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Pentenoic acid methylester preparation process

A technology of methyl pyretinate and trimethyl orthoacetate, which is applied in the technical field of preparing methyl pyretinate by a method, and can solve the problems of inability to obtain fine-quality methyl pyretinate, excess, low product yield, etc.

Active Publication Date: 2014-06-18
NANTONG TENDENCI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shortcoming of this technology is: reaction time is long, product yield is low, and trimethyl orthoacetate needs to be greatly excessive, and simultaneously the product methyl pyretinate content is low, can not obtain high-quality goods methyl pyretinate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Put 5060 kg (42 thousand moles) of trimethyl orthoacetate with a content of 99.6% in a 10,000-liter pressure reactor with a rectifying tower, and heat it up to 150-155 ° C (the reaction pressure can be adjusted by pressing nitrogen or a pressure relief valve) ), firstly add propionic acid (74 kg in total, 1 kilomol) catalyst at 7.4 kg / h through the injection metering pump for a total of 10 hours; 1 hour after the catalyst is added, add 98% content at a feed rate of 390 kg / h, moisture ≤ 0.1% prenyl alcohol (3510 kg in total, 4 thousand moles) for 9 hours; with the progress of the reaction, the methanol containing a small amount of trimethyl orthoacetate was separated from the top of the rectifying tower, and the reaction temperature was gradually increased to 180-190 ℃. ℃, and keep the reaction at 175-185 ℃ until the prenyl alcohol content in the pressure reactor is less than or equal to 0.5%, the reaction is finished, and the reaction time is 13.5 hours. The reaction ma...

Embodiment 2

[0012] Put 5783 kg (48 thousand moles) of trimethyl orthoacetate with a content of 99.6% in a 10,000-liter pressure reactor with a rectifying tower, and heat it up to 150-155 ° C (the reaction pressure can be adjusted by pressing nitrogen or a pressure relief valve) ), firstly add propionic acid (74 kg in total, 1 kilomol) catalyst at 7.4 kg / h through the injection metering pump for a total of 10 hours; 1 hour after the catalyst is added, add 98% content at a feed rate of 390 kg / h, moisture ≤ 0.1% prenol (3510 kg in total, 4 thousand moles) for 9 hours; with the progress of the reaction, the methanol containing a small amount of trimethyl orthoacetate was separated from the top of the rectifying tower, and the reaction temperature was gradually increased to 175-180 °C. ℃, and keep the reaction at 175-180 ℃ until the prenyl alcohol content in the pressure reactor is less than or equal to 0.5%, the reaction is finished, and the reaction time is 12 hours. The reaction mass w...

Embodiment 3

[0014] 5783 kilograms (48 thousand moles) of trimethyl orthoacetate with a content of 99.6% were put into a 10,000-liter pressure reaction kettle with a rectifying tower, and 5,783 kilograms (48 kilomoles) of trimethyl orthoacetate and a 50 kg of ionic liquid catalyst, heated to 150-155 °C (reaction pressure can be adjusted by pressing nitrogen or pressure relief valve), through injection metering pump, adding 98% content, moisture ≤ 0.1% isoprene at a feeding rate of 390 kg / hour Enol (3510 kg in total, 4 thousand moles) for 9 hours; with the progress of the reaction, methanol containing a small amount of trimethyl orthoacetate was separated from the top of the rectification tower, and the reaction temperature was gradually increased to 170-175 ° C, and at 170-175 DEG C of insulation reaction to the pressure reaction kettle in the prenyl alcohol content ≤ 0.5%, the reaction is over, the reaction time is 12 hours. The reaction mass was cooled to below 50°C, and the obtaine...

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Abstract

The invention mainly discloses a pentenoic acid methylester preparation method, which is characterized in that prenol and trimethyl orthoacetate are in pressurized reaction in the existence of catalysts, and the by-product methanol is recovered by rectifying, so that pentenoic acid methylester is prepared. The pentenoic acid methylester preparation process has the advantages that reaction time is only 12-15 hours by means of pressurizing and catalyst synthesis, and the content of the prepared pentenoic acid methylester is higher than 99.8%.

Description

technical field [0001] The invention relates to a process for preparing methyl behenate, in particular to a process for preparing methyl behenate by a synthetic method. Background technique [0002] The traditional synthesis process of methyl benzate is simply synthesizing prenol and a large excess of trimethyl orthoacetate in the presence of phosphoric acid catalyst. The disadvantage of this process is that the reaction time is long, the product yield is low, the trimethyl orthoacetate needs to be excessively large, and the product methyl behenate is low in content at the same time, so the fine methyl behenate cannot be obtained. SUMMARY OF THE INVENTION [0003] The main task of the present invention is to provide a preparation process of methyl behenate, specifically a preparation technology of methyl behenate with short reaction time, high product purity and low cost of raw materials. [0004] In order to solve the above technical problems, a method for preparing m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/533C07C67/343
Inventor 谭祖明谭伟刚
Owner NANTONG TENDENCI CHEM
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