Method for preparing 3-methyl-3-butylene-1-alcohol

A technology of butene and methyl, which is applied in the field of catalytic synthesis, can solve the problems of high reaction temperature, high reaction pressure, acid catalyst corrosion, etc., and achieve the effect of solving the reaction temperature

Inactive Publication Date: 2012-09-12
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of this invention is to provide a novel solid acid - a method for the synthesis of 3-methyl-3-buten-1-alcohol with a solid-supported stannous chloride catalyst, which solves the problem of acid catalyst corro

Method used

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  • Method for preparing 3-methyl-3-butylene-1-alcohol
  • Method for preparing 3-methyl-3-butylene-1-alcohol

Examples

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Effect test

Embodiment 1

[0042] The above-prepared 3gSnCl 2 The solid-supported catalyst is placed in the middle of a stainless steel fixed-bed reaction tube with an inner diameter of 8 mm and a length of 300 mm, and the upper and lower parts of the catalyst are filled with 40-60 mesh quartz sand; 2 The air in the fixed-bed reactor was purged clean, and the temperature was raised to 120°C to be constant. Put 100g of polyoxymethylene solid in a polyoxymethylene depolymerization spherical glass container, and raise the temperature to 150°C and keep it constant. Cut off N 2 , the flow rate is 30ml / min C 4 The mixed gas (the mass fraction of isobutylene is 10%) is passed into the spherical glass container of polyoxymethylene solid depolymerization, carrying the gaseous formaldehyde generated by the depolymerization of polyoxymethylene, and enters the fixed bed reactor equipped with catalyst. The speed is 10.4h -1 , to carry out the catalytic reaction of synthesizing 3-methyl-3-buten-1-ol. At this tim...

Embodiment 2

[0044] The above-prepared 3gSnCl 2 The solid-supported catalyst is placed in the middle of a stainless steel fixed-bed reaction tube with an inner diameter of 8 mm and a length of 300 mm, and the upper and lower parts of the catalyst are filled with 40-60 mesh quartz sand; 2 The air in the fixed-bed reactor was purged clean, and the temperature was raised to 120°C to be constant. Put 100g of polyoxymethylene solid in a spherical glass container for polyoxymethylene depolymerization, and raise the temperature to 200°C and keep it constant. Cut off N 2 , the flow rate is 30ml / min C 4 The mixed gas (the mass fraction of isobutylene is 10%) is passed into the spherical glass container of polyoxymethylene solid depolymerization, carrying the gaseous formaldehyde generated by the depolymerization of polyoxymethylene, and enters the fixed bed reactor equipped with catalyst. The speed is 16.6h -1 , to carry out the catalytic reaction of synthesizing 3-methyl-3-buten-1-ol. At this...

Embodiment 3

[0046] The above-prepared 3gSnCl 2 The solid-supported catalyst is placed in the middle of a stainless steel fixed-bed reaction tube with an inner diameter of 8 mm and a length of 300 mm, and the upper and lower parts of the catalyst are filled with 40-60 mesh quartz sand; 2 The air in the fixed-bed reactor was purged, and the temperature was raised to 180°C to be constant. Put 100g of polyoxymethylene solid in a polyoxymethylene depolymerization spherical glass container, and raise the temperature to 150°C and keep it constant. Cut off N 2 , the flow rate is 30ml / min C 4 The mixed gas (wherein the mass fraction of isobutylene is 10%) passes into the spherical glass container of polyoxymethylene solid depolymerization, carrying the gaseous formaldehyde generated by the depolymerization of polyoxymethylene, and enters the fixed bed reactor equipped with catalyst. The mass space velocity of formaldehyde is 10.4h -1 , to carry out the catalytic reaction of synthesizing 3-meth...

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Abstract

The invention relates to a method for synthesizing 3-methyl-3-butylene-1-alcohol on a solid acid catalyst and belongs to the field of catalytic synthesis. According to the method, by the solid acid catalyst, SnCl2 is immobilized on Al2O3, SiO2 and Al2O3-SiO2 compound oxides, which have a porous channel structure and hydroxyl groups on the surface, or silicon-aluminum molecular sieves, and isobutene and formaldehyde serving as raw materials are reacted to synthesize 3-methyl-3-butylene-1-alcohol. The catalytic synthesis is conducted in a solid-gas reactor, the catalyst is the SnCl2 immobilized catalyst, the reaction temperature is between 120 and 300 DEG C, and the reaction pressure is the normal pressure. The method solves the problem that acid catalysts erode equipment and contaminate environment in the conventional production process; and the method also solves the problem of requirement on high reaction temperature and high reaction pressure during use of the conventional alkali catalysts.

Description

technical field [0001] The invention relates to a preparation method of 3-methyl-3-buten-1-ol, which belongs to the field of catalytic synthesis. Background technique [0002] Tin protochloride, also known as tin dichloride, is a widely used Lewis acid catalyst, and its anhydrous is colorless or white needle-like crystals. Tin protochloride can accept electrons, and has a good catalytic effect in reactions such as acid alcohol esterification, acetal, ketal, dehydration, diene synthesis, and heterocycle synthesis. However, its application is more and more restricted due to its strong corrosiveness, difficulty in separating the same products, and the production of a large amount of waste water. [0003] The 3-methyl-3-buten-1-ol (also known as MBOH) produced by the reaction of isobutene and formaldehyde is an important raw material for the synthesis of terpenes, water reducers and rubber; the isomer of MBOH, 3-methyl-2- Buten-1-ol (also known as isopentenol) is a raw materia...

Claims

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Application Information

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IPC IPC(8): C07C33/025C07C29/38B01J27/135
Inventor 纪敏李雪峰朱建民周立明周已勇蔡天锡
Owner DALIAN UNIV OF TECH
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