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Pentenoic acid methylester preparation process

A technology for the preparation of methyl pyretinate, which is applied in the technical field of preparing methyl pyretinate by a method, which can solve the problem of low content and excess of the product methyl pyretinate, and the inability to obtain high-quality methyl pyretinate, etc. question

Active Publication Date: 2012-08-15
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 5,060 kg (42 kilomoles) of trimethyl orthoacetate with a content of 99.6% in a 10,000-liter pressure reactor with a rectification tower, and raise the temperature to 150-155°C (the reaction pressure can be adjusted by pressing nitrogen or a pressure relief valve ), first add propionic acid (total 74 kg, 1 kilomole) catalyst through injection metering pump at 7.4 kg / hour for a total of 10 hours; after adding catalyst for 1 hour, add 98% content, moisture≤ 0.1% isopentenol (3510 kilograms in total, 4 kilomoles) for 9 hours; as the reaction proceeds, methanol containing a small amount of trimethyl orthoacetate is separated from the top of the rectifying tower, and the reaction temperature is gradually increased to 180-190 °C, and keep warm at 175-185 °C until the prenol content in the pressure reactor is ≤0.5%, the reaction is over, and the reaction time is 13.5 hours. The reaction material was cooled to below 50°C, and the obtained reaction product was subjected to co...

Embodiment 2

[0012] Put 5,783 kg (48 thousand moles) of trimethyl orthoacetate with a content of 99.6% in a 10,000-liter pressure reactor with a rectification tower, and raise the temperature to 150-155 ° C (the reaction pressure can be adjusted by pressing nitrogen or a pressure relief valve ), first add propionic acid (total 74 kg, 1 kilomole) catalyst through injection metering pump at 7.4 kg / hour for a total of 10 hours; after adding catalyst for 1 hour, add 98% content, moisture≤ 0.1% isopentenol (3510 kilograms in total, 4 kilomoles) for 9 hours; as the reaction progresses, methanol containing a small amount of trimethyl orthoacetate is separated from the top of the rectifying tower, and the reaction temperature is gradually increased to 175-180 °C, and keep warm at 175-180 °C until the prenol content in the pressure reactor is ≤0.5%, the reaction is over, and the reaction time is 12 hours. Cool the reaction material to below 50°C, and the obtained reaction product is subjected ...

Embodiment 3

[0014] Put 5,783 kg (48 thousand moles) of trimethyl orthoacetate with a content of 99.6% in a 10,000-liter pressure reactor with a rectification tower and trimethyl orthoacetate made from methyl triethyl ammonium chloride and anhydrous aluminum trichloride 50kg of ionic liquid catalyst, heated up to 150-155°C (the reaction pressure can be adjusted by pressing in nitrogen or a pressure relief valve), through the injection metering pump, add 98% content, moisture ≤0.1% isoamyl at a feeding speed of 390 kg / hour Enol (3510 kg in total, 4 thousand moles) for 9 hours; as the reaction progressed, 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 170-175 ° C, and 170-175°C heat preservation reaction until the prenol content in the pressure reactor is ≤0.5%, the reaction is over, and the reaction time is 12 hours. Cool the reaction material to below 50°C, and the...

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PUM

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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 present invention relates to a kind of preparation technology of methyl pyribinate, in particular to a kind of technology of adopting the synthesis method to prepare methyl pyribinate. Background technique [0002] The traditional synthesis process of methyl bentinate simply synthesizes isopentenol and a large excess of trimethyl orthoacetate in the presence of a phosphoric acid catalyst. The shortcoming of this technology is: reaction time is long, product yield is low, trimethyl orthoacetate needs to be greatly excessive, and the content of product methyl pyretinate is low at the same time, can not obtain high-quality goods methyl pyretinate. Contents of the invention [0003] The main task of the present invention is to provide a kind of preparation technology of methyl pyribinate, specifically a kind of preparation technology of the methyl pyridinate with short reaction time, high product purity and low raw material cost. [0004] In orde...

Claims

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Application Information

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IPC IPC(8): C07C69/533C07C67/343
Inventor 谭祖明谭伟刚
Owner NANTONG TENDENCI CHEM
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