CN111995701A - Preparation method of chlorinated polyethylene - Google Patents
Preparation method of chlorinated polyethylene Download PDFInfo
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- CN111995701A CN111995701A CN202010944116.6A CN202010944116A CN111995701A CN 111995701 A CN111995701 A CN 111995701A CN 202010944116 A CN202010944116 A CN 202010944116A CN 111995701 A CN111995701 A CN 111995701A
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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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Abstract
The invention discloses a preparation method of chlorinated polyethylene, which comprises the following steps: s01: inputting polyethylene, an auxiliary agent and chlorine into a reaction kettle for stirring and mixing for half an hour; s02: heating the reaction kettle to 80 ℃ for 90-300 minutes; s03: after the reaction is finished, reducing the temperature of the materials to 42 ℃, performing deacidification washing discharging by using a vacuum filter, recovering hydrochloric acid mother liquor after the separation from the materials is finished, recovering the hydrochloric acid mother liquor into a hydrochloric acid containing box, and adjusting the pH value of the deacidified and washed materials by using process water, wherein the pH value is controlled to be 6; s04: drying by using a centrifugal machine, conveying the treated material into a neutralization reaction kettle, and carrying out secondary adjustment on the pH value of the material by using liquid caustic soda; s05: conveying the material subjected to liquid caustic soda separation to a boiling dryer at 75 ℃ for drying to remove moisture; the invention avoids the cavitation erosion phenomenon of chlorine gas to the reaction kettle, prolongs the service life of the reaction kettle, and can recycle redundant hydrochloric acid for reutilization during centrifugal drying.
Description
Technical Field
The invention belongs to the technical field of polyethylene manufacturing processes, and particularly relates to a preparation method of chlorinated polyethylene.
Background
The polyethylene is a thermoplastic resin prepared by polymerizing ethylene, and the application is as follows: the polyethylene can be processed by injection molding, extrusion molding, blow molding and the like, and is mainly used as agricultural films, industrial packaging films, medicine and food packaging films, mechanical parts, daily necessities, building materials, electric wires, cable insulation, coatings, synthetic paper and the like, the polyethylene can be classified into a high-pressure method, a medium-pressure method and a low-pressure method according to polymerization pressure, the high-pressure method is used for producing low-density polyethylene, but the growth rate of the polyethylene is greatly lagged behind that of the low-pressure method along with the development of production technology and catalysts, the low-pressure method comprises a slurry method, a solution method and a gas-phase method as the implementation method, the slurry method is mainly used for producing high-density polyethylene, and the solution method and the gas-phase method can not only produce high-density polyethylene, but also produce medium-low-density polyethylene by adding a comonomer and are also called linear low-density polyethylene, and various low-pressure method processes are developed rapidly.
The existing polyethylene preparation process has certain disadvantages in the using process, the used hydrochloric acid cannot be recycled in the preparation process of polyethylene, and chlorine gas is directly introduced into the reaction kettle, so that the reaction kettle is greatly corroded after long-term use, the service life of the reaction kettle is shortened, and further improvement and reinforcement are needed.
Disclosure of Invention
The invention aims to provide a preparation method of chlorinated polyethylene, which mainly solves the following technical problems:
in the preparation process of polyethylene, the used hydrochloric acid can not be recycled, and chlorine is directly introduced into the reaction kettle, so that the reaction kettle is greatly corroded after long-term use, and the service life of the reaction kettle is shortened.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of chlorinated polyethylene comprises the following steps:
s01: inputting polyethylene, an auxiliary agent and chlorine into a reaction kettle for stirring and mixing for half an hour;
s02: heating the reaction kettle to 80 ℃ for 90-300 minutes;
s03: after the reaction is finished, reducing the temperature of the materials to 42 ℃, performing deacidification washing discharging by using a vacuum filter, recovering hydrochloric acid mother liquor after the separation from the materials is finished, recovering the hydrochloric acid mother liquor into a hydrochloric acid containing box, and adjusting the pH value of the deacidified and washed materials by using process water, wherein the pH value is controlled to be 6;
s04: drying by using a centrifugal machine, conveying the treated material into a neutralization reaction kettle, carrying out secondary adjustment on the pH value of the material by using liquid caustic soda, carrying out centrifugal drying again after the adjustment is finished, and refluxing the separated liquid caustic soda into a liquid caustic soda supply box;
s05: and (4) conveying the material subjected to liquid caustic soda separation to a boiling dryer at 75 ℃ for drying to remove moisture.
As a further scheme of the invention: and a chlorine barrel is arranged in the reaction kettle, the chlorine barrel is hermetically connected with a chlorine pipeline, and chlorine is input into the chlorine barrel through the chlorine pipeline.
As a further scheme of the invention: the weight of the polyethylene is 1-3 tons, the weight of the auxiliary agent is 4KG-9KG, the weight of the chlorine is 1-3 tons, and the auxiliary agent is hydrochloric acid with the concentration of 1-19.9.
The invention has the beneficial effects that:
adopt special logical chlorine mode, chlorine lets in to the chlorine gas bucket in the reation kettle and not with reation kettle's inner wall direct contact, has avoided chlorine to reation kettle's cavitation erosion phenomenon for reation kettle life-span improves, can retrieve unnecessary hydrochloric acid when centrifugal drying, conveniently carries out reuse to the hydrochloric acid of retrieving, and waste water discharge reduces, environmental protection more.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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 of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of chlorinated polyethylene comprises the following steps:
s01: inputting polyethylene, an auxiliary agent and chlorine into a reaction kettle for stirring and mixing for half an hour;
s02: heating the reaction kettle to 80 ℃ for 90 minutes;
s03: after the reaction is finished, reducing the temperature of the materials to 42 ℃, performing deacidification washing discharging by using a vacuum filter, recovering hydrochloric acid mother liquor after the separation from the materials is finished, recovering the hydrochloric acid mother liquor into a hydrochloric acid containing box, and adjusting the pH value of the deacidified and washed materials by using process water, wherein the pH value is controlled to be 6;
s04: drying by using a centrifugal machine, conveying the treated material into a neutralization reaction kettle, carrying out secondary adjustment on the pH value of the material by using liquid caustic soda, carrying out centrifugal drying again after the adjustment is finished, and refluxing the separated liquid caustic soda into a liquid caustic soda supply box;
s05: conveying the material subjected to liquid caustic soda separation to a boiling dryer at 75 ℃ for drying to remove moisture;
wherein, be provided with chlorine bucket in the reation kettle, chlorine bucket and chlorine pipeline sealing connection input chlorine by the chlorine pipeline in to the chlorine bucket for chlorine does not increase reation kettle's life with reation kettle inner wall direct contact, and the weight of polyethylene is 1 ton, and the auxiliary agent weight is 4KG, and the weight of chlorine is 1 ton, and the auxiliary agent is the hydrochloric acid of 1% concentration.
Example 2
A preparation method of chlorinated polyethylene comprises the following steps:
s01: inputting polyethylene, an auxiliary agent and chlorine into a reaction kettle for stirring and mixing for half an hour;
s02: heating the reaction kettle to 80 ℃ for 150 minutes;
s03: after the reaction is finished, reducing the temperature of the materials to 42 ℃, performing deacidification washing discharging by using a vacuum filter, recovering hydrochloric acid mother liquor after the separation from the materials is finished, recovering the hydrochloric acid mother liquor into a hydrochloric acid containing box, and adjusting the pH value of the deacidified and washed materials by using process water, wherein the pH value is controlled to be 6;
s04: drying by using a centrifugal machine, conveying the treated material into a neutralization reaction kettle, carrying out secondary adjustment on the pH value of the material by using liquid caustic soda, carrying out centrifugal drying again after the adjustment is finished, and refluxing the separated liquid caustic soda into a liquid caustic soda supply box;
s05: conveying the material subjected to liquid caustic soda separation to a boiling dryer at 75 ℃ for drying to remove moisture;
wherein, be provided with chlorine bucket in the reation kettle, chlorine bucket and chlorine pipeline sealing connection input chlorine by the chlorine pipeline in to the chlorine bucket for chlorine does not increase reation kettle's life with reation kettle inner wall direct contact, and the weight of polyethylene is 2 tons, and the auxiliary agent weight is 6KG, and the weight of chlorine is 2 tons, and the auxiliary agent is the hydrochloric acid of 10% concentration.
Example 3
A preparation method of chlorinated polyethylene comprises the following steps:
s01: inputting polyethylene, an auxiliary agent and chlorine into a reaction kettle for stirring and mixing for half an hour;
s02: heating the reaction kettle to 80 ℃ for 300 minutes;
s03: after the reaction is finished, reducing the temperature of the materials to 42 ℃, performing deacidification washing discharging by using a vacuum filter, recovering hydrochloric acid mother liquor after the separation from the materials is finished, recovering the hydrochloric acid mother liquor into a hydrochloric acid containing box, and adjusting the pH value of the deacidified and washed materials by using process water, wherein the pH value is controlled to be 6;
s04: drying by using a centrifugal machine, conveying the treated material into a neutralization reaction kettle, carrying out secondary adjustment on the pH value of the material by using liquid caustic soda, carrying out centrifugal drying again after the adjustment is finished, and refluxing the separated liquid caustic soda into a liquid caustic soda supply box;
s05: conveying the material subjected to liquid caustic soda separation to a boiling dryer at 75 ℃ for drying to remove moisture;
wherein, be provided with chlorine bucket in the reation kettle, chlorine bucket and chlorine pipeline sealing connection input chlorine by the chlorine pipeline in to the chlorine bucket for chlorine does not increase reation kettle's life with reation kettle inner wall direct contact, and the weight of polyethylene is 3 tons, and the auxiliary agent weight is 9KG, and the weight of chlorine is 3 tons, and the auxiliary agent is the hydrochloric acid of 19.9 concentration.
The working principle of the preparation method of the chlorinated polyethylene is as follows: inputting polyethylene, an auxiliary agent and chlorine into a reaction kettle for stirring and mixing, heating the inside of the reaction kettle to 80 ℃, reacting for 90 minutes, reducing the materials to 42 ℃ after the reaction is finished, deacidifying, washing and discharging materials by using a vacuum filter, recovering hydrochloric acid mother liquor after the separation from the materials is finished, recovering the hydrochloric acid mother liquor into a hydrochloric acid containing box, and conveniently utilizing the recovered hydrochloric acid, wherein a chlorine barrel is arranged in the reaction kettle, the chlorine barrel is hermetically connected with a chlorine pipeline, the chlorine is input into the chlorine barrel by the chlorine pipeline so as not to be directly contacted with the inner wall of the reaction kettle, the service life of the reaction kettle is prolonged, adjusting the pH value of the deacidified and washed materials by process water, controlling the pH value to be 6, drying by using a centrifugal machine, conveying the processed materials into a neutralization reaction kettle, secondarily adjusting the pH value of the materials by liquid alkali, and centrifugally drying again after the adjustment is finished, and (3) refluxing the separated liquid caustic soda into a liquid caustic soda supply box, conveying the material subjected to liquid caustic soda separation into a boiling dryer at 75 ℃ for drying to remove moisture, and discharging qualified materials.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely exemplary and illustrative of the present invention and various modifications, additions and substitutions may be made by those skilled in the art to the specific embodiments described without departing from the scope of the invention as defined in the following claims.
Claims (3)
1. A preparation method of chlorinated polyethylene is characterized by comprising the following steps:
s01: inputting polyethylene, an auxiliary agent and chlorine into a reaction kettle for stirring and mixing for half an hour;
s02: heating the reaction kettle to 80 ℃ for 90-300 minutes;
s03: after the reaction is finished, reducing the temperature of the materials to 42 ℃, performing deacidification washing discharging by using a vacuum filter, recovering hydrochloric acid mother liquor after the separation from the materials is finished, recovering the hydrochloric acid mother liquor into a hydrochloric acid containing box, and adjusting the pH value of the deacidified and washed materials by using process water, wherein the pH value is controlled to be 6;
s04: drying by using a centrifugal machine, conveying the treated material into a neutralization reaction kettle, carrying out secondary adjustment on the pH value of the material by using liquid caustic soda, carrying out centrifugal drying again after the adjustment is finished, and refluxing the separated liquid caustic soda into a liquid caustic soda supply box;
s05: and (4) conveying the material subjected to liquid caustic soda separation to a boiling dryer at 75 ℃ for drying to remove moisture.
2. The method for preparing chlorinated polyethylene according to claim 1, wherein a chlorine barrel is arranged in the reaction kettle, the chlorine barrel is hermetically connected with a chlorine pipeline, and chlorine is input into the chlorine barrel through the chlorine pipeline.
3. A process for preparing a chlorinated polyethylene according to claim 1, wherein the polyethylene is present in an amount of 1 to 3 tons, the auxiliary is present in an amount of 4KG to 9KG, the chlorine is present in an amount of 1 to 3 tons, and the auxiliary is hydrochloric acid having a concentration of 1 to 19.9. fig..
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| CN202010944116.6A CN111995701A (en) | 2020-09-09 | 2020-09-09 | Preparation method of chlorinated polyethylene |
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| CN202010944116.6A CN111995701A (en) | 2020-09-09 | 2020-09-09 | Preparation method of chlorinated polyethylene |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114591453A (en) * | 2022-01-26 | 2022-06-07 | 山东奥星新材料股份有限公司 | Clean production method of chlorinated polyethylene |
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| CN1125734A (en) * | 1994-12-28 | 1996-07-03 | 青岛昌泰祥工贸有限公司 | Preparation method of high chlorinated polyethylene |
| CN102827313A (en) * | 2012-09-20 | 2012-12-19 | 山东瑞丰高分子材料股份有限公司 | Method for coproducing acid-phase-process synthesized chlorinated polyethylene and glycerol-process synthesized epoxy chloropropane |
| CN102863568A (en) * | 2011-07-07 | 2013-01-09 | 广西田东锦华化学有限公司 | Method for preparing chlorinated polyethylene through aqueous phase suspension method |
| CN103497264A (en) * | 2013-09-29 | 2014-01-08 | 中国平煤神马能源化工集团有限责任公司 | Reaction system and method for intermittent production of chlorinated polyvinyl chloride |
| CN105175585A (en) * | 2015-10-14 | 2015-12-23 | 奉化市裕隆化工新材料有限公司 | Method for preparing chlorinated polyethylene in acid medium |
| CN106279472A (en) * | 2016-08-16 | 2017-01-04 | 芜湖融汇化工有限公司 | A kind of special chlorinated polyethylene of automobile-used oil-resisting rubber hose and production technology thereof |
| CN205874279U (en) * | 2016-05-30 | 2017-01-11 | 广西锦华新材料科技有限公司 | Chlorinated polyethylene production system |
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2020
- 2020-09-09 CN CN202010944116.6A patent/CN111995701A/en active Pending
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| CN102827313A (en) * | 2012-09-20 | 2012-12-19 | 山东瑞丰高分子材料股份有限公司 | Method for coproducing acid-phase-process synthesized chlorinated polyethylene and glycerol-process synthesized epoxy chloropropane |
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| CN106279472A (en) * | 2016-08-16 | 2017-01-04 | 芜湖融汇化工有限公司 | A kind of special chlorinated polyethylene of automobile-used oil-resisting rubber hose and production technology thereof |
| CN206544934U (en) * | 2017-02-28 | 2017-10-10 | 山东三义实业股份有限公司 | A kind of haloflex dealkalize water comprehensive reutilization system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114591453A (en) * | 2022-01-26 | 2022-06-07 | 山东奥星新材料股份有限公司 | Clean production method of chlorinated polyethylene |
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