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Method for gas-phase solvent-free catalysis-free synthesis of 3-methyl-3-butenyl-1-alcohol

A solvent-free, butenyl-based technology is applied in the preparation field of solvent-free and catalytic synthesis of 3-methyl-3-butenyl-1-ol, which can solve the problems of low yield and the like, and achieves reduction of energy consumption and savings Operation steps, the effect of reducing difficulty

Active Publication Date: 2011-05-18
吉林众鑫化工集团有限公司
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

In June 2010, Dalian University of Technology Li Xuefeng and others published a research paper: using isobutylene and polyoxymethylene as raw materials and dioxane as solvent, using immobilized Sncl 4 Catalyst, can react under mild conditions, but the yield is low (60wt%)

Method used

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  • Method for gas-phase solvent-free catalysis-free synthesis of 3-methyl-3-butenyl-1-alcohol
  • Method for gas-phase solvent-free catalysis-free synthesis of 3-methyl-3-butenyl-1-alcohol
  • Method for gas-phase solvent-free catalysis-free synthesis of 3-methyl-3-butenyl-1-alcohol

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Embodiment 1

[0027] Embodiment 1:. The depolymerization of paraformaldehyde

[0028] In order to reduce side reactions and facilitate the refining of products, 3g of industrial paraformaldehyde and 30g of isobutylene are pulped first. After the 280ml stirred autoclave was replaced with N2, the slurry was pressed into the autoclave, the temperature was raised, the temperature and pressure were observed, and the gas composition was detected, and the depolymerization temperature, pressure and residence time of paraformaldehyde were calculated. The present invention controls the temperature to be 120-200° C., the depolymerization time to be 10-60 minutes, and the pressure to be 9.0-15.0 Mpag.

[0029] Paraformaldehyde HO-(CH 2 O) n-H, where n is generally 8 to 100, and formaldehyde is 90-99%. We use lower values ​​of n. Formaldehyde purity is 90-94%. Instead of using α, β, γ, δ and ε type paraformaldehyde to reduce the difficulty of depolymerization. Paraformaldehyde and isobutylene (liqu...

Embodiment 2

[0032] Example 2: Condensation reaction of isobutylene and formaldehyde prins to generate isopentenol (3.3.1).

[0033] The above-mentioned isobutene, formaldehyde, and the isobutene calculated according to the ratio of isobutene: formaldehyde = 8 ~ 15 mol ratio are heated and vaporized with high-pressure nitrogen, and then pressed into a plug flow reactor immersed in a hot oil bath, and the temperature is controlled at 200 ~ 300°C, pressure 9.0-15.0Mpag, residence time 1-3h; during this period, measure the composition of prenol (3, 3, 1), formaldehyde and isobutene in the reactor every 10 minutes until the residence time is reached, and then react The product is placed in a dry ice bath at -70°C to condense it completely, and the liquid phase composition is measured. The product isopentenol (3, 3, 1) isobutene and moisture are deducted, and the concentration is greater than 95wt%. The isobutene is separated and recycled. The product yield was 90 wt% based on isobutene and 97 ...

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Abstract

The invention provides a method for gas-phase solvent-free catalysis-free synthesis of 3-methyl-3-butenyl-1-alcohol, comprising the following steps: preparing paraformaldehyde (PFA) and isobutene into slurry material at first; then carrying out deploymerization according to technology condition requirements to obtain gas-phase formaldehyde and isobutene; and carrying out a prins reaction under rated conditions, thus greatly reducing energy consumption and pollutants. The purity of the product 3-methyl-3-butenyl-1-alcohol reaches above 94wt%, and the yields of the PFA and the isobutene respectively reaches 97% and 90%.

Description

technical field [0001] The present invention relates to a preparation method of 3-methyl-3-butenyl-1-alcohol, in particular to a method for preparing 3-methyl-3-butenyl-1-alcohol without solvent and catalyst . Background technique [0002] It is well known that 3-methyl-3-butenyl-1-ol, hereinafter referred to as prenol (3.3.1), is prepared by a thermal condensation process of a prins reaction. The reaction formula is: [0003] [0004] In 1955, Blomguist et al. first published that the target product was obtained from isobutylene, polyoxymethylene, glacial acetic acid and acetic anhydride at 190°C, 3.6 MPag, and the reaction time was 8 hours, but the yield was very low. In 1976, a paper was published by Paul and Paul Stapp of Phillips Petroleum Company, using isobutylene and polyoxymethylene at 13.8MPag, 275-300°C condensation reaction time 35 minutes, but the effect is not ideal, the conversion rate and Yields are low. The continuous research in the future is to chan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/025C07C29/14
Inventor 张汉倬阿蒙纳蒂崔永军
Owner 吉林众鑫化工集团有限公司
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