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Penisopenteneester recovery method

A technology of isopentenyl bentinate and a recovery method, which is applied in the fields of chemistry and pesticides, can solve problems such as high recovery cost, complex recovery process, and deteriorating working environment, and achieves reduction in production cost, simple recovery process, and simple process Effect

Inactive Publication Date: 2007-01-17
HUBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, it is mostly used to add concentrated alkali to hydrolyze it into sodium bentingate. After extracting the low fraction through high temperature and high vacuum, add sulfuric acid to acidify it into benting acid, and then add methanol to esterify it into DPE. The recovery process is mature, but the recovery process is too complicated , the recovery cost is high, and the moisture in the recovered DPE seriously exceeds the standard, which affects the subsequent reaction. The released prenol is decomposed into isopentene under the action of concentrated alkali and escapes, which deteriorates the working environment and causes a large amount of prenol to be wasted.

Method used

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Experimental program
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Effect test

Embodiment 1

[0021] Embodiment 1: tetraisopropyl titanate as transesterification catalyst (A process)

[0022] Add 312g of isopentenyl perineate (containing 1.0mol of MBDP), 320g of anhydrous methanol (10.0mol), and 3mL of tetraisopropyl titanate (0.01mol) into the DSH-2 high-pressure reactor, and start stirring , after the temperature was raised to 152°C, gas chromatographic analysis was taken every half hour. When the reaction time reached 7.5 hours, the mass fraction of MBDP tended to be stable, and the reaction was terminated. The reaction solution was cooled to room temperature, and DC analysis showed that the mass fraction of MBDP was 1.87 %, the residual mass of MBDP was 11.4g, and the conversion rate was 94.2%; the mass fraction and mass of prenol produced were 12.7% and 77.4g, respectively.

Embodiment 2

[0023] Embodiment 2: Sodium methylate is as transesterification catalyst (B technology)

[0024] Add isopentenyl perineate 312D (MBDP1.0mol), anhydrous methanol 192D (6.0mol), and liquid sodium methoxide 3.8g (0.02mol) into the high-pressure reactor, and after heating up to 140°C, gas chromatography tracking analysis , after the reaction time reaches 6h, the mass fraction of MBDP tends to be stable, the cooling reaction solution, DC analysis, the mass fraction of MBDP is 8.2%, the remaining MBDP mass is 40g, and the conversion rate is 79.6%; the mass fraction of prenol and The masses are 13.9%, 67.8g, respectively.

Embodiment 3

[0025] Embodiment 3: Potassium hydroxide is as transesterification catalyst (C technology)

[0026] Add respectively 312g (MBDP1.0mol) of isopentenyl perineate, 192g (6.0mol) of anhydrous methanol, 9.3g (0.02mol) of potassium hydroxide methanol solution of 12% in the autoclave, be warming up to 140 ℃, Follow-up analysis showed that after 9 hours of reaction, the reaction was terminated, the mass fraction of MBDP was 10.1%, the mass fraction of residual MBDP was 49.8g, and the conversion rate was 74.6%; the mass fraction and mass of prenol produced were 11.6% and 57.2g, respectively.

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Abstract

Recovering method of pyriti-acid isopentene ester is carried out by reacting methanol with pyriti-acid isopentene ester, ester exchanging, converting MBDP into DPE and isopentene alcohol, entering into fresh reactive liquid, reacting and circulation utilizing. The proportion of methanol, pyriti-acid isopentene ester and catalyst is 1.0-100:1.0:0.001-11.0mol. It is cheap and simple.

Description

technical field [0001] Belongs to chemical and pesticide technology. Background technique [0002] DPE, also known as methyl 3,3-dimethyl-4-pentenoate, is an important intermediate for the synthesis of pyrethroid pesticides [1] , usually prepared by reacting isopentenol with trimethyl orthoacetate and undergoing Claisen rearrangement [1] . During the synthesis of DPE, there will generally be a by-product (or base material) that accounts for about 1 / 4 of the quality of DPE: 3,3-dimethyl-4-pentenoic acid-3'-methyl-2'- Butenyl ester (MBDP) has a high boiling point. After most of the DPE is evaporated, it is discharged in the form of still bottom material, and about 20% of DPE remains in the still bottom material. If DPE is further distilled out, MBDP and DPE are combined Boiling will reduce the mass fraction of DPE in the finished product, and the product is unqualified, so it is necessary to have about 20% DPE remaining in the bottom material (prenyl peripinate), so reclaim...

Claims

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Application Information

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IPC IPC(8): C07C69/533C07C69/527C07C67/02C07C67/48
Inventor 陈坤
Owner HUBEI UNIV OF TECH
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