Micro-reaction system and method for synthesizing rubber scorch retarder CTP

A technology of micro-reaction and anti-scorch agent, applied in chemical instruments and methods, chemical/physical/physical chemical reactors, chemical/physical/physical chemical fixed reactors, etc., can solve the instability of cyclohexylsulfenyl chloride, Problems such as low overall reaction yield

Active Publication Date: 2021-09-10
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI +1
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  • Abstract
  • Description
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Problems solved by technology

[0006] Based on the above background technology, aiming at the instability of cyclohexylsulfenyl chloride and the low overall reaction yield in the stirred tank chlorination process, the present invention proposes to synthesize cyclohexylsulfenyl chloride by using a microchannel gas-liquid continuous reaction process, and particularly provides a A kind of technology of microchannel chlorination and kettle condensation synthesis CTP

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  • Micro-reaction system and method for synthesizing rubber scorch retarder CTP

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Embodiment 1

[0032] Microreactor systems such as figure 1Shown, wherein, the effective volume of the internal microchannel of the chlorination microreactor 3 is 2.7 milliliters, the volume of the stirred tank reactor is 1 liter, and the anchor type stirring paddle is equipped. Dicyclohexyl disulfide is delivered by pump 1 with a volume flow rate of 3.4ml / min, and the mixed alkanes of solvent n-heptane and isoheptane are delivered by pump 2 with a volume flow rate of 36.6ml / min. (no heat exchange) mixed to form a dicyclohexyl disulfide solution (mass concentration of the dicyclohexyl disulfide reaction solution can be calculated to be 12%), enter the micro heat exchanger 2 and cool down to minus 10°C, enter the chlorine after cooling The microreactor 3 mixes with the chlorine gas of 330ml / min (standard condition), and the reaction temperature in the control microreactor 3 is subzero 20 ℃, and the reaction time (calculated in liquid disulfide solution) is 4 seconds, and the reaction generate...

Embodiment 2

[0034] 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. Dicyclohexyl disulfide is delivered by pump 1 with a volume flow rate of 8.6ml / min, and the mixed alkanes of solvent n-heptane and isoheptane are delivered by pump 2 with a volume flow rate of 31.4ml / min. (without heat exchange) mixed to form a dicyclohexyl disulfide solution (mass concentration of dicyclohexyl disulfide reaction solution can be calculated to be 28.5%), enter the micro heat exchanger 2 and cool down to minus 10°C, enter chlorine after cooling The microreactor 3 is mixed with the chlorine gas of 875ml / min (standard condition), and the reaction temperature in the control microreactor 3 is subzero 10 ℃, and the reaction time (in terms of liquid disulfide solution) is 4 seconds, and the reaction generates cyclohexyl...

Embodiment 3

[0036] Microreactor systems such as figure 1 Show, wherein, chlorination microreactor 3 internal microchannel effective volume is 0.3 milliliter (obtained by reducing channel number and number of layers), stirred tank reactor volume 1 liter, is equipped with stirring paddle. Dicyclohexyl disulfide is transported by pump 1 with a volume flow rate of 8.6ml / min. The mixed alkanes of n-heptane and n-octane as solvent are transported by pump 2 with a volume flow rate of 31.4ml / min. (without heat exchange) mixed to form a dicyclohexyl disulfide solution (mass concentration of dicyclohexyl disulfide reaction solution can be calculated to be 28.5%), enter the micro heat exchanger 2 and cool down to minus 5°C, enter chlorine after cooling The microreactor 3 is mixed with the chlorine gas of 875ml / min (standard condition), and the reaction temperature in the control microreactor 3 is 0 ℃, and the reaction time (in terms of liquid disulfide solution) is 0.45 seconds, and the reaction gen...

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Abstract

A micro-reaction system and method for the synthesis of rubber anti-scorch agent CTP, the system is composed of a micro-heat exchanger, a micro-reactor, and a stirred tank reactor in series; the synthesis method is: dicyclohexyl disulfide is mixed in a micro-heat exchanger Internal pre-cooling, followed by continuous reaction with chlorine in the microreactor to generate cyclohexylsulfenyl chloride; cyclohexylsulfenyl chloride continuously flows out of the microreactor into the stirred tank reactor, and is combined with the pre-added sodium phthalimide The salt is condensed to generate a reaction solution containing N-cyclohexylthiophthalimide (CTP), and the CTP product is obtained through water separation and purification. Wherein, the reaction temperature in the microreactor is -20-15°C, and the reaction time is 0.01 second to 1.5 minutes; the reaction temperature in the stirred tank reactor is -10-10°C, and the reaction time is 10 minutes-60 minutes. The reaction time of the chlorination step of the present invention is greatly shortened, and the total yield of the two-step reaction is higher than 93%, which is 3-4 percentage points higher than that of the existing production technology.

Description

technical field [0001] The invention belongs to the field of synthesizing auxiliary agents in the rubber industry, and in particular relates to a micro-reaction system and method for synthesizing 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 vulcaniza...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/00B01J19/18C07D209/48
CPCB01J19/0093B01J19/18C07D209/48
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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