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System and method for synthesizing rubber scorch retarder CTP through continuous flow micro-reaction

一种合成橡胶、防焦剂的技术，应用在化学仪器和方法、化学/物理/物理化学反应器、化学/物理/物理化学过程等方向，能够解决副反应多、反应时间长、传质效率差等问题

Pending Publication Date: 2021-10-01
TANGYIN YONGXIN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the synthesis process of the batch reaction of CTP, because the reaction raw materials are easy to decompose and the two phases are not easy to be fully mixed evenly during the reaction, the mass transfer efficiency of this heterogeneous reaction will be poor, the reaction time will be long, the side reactions will be many, and the yield will be low. and the purity is not high

Method used

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  • System and method for synthesizing rubber scorch retarder CTP through continuous flow micro-reaction
  • System and method for synthesizing rubber scorch retarder CTP through continuous flow micro-reaction
  • System and method for synthesizing rubber scorch retarder CTP through continuous flow micro-reaction

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Continuous flow micro-reaction synthetic rubber anti-scorch agent CTP system

[0064] This embodiment provides a Figure 5 The shown continuous flow micro-reaction synthetic rubber anti-scorch agent CTP system includes: cyclohexyl sulfenyl chloride and catalyst mixed solution delivery pipeline 1, phthalimide sodium salt and catalyst mixed solution delivery pipeline 2, micro-reaction device 11, acidity Meter 12 and post-processing device 13.

[0065] In this embodiment, the cyclohexylsulfenyl chloride and catalyst mixed liquid delivery pipeline 1 is sequentially provided with a first filter 3, a first advection metering pump 5, a first mass flow meter 7 and a first pressure gauge9.

[0066] In this embodiment, the phthalimide sodium salt and the catalyst mixed liquid delivery pipeline 2 are sequentially provided with a second filter 4, a second advection metering pump 6, a second mass flow meter 8 and a second flow meter along the mixed liquid delivery direction. Two ...

Embodiment 2

[0075] Method for synthesizing rubber anti-scorch agent CTP by continuous flow micro-reaction

[0076] Carry out the synthesis of rubber anti-scorch agent CTP in the system that embodiment 1 provides, wherein, the micro-reaction device in the described system selects Y-type feed inlet microchannel reactor, and concrete synthetic process is as follows:

[0077]Mix the catalyst (benzyltriethylammonium chloride) evenly into the prepared cyclohexylsulfenyl chloride solution with a concentration of 12 to 25 wt% and a temperature of -5 to 15°C. The amount of the catalyst is cyclohexyl 5‰ of the mass of the sulfenyl chloride solution; the prepared sodium phthalimide solution with a concentration of 15-30 wt% is stored in an environment of -3-10°C.

[0078] Start the first and second advection metering pumps simultaneously afterwards, and the mixed solution of cyclohexylsulfenyl chloride and catalyst (referred to as reaction solution A) and phthalimide sodium salt solution (referred t...

Embodiment 3

[0082] Method for synthesizing rubber anti-scorch agent CTP by continuous flow micro-reaction

[0083] Carry out the synthesis of rubber anti-scorch agent CTP in the system that embodiment 1 provides, wherein, the micro-reaction device in the described system selects to have multi-stage stator-rotor high-shear reactor, and concrete synthetic process is as follows:

[0084] Mix the catalyst (benzyltriethylammonium chloride) evenly into the sodium phthalimide salt solution with a concentration of 15-30wt% and a temperature of -3-10°C. The amount of catalyst used is sodium phthalimide 5‰ of the quality of the salt solution; the prepared cyclohexylsulfenyl chloride solution with a concentration of 12-25 wt% is stored in an environment of -5-15°C.

[0085] Start the first and second advection metering pumps simultaneously afterwards, and the mixed solution of cyclohexylsulfenyl chloride solution (referred to as reaction solution A) and phthalimide sodium salt and catalyst (referred...

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Abstract

The invention belongs to the technical field of fine chemical engineering, and particularly relates to a system and a method for synthesizing a rubber scorch retarder CTP through continuous flow micro-reaction. The provided system comprises: a cyclohexylsulfenyl chloride and catalyst mixed liquid conveying pipeline; a phthalimide sodium salt and catalyst mixed liquid conveying pipeline; and a micro-reaction device, which is respectively connected with a discharge hole of the cyclohexylsulfenyl chloride and catalyst mixed liquid conveying pipeline and a discharge hole of the phthalimide sodium salt and catalyst mixed liquid conveying pipeline, wherein the micro-reaction device is a micro-channel reactor. According to the provided system, the rubber scorch retarder CTP is synthesized by virtue of full contact reaction of liquid and liquid two-phase flows in the micro-reaction device, so that the continuous reaction of CTP synthesis is realized, the production efficiency and reaction yield of CTP synthesis are greatly improved, the purity and quality stability of the product are improved, the system has a relatively good application prospect, and considerable economic benefits and social benefits can be generated.

Description

[0001] This application is a divisional application with an application date of March 18, 2019, an application number of 201910203186.3, and an invention titled "a system and method for continuous flow micro-reaction synthetic rubber anti-scorch agent CTP". technical field [0002] The invention belongs to the technical field of fine chemicals, and in particular relates to a system and method for continuous flow micro-reaction synthetic rubber anti-scorch agent CTP. Background technique [0003] The chemical name of rubber anti-scorch agent CTP (PVI) is N-cyclohexylthiophthalimide, CAS: 17796-82-6, molecular formula: C 14 h 15 o 2 SN, molecular weight: 261.3, physical and chemical properties: white or light yellow crystal, easily soluble in benzene, ether, acetone and ethyl acetate, soluble in warm n-heptane and carbon tetrachloride. Slightly soluble in gasoline, insoluble in kerosene and water. It is an additive that can effectively prevent rubber from scorching during p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/00C07D209/48
CPCB01J19/0093C07D209/48B01J2219/00867B01J2219/00889B01J2219/00876
Inventor 张迎宾宋魁璟尧红梅张鑫浩
Owner TANGYIN YONGXIN CHEM CO LTD
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