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The recovery method of ctp in the solvent after synthetic ctp is used

A recovery method and solvent technology, applied in the field of CTP recovery in solvent, can solve problems such as waste, increased environmental protection cost, CTP loss, etc.

Active Publication Date: 2022-05-10
TANGYIN YONGXIN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This will not only cause the loss and waste of CTP, increase the production cost, but also produce a large amount of heavy oil waste residue, which increases the cost of environmental protection treatment

Method used

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  • The recovery method of ctp in the solvent after synthetic ctp is used

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Pour 6000L of the solvent used in the synthesis of CTP into the distillation pot, raise the temperature to 80-90°C, turn on the vacuum, carry out vacuum distillation at a vacuum degree of 0.2-0.4MPa, and a liquid phase temperature of 80-90°C, and evaporate the solvent into the solvent receiver device, and then stored in metering tanks for easy return to CTP synthesis for recycling.

[0053] When the liquid phase temperature is 90°C and the vacuum degree is 0.4MPa, when no solvent evaporates, stop the vacuum distillation. Put the solvent mother liquor in a cooling crystallization kettle, add the solvent mother liquor after vacuum distillation to the aqueous solution of polyacrylamide compound (including polyacrylamide and sodium chloride with a mass ratio of 1:0.5) at 60°C (Mass concentration is 3%) 200L, after stirring at 20r / min for 10min, let it stand, and separate the water phase. After separating the oil phase from the water phase, the temperature was lowered to 20...

Embodiment 2

[0058] Pour 8000L of the solvent used in the synthesis of CTP into the distillation pot, raise the temperature to 70-90°C, turn on the vacuum, carry out vacuum distillation at a vacuum degree of 0.3-0.4MPa, and a liquid phase temperature of 70-90°C, and distill the solvent into the solvent receiver device, and then stored in metering tanks for easy return to CTP synthesis for recycling.

[0059] When the liquid phase temperature is 90°C and the vacuum degree is 0.4MPa, when no solvent evaporates, stop the vacuum distillation. Put the solvent mother liquor into the cooling crystallization kettle, add the solvent mother liquor after vacuum distillation to the aqueous solution of polyacrylamide compound (including polyacrylamide and sodium chloride with a mass ratio of 1:1) at 55°C (Mass concentration is 2%) 300L, after stirring at 25r / min for 15min, let it stand, and separate the water phase. After separating the oil phase from the water phase, the temperature was lowered to 15...

Embodiment 3

[0064] Pour 7000L of the solvent used in the synthesis of CTP into the distillation pot, raise the temperature to 60-80°C, turn on the vacuum, carry out vacuum distillation at a vacuum degree of 0.3-0.6MPa, and a liquid phase temperature of 60-80°C, and evaporate the solvent into the solvent receiver device, and then stored in metering tanks for easy return to CTP synthesis for recycling.

[0065] When the liquid phase temperature is 80°C and the vacuum degree is 0.6MPa, when no solvent evaporates, stop the vacuum distillation. Put the solvent mother liquor into a cooling crystallization kettle, add the solvent mother liquor after vacuum distillation to the aqueous solution of polyacrylamide compound (including polyacrylamide and sodium chloride with a mass ratio of 1:1.5) at 55°C (mass concentration is 3%) 400L, after stirring at 20r / min for 10min, let it stand, and separate the water phase. The oil phase after removing the water phase was stirred and cooled to 20°C at a sti...

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Abstract

The present invention relates to the technical field of rubber anti-scorch agent CTP production, in particular to the recovery method of CTP in the solvent after synthetic CTP is used, specifically comprises the following steps: A) the solvent after the synthetic CTP is used is vacuum degree is 0.2~0.6MPa, liquid Perform vacuum distillation at a phase temperature of 60-90°C; B) mix and stir the solvent mother liquor after vacuum distillation with the aqueous solution of the polyacrylamide compound at 50-60°C for 10-20min, after standing still, separate The water phase is removed, the temperature of the obtained oil phase is lowered to 10-20° C., and the CTP material is precipitated. The recovery method provided by the invention can obtain CTP with higher recovery rate and higher purity. The application results show that the recovery method provided by the invention can finally obtain a CTP recovery rate of not less than 92%, and a CTP purity greater than 98.3%.

Description

technical field [0001] The invention relates to the technical field of rubber anti-scorch agent CTP production, in particular to a method for recovering CTP in a solvent after synthetic CTP is used. Background technique [0002] Rubber anti-scorch agent CTP, chemical name N-cyclohexylthiophthalimide, was developed by Monsanto in the late 1960s and widely recognized by the rubber product industry in the early 1980s. This product can improve the scorch time of the rubber in the rubber containing sulfenamide accelerator, but has no effect on the vulcanization speed and the performance of the vulcanized rubber. The anti-scorch time of the rubber can be controlled by its dosage in a wide range. changes are adjusted. [0003] In the synthesis of CTP, industrial mineral spirits are mostly used as the carrier (or solvent) for the reaction. After the reaction is completed, the solvent needs to be distilled, purified, recovered and recycled. At present, the conventional process is a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/48
CPCC07D209/48
Inventor 宋魁璟李延辉张鑫浩张鑫淦
Owner TANGYIN YONGXIN CHEM CO LTD