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Micro-reaction system and method for synthesizing rubber anti-scorching agent CTP

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

Active Publication Date: 2020-01-14
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 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

Method used

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  • Micro-reaction system and method for synthesizing rubber anti-scorching agent 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

The invention relates to a micro-reaction system and a method for synthesizing rubber anti-scorching agent CTP. The system consists of a micro-heat exchanger, a micro-reactor and a stirring tank reactor in series. The synthesis method comprises the following steps of: pre-cooling dicyclohexyldisulfide in a micro heat exchanger, and then continuously reacting with chlorine gas in a micro reactor togenerate cyclohexyl sulfinyl chloride; cyclohexyl sulfinyl chloride continuously flowing out of the micro-reactor and entering the stirring tank reactor to be condensed with the sodium phthalimide salt added in advance to generate the reaction solution containing N-cyclohexylthiophthalimide (CTP), refining by water separation to obtain CTP product. Among them, the reaction temperature in the micro-reactor is -20-15 DEG C, and that reaction time is 0.01 second-1.5 minute; the reaction temperature in the stirring tank reactor is -10-10 DEG C, and that reaction time is 10-60 minutes. The reaction time of the chlorination step of the invention is greatly shortened, and the total yield of the two-step reaction is higher than 93%, which is 3-4% higher than the prior 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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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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