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Equipment and method for recycling dimethyl-4-pentenoic acid methyl ester rectification residual liquid

A technology of methyl bentitate and recovery equipment, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of reaction between ester groups and hydroxyl groups. The recovery process is simple and the effect of reducing the cost of recycling

Pending Publication Date: 2021-03-12
安徽鑫泰新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The whole process is complicated, there are many equipments, and a large amount of waste water will be produced in the process of saponification and acidification, which increases the recycling cost

Method used

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  • Equipment and method for recycling dimethyl-4-pentenoic acid methyl ester rectification residual liquid
  • Equipment and method for recycling dimethyl-4-pentenoic acid methyl ester rectification residual liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Utilize above-mentioned recovery equipment to reclaim the method for the rectification raffinate of methyl perineate, comprise the following steps:

[0033] 1) 1560kg (containing 10kmol) of isopentenyl pyreneate remaining in the condensation reactor 1, 320kg (10kmol) of anhydrous methanol, and 5.4kg (0.1kmol) of sodium methylate are put into the transesterification reactor In 3, the material in the transesterification reactor 3 was stirred at normal temperature and pressure for 20min;

[0034] 2) The steam jacket 32 ​​is heated up to 70° C., and the product after the material reaction in the transesterification reactor 3 is condensed through the packed tower 41 and the condenser 42 successively, enters the receiving tank 51 and returns to the packed tower 41 again, and refluxes After reacting for 10 hours, the front fraction enters the receiving tank 51 after being condensed by the packed tower 41 and the condenser 42, and then is introduced into the methanol recovery t...

Embodiment 2

[0038] Utilize above-mentioned recovery equipment to reclaim the method for the rectification raffinate of methyl perineate, comprise the following steps:

[0039] 1) 780kg (containing 5kmol) of isopentenyl pyreneate remaining in the condensation reactor 1, 1600kg (50mol) of anhydrous methanol, and 54kg (1kmol) of sodium methylate are put into the transesterification reactor 3 , the material in the transesterification reactor 3 was stirred at normal temperature and pressure for 30min;

[0040] 2) The steam jacket 32 ​​is heated up to 73° C., and the product after the material reaction in the transesterification reactor 3 is condensed through the packed tower 41 and the condenser 42 successively, enters the receiving tank 51 and returns to the packed tower 41 again, and refluxes After reacting for 11 hours, the front fraction enters the receiving tank 51 after being condensed by the packed tower 41 and the condenser 42, and then is introduced into the methanol recovery tank 6 t...

Embodiment 3

[0044] Utilize above-mentioned recovery equipment to reclaim the method for the rectification raffinate of methyl perineate, comprise the following steps:

[0045] 1) 78kg (containing 0.5kmol) of isopentenyl pyritinate remaining in the condensation reactor 1, 1600kg (50kmol) of anhydrous methanol, and 297kg (5.5kmol) of sodium methylate are put into the transesterification reactor In 3, the material in the transesterification reactor 3 was stirred at normal temperature and pressure for 40min;

[0046] 2) The steam jacket 32 ​​is heated up to 75° C., and the product after the material reaction in the transesterification reactor 3 is condensed through the packed tower 41 and the condenser 42 successively, enters the receiving tank 51 and returns to the packed tower 41 again, and refluxes After reacting for 12 hours, the front fraction enters the receiving tank 51 after being condensed by the packed tower 41 and the condenser 42, and then is introduced into the methanol recovery ...

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Abstract

The invention relates to equipment and a method for recycling dimethyl-4-pentenoic acid methyl ester rectification residual liquid, and belongs to the technical field of 3,3-dimethyl-4-pentenoic acidmethyl ester synthesis. A condensation reaction kettle and a metering tank in the recovery equipment are connected with an inlet of an ester exchange reaction kettle through pipelines, and an outlet of the ester exchange reaction kettle is connected with an inlet of a vacuum degree adjusting tank through a condensing device; an outlet of the vacuum degree adjusting tank is connected with three branch pipes, the three branch pipes are respectively connected with the condensing device, the methanol recovery tank and the crude product tank, and an outlet of the crude product tank is connected with a feeding hole of the condensation reaction kettle and the rectification kettle. The method has the beneficial effects that the 3, 3-dimethyl-4-pentenoic acid methyl ester rectification residual liquid 3, 3-dimethyl-4-pentenoic acid isopentene ester is subjected to ester exchange reaction with methanol and sodium methoxide; by adjusting the temperature of the transesterification reaction, the vacuum degree after condensation and the reaction time, methanol, isopentenol anddimethyl-4-pentenoic acid methyl ester with high mass fraction can be collected, the recycling process is simple, and therecycling cost is reduced.

Description

technical field [0001] The invention relates to the technical field of synthesis of trimethyl-pyridinate, in particular to a recovery device and method for the rectification raffinate of methyl-pyridinate. Background technique [0002] At present, trimethyl pyribinate is condensed by isopentenol and trimethyl orthoacetate in a catalyst propionic acid at a certain temperature and pressure to generate crude methyl pyribinate. However, during the synthesis process, side reactions will occur, resulting in the reboiler isopentenyl berenate. [0003] [0004] During the rectification and purification process of the crude product of methyl perineate, isopentenyl perinetinate exists in the tower still in the form of raffinate. The treatment of traditional pyridyl ester rectification raffinate needs to go through saponification, acidification, esterification, rectification and other processes to generate pyridinic acid isopentenyl ester in the bottom material into pyridinic acid ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/03C07C67/48C07C67/54C07C69/533C07C29/128C07C29/80C07C31/04C07C33/03
CPCC07C29/1285C07C29/80C07C67/03C07C67/48C07C67/54C07C69/533C07C31/04C07C33/03
Inventor 霍朝飞杨仁春魏学岭刘欢张焕壮任一鸣蒯龙潘梦张翠歌李芳许茂东张荣莉李兴扬唐定兴石志盛
Owner 安徽鑫泰新材料有限公司
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