Tert-carboxylic acid synthesis method

A technology of tertiary carbonic acid and tertiary carbonic acid anhydride, which is applied in the field of preparation of tertiary carbonic acid, can solve problems such as catalyst recovery difficulties, instrument corrosion, and lower reaction pressure, and achieve the effects of improving device economy, reducing waste water, and lowering reaction pressure

Active Publication Date: 2016-01-06
WANHUA CHEM GRP CO LTD
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Problems solved by technology

[0008] In order to solve the above-mentioned technical problems, an object of the present invention is to provide a method for synthesizing tertiary carbonic acid, using modified strong acidic ionic liquid as solvent and catalyst, which can dissolve carbon monoxide well, reduce reaction pressure, and simultaneously catalyst is easy to separate, solve Problems such as difficulty in catalyst recovery and instrument corrosion in the prior art are solved

Method used

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  • Tert-carboxylic acid synthesis method

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Embodiment 1

[0040] Weigh 1440g of pyridine butane sulfonic acid bisulfate ionic liquid (Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences) and add it to a 2.5L high-pressure reactor, replace the gas in the reactor with carbon monoxide and pressurize at 0.5Mpa, control the reaction temperature at 10°C, and keep stirring Add 6.62g of cuprous oxide and continue stirring for 2h to prepare a strongly acidic ionic liquid-copper carbonyl catalyst. Then feed 47.1 g of diisobutene, keep the pressure of carbon monoxide in the kettle at 0.5 Mpa, and raise the temperature to 20° C., and the reaction time is 1 h. The solution after the reaction enters the flash tank through cooling, and the pressure of the flash tank is normal pressure, and the gas phase after the flash is recycled, and the liquid phase enters the hydrolysis tower, and the hydrolysis tower is operated at room temperature and normal pressure. Carbonic anhydride is hydrolyzed to produce C9 tertiary carbonic acid and the...

Embodiment 2

[0042] Such as figure 1 As shown, C9 tertiary carbonic acid is synthesized in a Ф30cm reactive distillation column. The reactive distillation column includes Zone I, Zone II, Zone III and Zone IV, with the number of theoretical plates being 40, 32, 5 and 2 respectively, among which Zone I is located at the top of the column, followed by Zone II and Zone III Zone, Zone IV is located at the bottom of the tower and contains the bottom of the tower. First dissolve cobalt oxide in 1-butyl-3-methyl-imidazolium bisulfate ionic liquid (Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences) at a mass ratio of 1:100, and feed metal oxide in the upper part of zone I of reactive distillation column R100# Material / strongly acidic ionic liquid stream 2, feed rate 48.22g / s. CO stream 1 is introduced from the lower part of the II zone of the reactive distillation column R100#, the flow rate is 10NL / s, and the pressure inside the tower is maintained at 0.5Mpa. When the temperatu...

Embodiment 3

[0044] Synthesize C9 tertiary carbonic acid in a Ф30cm reactive distillation tower, and the reaction equipment is the same as in Example 2. First, cuprous oxide is dissolved in pyridine butane sulfonic acid bisulfate ionic liquid at a mass ratio of 1:200, and metal oxide (cuprous oxide) / strongly acidic ions are fed to the upper part of zone I of reactive distillation column R100# Liquid stream 2, feed rate 48.11 g / s. CO stream 1 is introduced from the lower part of the II zone of the reactive distillation column R100#, the flow rate is 10NL / s, and the pressure inside the column is maintained. When the temperature in the I zone is 10°C, the two streams are contacted in countercurrent to produce a strong acidic ionic liquid - Metal carbonyl complex catalysts. The (diisobutylene) olefin stream 3 is passed into the lower part of zone I, the feed rate is 0.35g / s, and the temperature in zone II is kept at 0°C, and diisobutene and carbon monoxide are catalyzed by the strong acidic i...

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Abstract

The invention discloses a tert-carboxylic acid synthesis method. According to the method, olefin and carbon monoxide serve as raw materials, and a tert-carboxylic acid product is obtained through catalyzed synthesis under normal pressure or low pressure in the presence of strongly acidic ionic liquid-metal carbonyl complex catalyst. Corrosion is avoided, catalyst consumption is low, three-waste discharge is low, the tert-carboxylic acid product and the catalyst can be separated easily after reaction ends, and the defects of existing technologies that separation effect is poor and dilute sulphuric acid recovery is hard are overcome.

Description

technical field [0001] The invention relates to a method for synthesizing tertiary carbonic acid, in particular to a method for preparing tertiary carbonic acid under low-pressure conditions by using a reactive distillation column with a modified strongly acidic ionic liquid as a solvent and a catalyst. Background technique [0002] Tertiary carbonic acid is a kind of important chemical raw materials, widely used in the production of polymers, drugs, agricultural chemicals, cosmetics and metal processing fluids and other fields. [0003] In the 1950s, H. Koch and his colleagues in Germany used strong acid catalysts to carbonylate olefins, forming the famous Koch reaction. In the 1960s, Enjay Company and Exxon Company in the United States and Shell Company in the Netherlands all used boron trifluoride as a catalyst to realize the industrial production of tertiary carbonic acid. In the 1970s, the Japanese National Industrial Research Institute improved the Kcoh method to synt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/128C07C51/087C07C51/44
CPCY02P20/584C07C51/087C07C51/44C07C51/54C07C53/128
Inventor 何岩刘军袁帅黎源吕艳红王文姜庆梅
Owner WANHUA CHEM GRP CO LTD
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