Micro-reaction system and method for continuous synthesis of rubber anti-scorch agent CTP

A scorch inhibitor, micro-reaction technology, applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, chemical/physical/physical-chemical stationary reactors, etc., can solve the problem of low total reaction yield, imine The problem of high concentration can achieve the effect of remarkable technology, reducing imine residue and high utilization rate

Active Publication Date: 2021-07-23
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Based on the above background technology, aiming at the problems of unstable cyclohexylsulfenyl chloride, high imine concentration in the product and low overall reaction yield under the stirred tank chlorination&condensation process, the present invention proposes to synthesize cyclohexyl sulfenyl chloride by microchannel gas-liquid continuous reaction process. Hexylsulfenyl chloride, and the intermediate product is continuously condensed with imine solution in a microchannel reactor to synthesize CTP

Method used

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  • Micro-reaction system and method for continuous synthesis of rubber anti-scorch agent CTP
  • Micro-reaction system and method for continuous synthesis of rubber anti-scorch agent CTP

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Embodiment 1

[0035] Microreactor systems such as figure 1 Shown, wherein, the effective volume of the internal microchannel of the chlorination microreactor 3 is 2.7 milliliters, and the volume of the stirred tank reactor is 1 liter, equipped with stirring paddles. Pre-prepared dicyclohexyl disulfide solution, the solvent is n-heptane and isoheptane mixed alkanes, wherein the mass concentration of dicyclohexyl disulfide is 11.9%, delivered by a metering pump, the volume flow rate is 40.0ml / min, enter Micro-heat exchanger 2 is cooled to subzero 5 ℃, enters chlorination micro-reactor 3 after cooling and mixes with the chlorine gas of 330ml / min (standard condition), and control reaction temperature in micro-reactor 3 is subzero 15 ℃, and reaction time (in liquid Disulfide solution meter) is 4 seconds, and reaction generates cyclohexyl sulfenyl chloride, and cyclohexyl sulfenyl chloride enters in the condensation microreactor 5, and enters the phthalimide sodium salt solution of this microreac...

Embodiment 2

[0037] Microreactor systems such as figure 1 Show, wherein, chlorination microreactor 3 internal microchannel effective volume is 0.3 milliliters (obtained by reducing channel number and number of layers), stirred tank reactor volume 2 liters, is equipped with stirring paddle. Pre-prepared dicyclohexyl disulfide solution, the solvent is n-heptane and isoheptane mixed alkanes, wherein the mass concentration of dicyclohexyl disulfide is 30%, transported by a metering pump, the volume flow rate is 50.0ml / min, enter Micro heat exchanger 2 is cooled to subzero 5 ℃, enters chlorination microreactor 3 after cooling and mixes with the chlorine gas of 1.16L / min (standard condition), controls the reaction temperature in microreactor 3 to be-5 ℃, and reaction time (with Liquid disulfide solution) is 0.36 seconds, and the reaction generates cyclohexylsulfenyl chloride, and cyclohexylsulfenyl chloride enters in the condensation microreactor 5, and enters the phthalimide sodium salt solutio...

Embodiment 3

[0039] Microreactor systems such as figure 1 Shown, wherein, the effective volume of the internal microchannel of the chlorination microreactor 3 is 2.7 milliliters, and the volume of the stirred tank reactor is 10 liters, equipped with stirring paddles. Dicyclohexyl disulfide is delivered by pump 1 with a volume flow rate of 46ml / min. The mixed alkanes of solvent n-heptane and isoheptane are delivered by pump 2 with a volume flow rate of 67.1ml / min. No heat exchange) mixed to form a dicyclohexyl disulfide solution (the mass concentration of the dicyclohexyl disulfide reaction solution can be calculated to be 50%), enter the micro heat exchanger 2 and cool down to minus 5°C, and enter the chlorination after cooling The microreactor 3 is mixed with chlorine gas of 4.7L / min (standard condition), and the reaction temperature in the microreactor 3 is controlled to be minus 5°C, and the reaction time (in terms of liquid disulfide solution) is 1.4 seconds, and the reaction generates...

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Abstract

A micro-reaction system and method for continuous synthesis of rubber anti-scorch agent CTP, the system is composed of a micro-heat exchanger, a chlorination micro-reactor, a condensation micro-reactor, and a stirred tank reactor in series; the synthesis method is: dicyclohexyl The disulfide is pre-cooled in the micro heat exchanger, and then continuously reacts with chlorine gas in the chlorination microreactor to generate cyclohexylsulfenyl chloride; cyclohexylsulfenyl chloride continuously flows out of the chlorination microreactor and enters the condensation microreactor, Condensate with the pre-prepared phthalimide salt to generate a reaction solution containing N-cyclohexylthiophthalimide (CTP), which enters the stirred tank reactor for precipitation or continues to stir and agglomerate The CTP slurry is obtained, and the CTP product is obtained through water separation and refining. The invention realizes the continuous synthesis of CTP products widely used in the rubber additive industry; the condensation reaction time in the microchannel reactor is on the millisecond level, and the sinking / stirring time in the stirred tank reactor is shortened to 10-20 minutes, and the two-step reaction The total yield is as high as 96.6%.

Description

technical field [0001] The invention belongs to the field of auxiliary agent synthesis in the rubber industry, and in particular relates to a micro-reaction system and method for continuous synthesis of rubber anti-scorch agent CTP. Background technique [0002] Rubber anti-scorch agent CTP is an indispensable additive to prevent scorch behavior in the rubber industry. Raw rubber needs to go through a series of processes such as mastication, mixing, calendering, and vulcanization to become rubber products. In the processing process before vulcanization, due to the heat and high temperature generated during mechanical work, the rubber often undergoes early vulcanization (called coke). burning), making it difficult for the rubber compound to continue to vulcanize and cross-link. The combination of the anti-scorch agent CTP can realize the sealed mixing of the rubber in rubber production, prolong the scorch time, and at the same time not hinder the normal performance of the vu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/00B01J19/18C07D209/48
CPCB01J19/0093B01J19/18B01J2219/00013B01J2219/0086B01J2219/00873C07D209/48
Inventor 陈光文焦凤军杜孟成许思俊宋彦哲韩梅尧超群
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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