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A kind of method for preparing chlorosulfonated polyethylene

A technology of chlorosulfonated polyethylene and polyethylene, which is applied in the field of preparation of chlorosulfonated polyethylene, can solve the problems of destroying the crystallinity of polyethylene, and achieve the effects of avoiding negative environmental impact, reliable production process control, and stable quality

Active Publication Date: 2018-10-16
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0021] The disadvantage of the above patent application is that the chlorination step is carried out when the reaction does not meet the temperature and pressure requirements, and the crystallinity of polyethylene cannot be well destroyed, and polyethylene is precipitated when the sulfonylation reaction cools down.

Method used

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  • A kind of method for preparing chlorosulfonated polyethylene

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Such as figure 1 Shown, a kind of method for preparing chlorosulfonated polyethylene, its steps are as follows:

[0057] (a) Add 1 kg of polyethylene polymer with a water content of less than 0.5% and a mixture of 20 kg of chloroform and carbon tetrachloride into the reactor, the reaction temperature is 115 ° C ~ 120 ° C, the pressure is 0.25 MPa ~ 0.30 MPa, dissolve 1 After 1 hour, add 2.5g of initiator azobisisobutyronitrile, feed chlorine gas for 1 hour, pre-chlorination temperature is 105°C-110°C, pre-chlorination pressure is 0.25MPa-0.30MPa, and the reaction time is determined according to the requirements of the pre-chlorination degree. The test pre-chlorination degree is 18%, and the tail gas of the reaction is connected to the gas absorption device.

[0058] (b) Pump the chlorinated polyethylene with a pre-chlorination degree of 18% to the next reaction kettle, cool down to 75°C-80°C, heat the mixed gas to 30°C-40°C and feed it into the reaction kettle. 0.1L / h...

Embodiment 2

[0061] Such as figure 1 Shown, a kind of preparation method of preparing chlorosulfonated polyethylene, its steps are as follows:

[0062] (a) Add 1.2kg of polyethylene polymer with a water content of less than 1% and a mixture of 20kg of chloroform and carbon tetrachloride into the reactor at a reaction temperature of 120°C to 125°C and a pressure of 0.30MPa to 0.35MPa, and dissolve After 1 hour, add 2.2g of initiator azobisisobutyronitrile, feed chlorine gas for 50 minutes, pre-chlorination temperature is 105°C-110°C, pre-chlorination pressure is 0.25MPa-0.30MPa, and the reaction time is determined according to the requirements of pre-chlorination degree , the test pre-chlorination degree is 15%, and the tail gas of the reaction is connected to the gas absorption device.

[0063] (b) Pump the chlorinated polyethylene with a pre-chlorination degree of 15% to the next reaction kettle, cool down to 70°C-75°C, heat the mixed gas to 30°C-40°C and feed it into the reaction kettle...

Embodiment 3

[0066] Such as figure 1 Shown, a kind of method for preparing chlorosulfonated polyethylene, its steps are as follows:

[0067] (a) Add 1.5kg of polyethylene polymer with a water content of less than 1% and 20kg of a mixture of chloroform and carbon tetrachloride into the reactor, the reaction temperature is 110°C ~ 115°C, the pressure is 0.23MPa ~ 0.25MPa, dissolve After 2 hours, add 1.5g of initiator azobisisobutyronitrile, feed chlorine gas for 70 minutes, pre-chlorination temperature is 105°C-110°C, pre-chlorination pressure is 0.25MPa-0.30MPa, and the reaction time is determined according to the requirements of pre-chlorination degree , the test pre-chlorination degree is 20%, and the tail gas of the reaction is connected to the gas absorption device.

[0068] (b) Pump the chlorinated polyethylene with a pre-chlorination degree of 20% to the next reaction kettle, cool down to 70°C-75°C, heat the mixed gas to 30°C-40°C and feed it into the reaction kettle at a rate of 0....

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Abstract

The invention belongs to the field of organic synthesis technology, and provides a method for preparing chlorosulfonated polyethylene by a gas-solid-liquid three-phase reaction. The method comprises the following steps: (a) polyethylene whose content is less than 1% and a mixed solvent are added into a reactor; (b) after polyethylene is fully dissolved, an initiator azodiisobutyronitrile is added, and chlorine is introduced; (c) a prechlorinated substance is conveyed into a next reactor, and temperature of the prechlorinated substance is reduced; after the reaction is finished, contents of chlorine and sulfur are analyzed, when the contents are qualified, 1% of an epoxy resin stabilizing agent is added, nitrogen is introduced, anti-coagulating agent talcum powder is added, materials are discharged, and the chlorosulfonated polyethylene product is obtained. The production process is reliably controlled, the product performance is good, and quality is stable. Negative environmental influences caused by using carbon tetrachloride are avoided, and the product is environmentally friendly.

Description

technical field [0001] The invention belongs to the field of preparation of chlorosulfonated polyethylene, and relates to a method for preparing chlorosulfonated polyethylene, in particular to a method for preparing chlorosulfonated polyethylene by gas-solid-liquid reaction. Background technique [0002] Chlorosulfonated polyethylene is a special synthetic rubber obtained by chlorination and chlorosulfonylation of polyethylene. Due to the saturation of the structure and the presence of chlorosulfonyl groups, it has good crosslinkability, and the weather resistance, ozone resistance, oil resistance, chemical resistance, abrasion resistance, radiation resistance and flame retardancy of the vulcanized rubber Excellent performance and air tightness, good color stability, widely used in automotive rubber parts, flame retardant wires and cables, roof waterproofing, chemical equipment anti-corrosion lining, shoemaking and coatings. [0003] There are two production methods of chlo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F110/02C08F8/38C08F8/22
Inventor 邹向阳孙聚华东升魁王妍红
Owner PETROCHINA CO LTD
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