Method for continuously producing 3-methyl-3-butylene-1-alcohol

A butene and methyl technology, applied in organic chemistry, oxygen-containing functional group reduction preparation, etc., can solve the problems of unstable quality, high reaction pressure, and many side reactions, and achieve high heat and mass transfer efficiency and mild reaction conditions. , the effect of fast response

Inactive Publication Date: 2013-10-02
JIANGSU SOBUTE NEW MATERIALS +1
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a method for continuous production of 3-methyl-3-butene-1-ol, which solves the problem of small contact area between reaction media and low heat and mass transfer efficiency due to the use of gap

Method used

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  • Method for continuously producing 3-methyl-3-butylene-1-alcohol

Examples

Experimental program
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Effect test

Embodiment 1

[0024] use figure 1 The shown continuous reaction device carries out the following operation process. Add 100kg of paraformaldehyde and 380L of industrial methanol to the stirring tank 1 (the purity of industrial methanol is: 98%, the converted molar ratio of paraformaldehyde and methanol is: 1:2.8), heat to 50°C under stirring, and continue stirring 2h until the paraformaldehyde is completely dissolved, then the paraformaldehyde solution and isobutylene are fed into the raw material bottle 2 at a volume ratio of 8.6:1 (the converted molar ratio of paraformaldehyde and isobutylene is 1:6.5), and then the raw material Fill the bottle 2 with nitrogen to 0.7MPa, and use the advection pump 3 to the tubular fixed bed reactor 4 at a space velocity of 1h -1 Continuously feed into the reactor 5, maintain the reaction temperature at 230°C, the reaction pressure at 8.5MPa, and continue to react for 25 hours. After the material is reacted in the tubular fixed bed reactor 4, it is cooled...

Embodiment 2

[0026] use figure 1 The shown continuous reaction device carries out the following operation process. Add 50kg of paraformaldehyde and 163L of industrial methanol to the stirring tank 1 (the purity of industrial methanol is: 98%, the converted molar ratio of paraformaldehyde and methanol is: 1:2.4), heat to 45°C while stirring, and continue stirring 2.5h until the paraformaldehyde is completely dissolved, then the paraformaldehyde solution and isobutylene are fed into the raw material bottle 2 at a volume ratio of 7.5:1 (the molar ratio of paraformaldehyde and isobutylene is converted to 1:7.6), and then Fill the raw material bottle 2 with nitrogen to 0.75MPa, and use the advection pump 3 to the tube-and-tube fixed-bed reactor 4 at a space velocity of 1.2h -1 Continuously feed into the reactor 5, maintain the reaction temperature at 240°C, the reaction pressure at 8.0MPa, and continue to react for 14 hours. After the material is reacted in the tubular fixed bed reactor 4, it ...

Embodiment 3

[0028] use figure 1 The shown continuous reaction device carries out the following operation process. Add 80kg of paraformaldehyde and 282L of industrial methanol to the stirred tank 1 (the purity of industrial methanol is: 98%, the converted molar ratio of paraformaldehyde and methanol is: 1:2.6), heat to 55°C while stirring, and continue stirring 2h until the paraformaldehyde is completely dissolved, then feed the paraformaldehyde solution and isobutylene into the raw material bottle 2 at a volume ratio of 8.0:1 (the converted molar ratio of paraformaldehyde to isobutylene is 1:7.0), and then feed the raw material Fill the bottle 2 with nitrogen to 0.8MPa, and use the advection pump 3 to the tube-and-tube fixed-bed reactor 4 at a space velocity of 1.8h -1 Continuously feed into the reactor 5, maintain the reaction temperature at 250°C, the reaction pressure at 9.0MPa, and continue to react for 18 hours. After the material is reacted in the tubular fixed bed reactor 4, it is...

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Abstract

The invention relates to a method for continuously producing 3-methyl-3-butylene-1-alcohol. The method comprises the steps of firstly dissolving polyformaldehyde in methanol; mixing the obtained solution with isobutylene to obtain a mixture; then pumping the mixture into a multitubular fixed bed reactor; contacting the mixture with gamma-Al2O3 dipped with an alkali metal phosphate catalyst dissolved by deionized water filled in the reactor; carrying out a nucleophilic addition reaction under the effect of the catalyst; then cooling reaction products; carrying out gas-liquid separation; and then rectifying and drying the separated solution. The method overcomes disadvantages of small contacting area of reaction mediums, low heat and mass transfer efficiency, high reaction pressure, many side reactions, low production efficiency, unstable quality and poor security and reliability and the like which are caused by adopting an intermittent tank reactor, so that continuous production of 3-methyl-3-butylene-1-alcohol by using isobutylene and polyformaldehyde as raw materials is realized.

Description

technical field [0001] The invention relates to a continuous production method of 3-methyl-3-buten-1-ol, a key synthetic raw material of the third-generation polycarboxylic acid high-efficiency water reducer for concrete, and belongs to the technical field of organic chemical industry. Background technique [0002] 3-Methyl-3-butene-1-ol (MBOH) is the initiator of the side chain-TPEG polyether of the third generation polycarboxylate high-efficiency water reducer for synthetic concrete. The TPEG polyether synthesized from this raw material is suitable for The quality and performance of polycarboxylate high-efficiency superplasticizer products play a decisive role, making it have strong ability to maintain the dispersion of cement particles, low dosage, high water-reducing rate, good reinforcement effect, durability, no corrosion of steel bars and Environmentally friendly and other advantages. In addition, 3-methyl-3-buten-1-ol can be isomerized into isopentenol, which is use...

Claims

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Application Information

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IPC IPC(8): C07C33/025C07C29/14
Inventor 冉千平王涛杨勇范士敏刘加平
Owner JIANGSU SOBUTE NEW MATERIALS
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