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A kind of method that tert-butanol and formaldehyde prepare isoprene

A technology for the preparation of formaldehyde and isoprene, applied in the direction of hydrocarbon production from oxygen-containing organic compounds, organic chemistry, chemical recovery, etc., can solve the problems of low process yield, equipment corrosion, cumbersome steps, etc., and achieve high yield, Corrosion Reduction and Yield Improvement Effects

Active Publication Date: 2019-04-12
SHANDONG YUHUANG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to realize the production of isoprene by chemical synthesis, solve the chain scission problem of C4 and C5, and promote the development and utilization of C4 downstream products, optimize the process conditions in the isoprene synthesis method, and improve the existing production of isoprene The pentadiene process has problems such as low yield, complex operation, cumbersome steps, and serious equipment corrosion. The invention provides a method for synthesizing isoprene in one step

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A method for preparing isoprene from tert-butanol and formaldehyde, including the steps:

[0025] 1) Mix 24.13g industrial grade phosphoric acid aqueous solution (85%) and 2.68g industrial grade oxalic acid uniformly, add 45.08g industrial grade formaldehyde aqueous solution (37%) and mix evenly, then add 171.54g industrial grade tert-butanol aqueous solution (85%) Mix well, and finally add 1.85g technical grade copper sulfate to obtain a reaction solution;

[0026] 2) Turn on the heating of the preheater (the temperature is set to 120℃) and the tubular reactor (the temperature is set to 60℃), and pour nitrogen into the reaction device; use a liquid sample pump at 1.8mL / min Sampling speed: During the feeding process, the pressure in the reaction device is adjusted to 1.2Mpa through the back pressure valve;

[0027] 3) After the reaction, the reaction liquid enters the receiving tank through the condenser. The reaction liquid is stratified in the receiving tank. The lower laye...

Embodiment 2

[0029] A method for preparing isoprene from tert-butanol and formaldehyde, including the steps:

[0030] 1) Mix 23.11g technical grade phosphoric acid aqueous solution (85%) and 2.1g technical grade oxalic acid uniformly, add 50.12g technical grade formaldehyde aqueous solution (37%) and mix evenly, then add 170.45g technical grade tert-butanol aqueous solution (85%) Mix evenly, and finally add 1.76g industrial grade iron sulfate to obtain a reaction solution;

[0031] 2) Turn on the heating of the preheater (the temperature is set to 120℃) and the tubular reactor (the temperature is set to 165℃), and pass nitrogen into the reaction device; use a liquid injection pump to feed at 25mL / min Sampling speed is injected, and the pressure in the reaction device is adjusted to 1.4Mpa through the back pressure valve during the feeding process;

[0032] 3) After the reaction, the reaction liquid enters the receiving tank through the condenser. The reaction liquid is stratified in the receivin...

Embodiment 3

[0034] A method for preparing isoprene from tert-butanol and formaldehyde, including the steps:

[0035] 1) Mix 24.11g technical grade phosphoric acid aqueous solution (85%) and 1.56g technical grade boric acid uniformly, add 50.05g technical grade formaldehyde aqueous solution (37%) and mix evenly, then add 170.63g technical grade tert-butanol aqueous solution (85%) Mix evenly, and finally add 2.65g technical grade copper chloride to obtain a reaction solution;

[0036] 2) Turn on the heating of the preheater (the temperature is set to 110℃) and the tubular reactor (the temperature is set to 158℃), and pour nitrogen into the reaction device; use a liquid injection pump at 2.2mL / min The injection speed is used for sampling, and the pressure in the reaction device is adjusted to 0.8Mpa through the back pressure valve during the feeding process;

[0037] 3) After the reaction, the reaction liquid enters the receiving tank through the condenser. The reaction liquid is stratified in the...

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PUM

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Abstract

The invention discloses a method for preparing isoprene from tert-butyl alcohol and formaldehyde, belonging to the technical field of chemical synthesis. The method comprises the following steps: with an industrial formaldehyde solution and a tert-butyl alcohol solution as reactants, industrial phosphoric acid as a catalyst and metal salt as a reaction promoter, carrying out preheating, and carrying out reaction under a certain temperature and pressure so as to obtain isoprene. With the method provided by the invention, metal salt added into a reaction system is used as the reaction promoter, so the yield of isoprene can be effectively improved, and corrosion of liquid acid to equipment can be greatly mitigated; and a counterbalance valve is adopted as a reaction device to control pressure in a reactor, so good pressure control effect is realized, and the counterbalance valve exerts an emptying effect at the same time, wherein a receiving tank is internally divided into a lower layer water phase and an upper layer oil phase. The method provided by the invention has the following advantages: process conditions are easily controllable; pressure is stable; the catalyst and tert-butyl alcohol are reusable; and isoprene has high yield (relative to formaldehyde, isoprene has the highest yield of 74.21%).

Description

Technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for preparing isoprene from tert-butanol and formaldehyde. Background technique [0002] Isoprene has a typical conjugated double bond structure. It is a colorless and volatile organic chemical raw material. It is mainly used in the field of synthetic rubber. It can not only produce cis 1,4-isoprene rubber and trans 1, 4-isoprene rubber can replace natural rubber, and can also synthesize special polymer materials and other fine chemicals. [0003] At present, the production of isoprene has achieved industrialization. There are two methods: separation method and synthesis method. The separation method is the earliest industrial method to produce isoprene, mainly through solvent extraction and other methods to crack isoprene from petroleum. Separated from five components. But from a long-term perspective, with the change of the ethylene industry pattern, especially t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C1/24C07C11/18
CPCY02P20/584
Inventor 赵存胜景文何龙肖博常俊丽陈双喜王胜伟
Owner SHANDONG YUHUANG CHEM CO LTD