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Method for synthesizing 3-methyl-3-butene-1-ol

A technology of butene and methyl, applied in the field of synthesizing 3-methyl-3-butene-1-ol, can solve the problems of low production efficiency, batch reaction mixing, high operating intensity and the like

Active Publication Date: 2016-03-30
HANGZHOU ZJU HOLLEY TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] One of object of the present invention is to solve the side reaction that existing technology exists in the process of producing 3-methyl-3-buten-1-alcohol more, product yield is lower, unfriendly to environment, intermittent reaction mixes and The mass and heat transfer effect is not good, the production efficiency is low and the operation intensity is high, the safety hazard is large, the product quality is unstable, etc.

Method used

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Examples

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Embodiment 1

[0024] see figure 1 , the formaldehyde solution with methanol as the solvent (hereinafter referred to as formaldehyde methanol solution) is pressurized to 18MPa by the formaldehyde methanol solution feed pump 1, and then heated to 160°C by the formaldehyde methanol solution preheater 2, after reaching a near critical state Continuously enter the tubular reactor 5 from the top of the tubular reactor 5 with a mixing zone in the form of spray; at the same time, another raw material isobutene is pressurized to 18MPa through the isobutylene feed pump 3, and then passed through the isobutylene preheater 4 Heating to 280°C, after reaching the supercritical state, it continuously enters the tubular reactor 5 from the top side of the tubular reactor 5, and the raw material formaldehyde-methanol solution and the raw material isobutylene that reach the tubular reactor 5 through the above-mentioned process The reaction takes place in the tubular reactor 5 (reaction temperature is 280° C.,...

Embodiment 2

[0027] see figure 1 The raw material formaldehyde-methanol solution (formaldehyde solution with methanol as solvent) is pressurized to 15MPa by the formaldehyde-methanol solution feed pump 1, and then heated to 150°C by the formaldehyde-methanol solution preheater 2. Continuously enter the tubular reactor 5 from the top of the tubular reactor 5 with a mixing zone; at the same time, another raw material isobutene is pressurized to 15 MPa by the isobutene feed pump 3, and then heated to 220 by the isobutene preheater 4 °C, after reaching the supercritical state, it enters the tubular reactor 5 continuously from the top side of the tubular reactor 5, and the raw material formaldehyde methanol solution and the raw material isobutylene that reach the tubular reactor 5 through the above process are in the tubular reactor. Reaction takes place in reactor 5 (reaction temperature is 220° C., reaction pressure is 15 MPa) to obtain 3-methyl-3-buten-1-ol product. The 3-methyl-3-buten-1-o...

Embodiment 3

[0030] see figure 1 , the raw material formaldehyde methanol solution (formaldehyde solution with methanol as solvent) is pressurized to 20MPa by the formaldehyde methanol solution feed pump 1, and then heated to 200°C by the formaldehyde methanol solution preheater 2. After reaching a near critical state, it is sprayed Continuously enter the tubular reactor 5 from the top of the tubular reactor 5 with a mixing zone; at the same time, another raw material isobutene is pressurized to 22 MPa by the isobutylene feed pump 3, and then heated to 300 MPa by the isobutylene preheater 4 °C, after reaching the supercritical state, it enters the tubular reactor 5 continuously from the top side of the tubular reactor 5, and the raw material formaldehyde methanol solution and the raw material isobutylene that reach the tubular reactor 5 through the above process are in the tubular reactor. Reaction takes place in reactor 5 (reaction temperature is 300° C., reaction pressure is 22 MPa) to o...

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Abstract

The present invention provides a method for synthesizing 3-methyl-3-butene-1-ol. The method comprises the following steps: pressurizing a raw material, a formaldehyde methanol solution, to 15-22 MPa, heating to 150-200 DEG C, and continuously feeding the solution, in a spray form, into a reactor after achieving a near-critical state; and meanwhile pressurizing another raw material, isobutylene, to 15-22 MPa, heating to 220-300 DEG C and continuously feeding into the reactor. The raw material formaldehyde methanol solution and the raw material isobutylene react in the reactor under conditions of temperature of 220-300 DEG C and pressure of 15-22 MPa. According to the method for synthesizing 3-methyl-3-butene-1-ol provided by the present invention, occurrences of formaldehyde self-polymerization and disproportionation reaction are reduced, and the product yield is improved. The reaction rate is increased, and the reaction effect is improved.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, in particular to a method for synthesizing 3-methyl-3-buten-1-ol. Background technique [0002] 3-Methyl-3-buten-1-ol is a colorless transparent liquid at normal temperature and pressure, and is an important intermediate used in the synthesis of polycarboxylic acid concrete water reducers, pyrethroid pesticides, lemon Aldehydes, carotenoids and vitamin A. At present, the synthetic method of 3-methyl-3-butene-1-ol mainly contains following several kinds: (1) take methallyl chloride as raw material, react with Grignard reagent to obtain 3-methyl-3-butane En-1-alcohol; (2) use isoprene as raw material to obtain 3-methyl-3-buten-1-alcohol through isomerization reaction; (3) use formaldehyde and isobutene as raw material, in catalyst action 3-methyl-3-butene-1-alcohol (see patent document 1) is obtained by prins reaction (homogeneous phase / heterogeneous phase) under; (4) take forma...

Claims

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Application Information

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IPC IPC(8): C07C33/025C07C29/38
CPCC07C29/38C07C33/025
Inventor 吴嘉林龙勇鲍艳胡晓萍
Owner HANGZHOU ZJU HOLLEY TECH
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