Preparation method for 3-methyl-3-butene-1-ol

A technology of butene and methyl, applied in the field of synthesis of fine chemicals, can solve the problems of increased energy consumption, high risk, large reactor volume, etc., and achieves reduced investment and risk, high conversion rate and selectivity , good mass transfer and heat transfer performance

Active Publication Date: 2014-05-21
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This type of method has good application potential, but there are still many shortcomings in the current process: (1) the reaction temperature is as high as 200-300 ° C, the reaction pressure is as high as 10-30 MPa, and the reaction time is longer, generally higher than 30 minutes, In this way, the reactor will be very large in large-scale production, and the equipment investment is very large and dangerous under such harsh conditions; (2) The molar ratio of isobutylene to formaldehyde is generally 10:1 to 20:1. On the one hand, It will cause low effective utilization of equipment, on the other hand, so many isobutene cycles will cause high energy consumption
[0009] 2. The excess of isobutylene is 10-20 times, on the one hand, the volume of the reactor is large, and on the other hand, the energy consumption is increased
[0010] 3. 80% of the reaction system is isobutylene, which is very dangerous

Method used

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  • Preparation method for 3-methyl-3-butene-1-ol

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Experimental program
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Effect test

Embodiment 1

[0040] The temperature of the tubular reactor is set at 300°C, the reaction system pressure is 8MPa, the flow rate of 0.0023wt% europium nitrate aqueous solution is 11.52g / min, the flow rate of 37wt% formaldehyde aqueous solution is 24g / min, and the flow rate of isobutylene is 16.58g / min min, the residence time of the reaction solution in the reactor is about 3s (the residence time is the reaction time, the same below). Liquid chromatography analysis showed that the formaldehyde conversion rate was 98.02%, and gas chromatography analysis showed that the selectivity of 3-methyl-3-buten-1-ol was 94.33%. (The mass ratio of europium nitrate to formaldehyde is 0.00003:1, the mass ratio of water to formaldehyde is 3:1, and the molar ratio of isobutylene to formaldehyde is 1:1)

Embodiment 2

[0042] Set the temperature of the tubular reactor to 300°C, the pressure of the reaction system to 15MPa, the flow rate of 0.0016wt% europium nitrate aqueous solution to 17.01g / min, the flow rate of 37wt% formaldehyde aqueous solution to 7.3g / min, and the flow rate of isobutylene to 6.05g / min , the residence time of the reaction solution in the reactor is about 15s. Liquid chromatography analysis showed that the formaldehyde conversion rate was 99.11%, and gas chromatography analysis showed that the selectivity of 3-methyl-3-buten-1-ol was 95.06%. (The mass ratio of europium nitrate to formaldehyde is 0.0001:1, the mass ratio of water to formaldehyde is 8:1, and the molar ratio of isobutylene to formaldehyde is 1.2:1)

Embodiment 3

[0044] Set the temperature of the tubular reactor to 330°C, the pressure of the reaction system to 8MPa, the flow rate of 0.0008wt% samarium sulfate aqueous solution to 7.38g / min, the flow rate of 37wt% formaldehyde aqueous solution to 1.5g / min, and the flow rate of isobutylene to 1.04g / min , the residence time of the reaction solution in the reactor is about 15s. Liquid chromatography analysis showed that the formaldehyde conversion rate was 98.76%, and gas chromatography analysis showed that the selectivity of 3-methyl-3-buten-1-ol was 95.44%. (The mass ratio of samarium sulfate to formaldehyde is 0.0001:1, the mass ratio of water to formaldehyde is 15:1, and the molar ratio of isobutylene to formaldehyde is 1:1)

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Abstract

The invention discloses a preparation method for 3-methyl-3-butene-1-ol. The preparation method comprises the following steps of causing water, transition metal salt, isobutylene and formaldehyde to enter a condensation reactor, and performing condensation reaction under the conditions of 300 to 360 DEG C and 5 to 25MPa, wherein the transition metal salt is one or two or more of vanadium, chromium, iridium, iron, rhenium, ruthenium, cadmium, platinum, cerium, praseodymium, neodymium, samarium, europium, terbium, dysprosium, thulium and the like, the condensation reaction can be completely implemented within 1 to 100s under the synergistic catalysis of transition metal ions and [H3O<+>], and only a small amount of isobutylene is required; performing light component removal, dehydration and heavy component removal on condensation reaction liquid to obtain high-purity 3-methyl-3-butene-1-ol.

Description

technical field [0001] The invention relates to the field of synthesis of fine chemicals, in particular to a synthesis method of 3-methyl-3-buten-1-ol. technical background [0002] 3-Methyl-3-buten-1-ol is an important intermediate in the synthesis of fragrances, medicines, pesticides, etc.: (1) This substance can be used to synthesize citral, and thus further synthesize L-menthol and ionone , carotenoids, vitamin A, vitamin E, etc.; (2) After being converted into 3-methyl-2-buten-1-ol by hydroisomerization, it can be used to synthesize pyrethrins; (3) Dehydration into iso Pentadiene can be used to synthesize rubber; (4) This substance can also be used to synthesize high-performance polycarboxylate cement water reducer. [0003] The synthetic method of 3-methyl-3-butene-1-ol mainly contains following three kinds at present: [0004] (1) Using SnCl2 as a catalyst to condense isobutene and formaldehyde to prepare 3-methyl-3-buten-1-ol. GB1197971 uses SnCl2 and ZnCl2 as cat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/025C07C29/38
CPCC07C29/38C07C33/025
Inventor 李鹏张永振刘英俊崔乐超曹善健庞计昌李乐乐黎源
Owner WANHUA CHEM GRP CO LTD
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