the raw materials before the reaction, and the chlorine introducing amount and the chlorine introducing uniformity are difficult to realize; 3. the method is divided into three to four sections of multi-stage reaction, the process is difficult to control, and the automatic industrial production cannot be realized.
Disclosure of Invention
The invention mainly aims to provide a preparation method of high chlorinated polyethylene, which solves the problems that high reaction pressure is easy to form a kettle, chlorine is not uniformly introduced, a finished product is not transparent, chlorine introduction amount is not high, a finished product is easy to gel and the like due to the fact that the high chlorinated polyethylene resin produced by an aqueous phase method process in the market at present adopts various initiators for reaction or various groups are introduced into raw material polyethylene to accelerate chlorine introduction by using an auxiliary agent, and multi-stage chlorine introduction reaction is adopted.
The invention provides a preparation method of high chlorinated polyethylene, which comprises the following steps:
adding deionized water, low molecular weight polyethylene powder, an emulsifier and a dispersant into a reaction kettle for pre-dispersion suspension, adding an initiator when the preset temperature is reached, then starting heating up and introducing chlorine, wherein the chlorine introducing speed is 10-20kg/min, the heating up speed is 2-4 ℃/10min, the reaction pressure is controlled to be not more than 0.3Mpa, and the required chlorine introducing amount is more than 80% before the temperature reaches 90 ℃; when the pressure begins to rise to be higher than 0.35Mpa, slowing down the chlorine introducing speed to 2-10kg/min, and continuing introducing chlorine to 110-115 ℃ until the pressure is not higher than 0.4 Mpa; finally, the finished product is obtained through the working procedures of heat preservation, temperature reduction, deacidification, neutralization, water washing, dehydration and drying.
Preferably, the molecular weight of the low molecular weight polyethylene powder is 2000-3000, and the fineness is 60-80 meshes.
Preferably, the emulsifier is peregal O or alkylphenol ethoxylates, and the using amount of the emulsifier is 2-4% of the weight of the low molecular weight polyethylene powder.
Preferably, the dispersant is sodium polymethacrylate or polyvinylpyrrolidone, and the dosage of the dispersant is 1-3% of the mass of the low molecular weight polyethylene powder.
Preferably, the initiator is dibenzoyl peroxide, and the amount of the initiator is 1.5-2% of the mass of the low molecular weight polyethylene powder.
Preferably, the predetermined starting chlorine introduction temperature is 65 ℃.
Preferably, the required chlorine passing amount is 3.5 to 4.5 times of the mass of the low molecular weight polyethylene powder.
The processes of heat preservation, temperature reduction, deacidification, neutralization, water washing, dehydration and drying are well-known technologies and are not described in detail herein.
The invention takes low molecular weight polyethylene powder as raw material, selects single initiation chlorination system reaction, uniformly introduces strictly controlled chlorine introduction amount, and controls temperature rise speed to achieve uniform chlorination reaction of the raw material, chlorine content reaches more than 65%, and high performance high chlorinated polyethylene resin with uniform chlorination.
Advantageous effects
The high chlorinated polyethylene obtained by the invention has good solubility, high transparency, excellent anti-corrosion performance, high drying speed, strong salt mist resistance and low viscosity, and can completely replace chlorinated rubber for heavy corrosion prevention and marine paint; the method adopts a single initiator, has high chlorine flux, uniform chlorine flux, low reaction pressure, no kettle closure at key temperature, high finished product yield, improved product performance and 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.
In order to make those skilled in the art better understand the technical solutions of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, shall fall within the protection scope of the present invention.
It should be 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.
Example 1
3000 kg of deionized water, 200 kg of low molecular weight polyethylene powder, 7 kg of sodium polymethacrylate and 4 kg of alkylphenol ethoxylates are placed in an enamel reactor with the volume of 5000L for complete pre-dispersion, 3 kg of dibenzoyl peroxide is added, chlorine starts to be introduced after air is replaced by nitrogen when the temperature reaches 65 ℃, the chlorine introduction speed is controlled to be 10-20kg/min, the temperature rising speed is controlled to be 2-4 ℃/10min, the reaction pressure is controlled not to exceed 0.3Mpa, the chlorine introduction is reduced when the pressure is exceeded or the temperature rises too fast until about 88 ℃, the total chlorine introduction is not lower than 650 kg, when the pressure begins to rise to be higher than 0.35Mpa, the chlorine introduction speed is reduced to 2-10kg/min, the temperature does not exceed 0.4Mpa, the chlorine introduction is stopped when the temperature reaches 115 ℃, and then the chlorine introduction is stopped by the procedures of water washing, neutralization, centrifugation and drying, thus obtaining the finished product.
Example 2
3000 kg of deionized water, 200 kg of low molecular weight polyethylene powder, 7 kg of sodium polymethacrylate and 4 kg of alkylphenol ethoxylates are filled into an enamel reactor with the volume of 5000L, after the deionized water, the low molecular weight polyethylene powder, the sodium polymethacrylate and the alkylphenol ethoxylates are completely pre-dispersed, 3 kg of dibenzoyl peroxide is added, chlorine starts to be introduced after air is replaced by nitrogen when the temperature reaches 65 ℃, the chlorine introduction speed is controlled to be 10-20kg/min, the temperature rising speed is controlled to be 2-4 ℃/10min, the reaction pressure is controlled not to exceed 0.3Mpa, the chlorine introduction is reduced when the pressure is exceeded or the temperature rises too fast until about 88 ℃, the total chlorine introduction is not lower than 600 kg, when the pressure begins to rise to be higher than 0.35Mpa, the chlorine introduction speed is reduced to 2-10kg/min, the temperature rises without limitation, the pressure is not higher than 0.4Mpa, the chlorine introduction is stopped until the temperature reaches 750 kg of total chlorine introduction, and then the finished product is obtained after the temperature reduction, water washing, neutralization, centrifugation and drying.
Example 3
3000 kg of deionized water, 200 kg of low molecular weight polyethylene powder, 7 kg of sodium polymethacrylate and 4 kg of alkylphenol polyoxyethylene are filled in an enamel reactor with the volume of 5000L, after the deionized water, the low molecular weight polyethylene powder, the sodium polymethacrylate and the alkylphenol polyoxyethylene ether are completely pre-dispersed, 3 kg of dibenzoyl peroxide are added, chlorine starts to be introduced after the air is replaced by nitrogen when the temperature reaches 65 ℃, the chlorine introducing speed is controlled to be 10-20kg/min, the heating speed is controlled to be 2-10kg/min, the reaction pressure is controlled not to exceed 0.3Mpa, the chlorine introducing amount is reduced when the pressure is exceeded or the temperature is increased too fast until about 88 ℃, the total chlorine introducing amount is not less than 550 kg, when the temperature reaches 92 ℃, the pressure starts to be increased to be more than 0.38Mpa, the chlorine introducing speed is reduced to 2-10kg/min, the temperature is not limited, the pressure is not higher than 0.4Mpa, the chlorine introducing is stopped until the total chlorine introducing amount reaches 780 kg when the temperature reaches 115 ℃, and then the finished product is obtained by water washing, neutralizing, centrifuging and drying.
Example 4
3000 kg of deionized water, 200 kg of low molecular weight polyethylene powder, 7 kg of sodium polymethacrylate and 4 kg of alkylphenol ethoxylates are placed in an enamel reactor with the volume of 5000L for complete pre-dispersion, 3 kg of dibenzoyl peroxide is added, chlorine starts to be introduced after air is replaced by nitrogen when the temperature reaches 65 ℃, the chlorine introduction speed is controlled to be 10-20kg/min, the temperature rising speed is controlled to be 2-10kg/min, the reaction pressure is controlled to be not more than 0.3Mpa, the chlorine introduction is reduced when the pressure is exceeded or the temperature rises too fast until about 88 ℃, the total chlorine introduction is not less than 680 kg, when the pressure begins to rise to be more than 0.35Mpa, the chlorine introduction speed is reduced to be 2-10kg/min, the temperature does not exceed the limit, the pressure is not higher than 0.4Mpa, the chlorine introduction is stopped when the temperature reaches 115 ℃, the total chlorine introduction is 900 kg, and then the finished product is obtained by water washing, neutralization, centrifugation and drying.
Comparative example 1
High and low temperature initiation and staged reaction are adopted to prepare the high chlorinated polyethylene under the condition of the same raw materials.
3000 kilograms of deionized water, 200 kilograms of low molecular weight polyethylene powder, 7 kilograms of sodium polymethacrylate and 4 kilograms of alkylphenol ethoxylates are filled in an enamel reactor with the volume of 5000L, after the pre-dispersion is completed, 0.8 kilogram of lauroyl peroxide and 1.5 kilograms of dibenzoyl peroxide are introduced, the chlorine is introduced in four sections, the chlorine is introduced in the first section after the air is replaced by nitrogen when the temperature reaches 55 ℃, the chlorine introduction amount is about 150 kilograms, and the pressure in the first section is 0.2MPa; in the second stage, when the temperature is raised to 75 ℃, about 250 kilograms of chlorine gas is introduced, and the pressure in the second stage is 0.3Mpa; the third stage is that when the temperature is raised to 90 ℃, 300 kg of chlorine is introduced, and the pressure of the third stage is 0.4MPa or above; and the fourth stage is that the chlorine introduction is finished when the temperature is raised to 105 ℃ to 115 ℃, the total chlorine introduction amount is 820 kilograms, the chlorine introduction is stopped, and then the temperature is reduced, and the finished product is obtained after the procedures of water washing, neutralization, centrifugation and drying.
The result of the detection
| Detecting items | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 |
| Appearance of the product | White or yellowish particles | White near-powder particles | Yellowish bulky granule | Yellowish particles | Yellowish particles |
| Fineness/mesh number | 40 | 60 | 20 | 40 | 40 |
| Content of chlorine/%) | 65％ | 64％ | 64％ | 68％ | 64％ |
| Solubility (20% in toluene) | Transparent, non-insoluble particles | White, slightly transparent and insoluble particle-free | Yellow, slightly transparent and insoluble particle-free | Transparent and insoluble particle-free | Opaque with insoluble particles |
| viscosity/T4. S | 13 | 13.5 | 13 | 12 | 13 |
| Moisture content | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
| Hydrochloric acid residue% | 0.001 | 0.05 | 0.1 | 0.002 | 0.1 |
Compared with the existing high-low temperature staged initiation aqueous phase method process, the detection result shows that the solubility of the product obtained by the method is remarkably improved, and the application of the heavy-duty anticorrosive paint is more facilitated due to low residual quantity of hydrochloric acid. The production process of the embodiment 1 and the embodiment 4 has low reaction pressure, continuous chlorine introducing speed and sufficient chlorine introducing amount, the later-stage flux of chlorine introducing of the embodiment 2 is not enough to influence the performance of the product, and the early-stage insufficient chlorine introducing of the embodiment 3 increases the reaction pressure when the temperature reaches about 90 ℃, so that a agglomeration kettle is easily generated. In the comparative example 1, two initiators of high and low temperature are selected, the chlorine introducing temperature is lower, the chlorine is introduced in sections to obtain the composite reaction of the initiators, the pressure is obviously increased in the third section, the reaction in the kettle is violent, and the production operation difficulty is increased.
Chlorinated rubber performance indexes are as follows:
as can be seen from the performance indexes of the chlorinated rubber, the performance indexes of the high chlorinated polyethylene obtained by the method are very close to those of chlorinated rubber by a water phase method and a solvent method.
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 (4)
1. A preparation method of high chlorinated polyethylene is characterized by comprising the following steps:
3000 kg of deionized water, 200 kg of low molecular weight polyethylene powder, 7 kg of sodium polymethacrylate and 4 kg of alkylphenol ethoxylates are filled in an enamel reactor with the volume of 5000L, after the deionized water, the low molecular weight polyethylene powder, the sodium polymethacrylate and the alkylphenol ethoxylates are completely pre-dispersed, 3 kg of dibenzoyl peroxide is added, chlorine starts to be introduced after air is replaced by nitrogen at the temperature of 65 ℃, the chlorine introduction speed is controlled to be 10-20kg/min, the temperature rising speed is controlled to be 2-4 ℃/10min, the reaction pressure is controlled not to exceed 0.3Mpa, the chlorine introduction is reduced when the pressure is exceeded or the temperature rises too fast until 88 ℃, the total chlorine introduction is not lower than 650 kg, the chlorine introduction speed is reduced to 2-10kg/min when the pressure starts to rise to be higher than 0.35Mpa, the temperature is not limited while the pressure is not higher than 0.4Mpa, the chlorine introduction is stopped until the total chlorine introduction is 820 kg of 115 ℃, and then the finished product is obtained after the temperature is reduced and washed, neutralized, centrifuged and dried.
2. A preparation method of high chlorinated polyethylene is characterized by comprising the following steps:
3000 kg of deionized water, 200 kg of low molecular weight polyethylene powder, 7 kg of sodium polymethacrylate and 4 kg of alkylphenol ethoxylates are filled into an enamel reactor with the volume of 5000L, after the deionized water, the low molecular weight polyethylene powder, the sodium polymethacrylate and the alkylphenol ethoxylates are completely pre-dispersed, 3 kg of dibenzoyl peroxide is added, chlorine starts to be introduced after air is replaced by nitrogen at the temperature of 65 ℃, the chlorine introduction speed is controlled to be 10-20kg/min, the temperature rising speed is controlled to be 2-4 ℃/10min, the reaction pressure is controlled not to exceed 0.3Mpa, the chlorine introduction is reduced when the pressure is exceeded or the temperature rises too fast until 88 ℃, the total chlorine introduction is not lower than 600 kg, the chlorine introduction is reduced when the pressure starts to rise to be higher than 0.35Mpa, the chlorine introduction speed is reduced to 2-10kg/min, the temperature is not limited, the pressure is not higher than 0.4Mpa, the chlorine introduction is stopped until the temperature reaches 750 kg of the total chlorine introduction, and then the finished product is obtained after the temperature is reduced and washed, neutralized, centrifuged and dried.
3. A preparation method of high chlorinated polyethylene is characterized by comprising the following steps:
3000 kg of deionized water, 200 kg of low molecular weight polyethylene powder, 7 kg of sodium polymethacrylate and 4 kg of alkylphenol polyoxyethylene are filled in an enamel reactor with the volume of 5000L, after the deionized water, the low molecular weight polyethylene powder, the sodium polymethacrylate and the alkylphenol polyoxyethylene ether are completely pre-dispersed, 3 kg of dibenzoyl peroxide are added, chlorine starts to be introduced after air is replaced by nitrogen when the temperature reaches 65 ℃, the chlorine introducing speed is controlled to be 10-20kg/min, the heating speed is controlled to be 2-10kg/min, the reaction pressure is controlled not to exceed 0.3Mpa, the chlorine introducing amount is reduced when the pressure exceeds the pressure or the temperature rises too fast until 88 ℃, the total chlorine introducing amount is not less than 550 kg, when the temperature reaches 92 ℃, the pressure starts to rise to be more than 0.38Mpa, the chlorine introducing speed is reduced to 2-10kg/min, the temperature does not rise to be limited and the pressure is not higher than 0.4Mpa, the chlorine introducing is stopped until the temperature reaches 780 kg of the total chlorine introducing amount, and then the finished product is obtained by the procedures of water washing, neutralization, centrifugation and drying.
4. A preparation method of high chlorinated polyethylene is characterized by comprising the following steps:
3000 kg of deionized water, 200 kg of low molecular weight polyethylene powder, 7 kg of sodium polymethacrylate and 4 kg of alkylphenol ethoxylates are placed in an enamel reactor with the volume of 5000L for complete pre-dispersion, 3 kg of dibenzoyl peroxide is added, chlorine starts to be introduced after air is replaced by nitrogen when the temperature reaches 65 ℃, the chlorine introduction speed is controlled to be 10-20kg/min, the temperature rising speed is controlled to be 2-10kg/min, the reaction pressure is controlled to be not more than 0.3MPa, the chlorine introduction is reduced when the pressure is exceeded or the temperature rises too fast until 88 ℃, the total chlorine introduction is not less than 680 kg, the chlorine introduction is reduced when the pressure starts to rise to be more than 0.35MPa, the chlorine introduction speed is reduced to be 2-10kg/min, the temperature is not limited while the pressure is not higher than 0.4MPa, the chlorine introduction is stopped when the temperature reaches 115 ℃, and then the chlorine introduction is reduced by water washing, neutralization, centrifugation and drying, thus obtaining the finished product.
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| CN101704911B (en) * | 2009-11-14 | 2012-05-23 | 潍坊高信化工科技有限公司 | Method for producing highly-chlorinated polyethylene |
| CN104650473A (en) * | 2013-11-25 | 2015-05-27 | 江苏中煦高分子材料有限公司 | Chlorinated polyethylene rubber produced by water phase suspension method and synthesis technology thereof |
| CN107118290B (en) * | 2017-06-09 | 2019-02-22 | 江苏科利新材料有限公司 | A kind of method that environment-friendly type water phase method prepares haloflex |
| KR102252430B1 (en) * | 2018-12-10 | 2021-05-14 | 주식회사 엘지화학 | Polyethylene and its chlorinated polyethylene |
| CN110105479B (en) * | 2019-06-06 | 2021-10-08 | 金辉 | Low-consumption environment-friendly preparation method of chlorinated polyvinyl chloride by aqueous phase suspension method |
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