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Method for gaseous-phase catalysis-free continuous synthesizing of 3-methyl-3-butenyl-1-alcohol

A butene-based, continuous process technology, applied in organic chemistry, reduction preparation of oxygen-containing functional groups, etc., can solve problems such as blockage of pipelines

Inactive Publication Date: 2013-08-21
吉林众鑫化工集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the problem that after paraformaldehyde is pulped with isobutylene, in the process of depolymerization, formaldehyde self-polymerizes to generate paraformaldehyde, and chain breaks to generate paraformaldehyde to block pipelines and equipment, thereby improving the recovery of paraformaldehyde Rate

Method used

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  • Method for gaseous-phase catalysis-free continuous synthesizing of 3-methyl-3-butenyl-1-alcohol
  • Method for gaseous-phase catalysis-free continuous synthesizing of 3-methyl-3-butenyl-1-alcohol

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Example 1 (pre-depolymerization of paraformaldehyde ）

[0020] The pre-depolymerization of paraformaldehyde is at 0.1M 3 carried out in a stirred and jacketed atmospheric tank reactor. First replace the reactor with N2 and then add 20Kg of methanol and 0.4Kg of TEA. Turn on the stirrer, slowly add 20Kg of 96wt%~97wt% paraformaldehyde, and pass 80°C hot water into the jacket to keep the liquid phase temperature in the kettle at 40~60°C for about 40~100min. There was no solid precipitate in the kettle. This liquid was put into an autoclave and pressurized with nitrogen to prepare for the synthesis reaction.

[0021] The formaldehyde content of the pre-depolymerization liquid is 46wt%-48wt%, and the rest is methanol and a small amount of water.

Embodiment 2

[0022] Example 2: (Synthesis of 3-methyl-3-butenyl-1-ol from isobutene and formaldehyde)

[0023] Mix fresh isobutene and recovered isobutene, send it to the inlet of the high pressure pump at a pressure of 0.2-0.3MPag, pressurize it to 13.0MPag, and pass through the steam heater and heat exchanger in turn heat medium) and an electric heater to raise the temperature to 270-290°C and send it into the synthesis reactor. The reactor pressure is 12-13.5MPag. The paraformaldehyde pre-depolymerization solution prepared in example 1 is also delivered to the plug flow reactor by nitrogen pressure, and the pre-depolymerization solution is evaporated and vaporized immediately in the reactor, and the quantity of two kinds of feeds is adjusted so that isobutylene and The molar ratio of formaldehyde was 12:1 and the retention time was 1 hour. The temperature in the reactor is 260°C and 270°C. The gas at the outlet of the reactor exchanges heat with the incoming isobutylene, and the pre...

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Abstract

The invention discloses a method for the gaseous-phase catalysis-free continuous synthesizing of 3-methyl-3-butenyl-1-alcohol. According to the method, no paraformaldehyde serving as a main related raw material is used for pulping in isobutylene liquid, so that when the suspension liquid of the paraformaldehyde is heated to depolymerize, the escaped formaldehyde cannot automatically polymerize again to form solid paraformaldehyde and delink to generate trioxymethylene, and thus, heat exchangers and pipelines cannot be blocked. The method comprises the steps of: pre-depolymerizing the paraformaldehyde (allowed to be above 96wt%) in methanol to form formaldehyde dissolved in the methanol, and thus obtaining a pre-depolymerizing liquid; and pressurizing to continuously feed the formaldehyde to a reactor to be subjected to a synthetic reaction with isobutylene at the temperature of 270-290 DEG C and pressure of 10.0MPag-16MPag according to an olefine aldehyde molar ratio of 8-15 for a retention time of 50-100 minutes. The product yield can reach 93-95%.

Description

technical field [0001] The invention relates to a method for continuously synthesizing 3-methyl-3-butenyl-1-ol in a gas phase without catalysis. Background technique [0002] 3-methyl-3-butenyl-1-ol is produced by isobutene and formaldehyde through the Prince reaction. Since this product is an important intermediate for the synthesis of fragrances, medicines, pesticides, and citral, it can be dehydrated to produce isoamyl Diene is an important raw material of isoprene. Especially in the past ten years, with the rapid development of the third generation of high-performance polycarboxylate cement superplasticizer, the demand for 3-methyl-3-butenyl-1-ol is increasing day by day. There are more than 20 patents in this field at home and abroad. In particular, Jilin Zhongxin Chemical Group Co., Ltd.'s first domestic device with an annual output of 5,000 tons adopts the company's own technology "gas-phase solvent-free and non-catalytic synthesis of 3-methyl-3-butenyl-1-ol (patent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/025C07C29/14
Inventor 郑德昌赵德平何永亮崔庆龙张汉倬
Owner 吉林众鑫化工集团有限公司
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