Method of measuring water phase C4 alcohols in isoprene synthesis industry (olefin aldehyde method)

A technology of isoprene and carbon tetraol, applied in the field of analytical chemistry, can solve problems such as complex composition and achieve accurate results

Inactive Publication Date: 2018-03-16
SHANDONG YUHUANG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This just makes the component composition in the water phase extremely complicated, how under this complex condition, accurately measure the content of carbon tetraol in the water phase, relevant patent has not yet reported

Method used

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  • Method of measuring water phase C4 alcohols in isoprene synthesis industry (olefin aldehyde method)

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Since the mass concentration of tert-butanol in the water phase generally does not exceed 10% under actual conditions, a tert-butanol solution with a concentration range of 0-10% was prepared, and the concentration was attached to the concentration by its peak area percentage. figure 1 . Depend on figure 1 It can be seen that the fitting curve is a straight line, and the coefficient of determination R 2 It is 0.9994, and the fitting degree is good.

[0023] Take 192g of 85wt% tert-butanol solution, 30g of 37wt% formaldehyde solution, and 30g of 88wt% phosphoric acid solution, mix the three evenly, and inject the mixed solution into the tubular reactor with a precision metering pump. The reaction temperature is 170°C and the pressure is 1.4MPa. The residence time was 20 minutes, and the obtained product was extracted with n-heptane. The oil phase was located in the upper layer, and the water phase was located in the lower layer. The yield of isoprene was 69%, and 325 g...

Embodiment 2

[0025] Take 180g of 85wt% tert-butanol solution, 41g of 37wt% formaldehyde solution, and 28g of 88wt% phosphoric acid solution, mix the three evenly, and inject the mixed solution into the tubular reactor with a precision metering pump. The reaction temperature is 160°C and the pressure is 1.0MPa. The residence time was 20 minutes, and the obtained product was extracted with n-heptane. The oil phase was located in the upper layer, and the water phase was located in the lower layer. The yield of isoprene was 59%, and 244 g of the aqueous phase containing tert-butanol was obtained. Take 90 g of the aqueous phase, add sodium carbonate solution, adjust the pH to 9, and distill under reduced pressure at a water bath temperature of 55°C to obtain a colorless and clear solution. Analyzed by gas chromatography, it was calculated that the mass of tert-butanol in the water phase was 4.39g, and the concentration was 4.88%.

Embodiment 3

[0027] Take 150g of 85wt% tert-butanol solution, 47g of 37wt% formaldehyde solution, and 23g of 88wt% phosphoric acid solution, mix the three evenly, and inject the mixed solution into the tubular reactor with a precision metering pump. The reaction temperature is 175°C and the pressure is 1.0MPa. The residence time was 30 min, and the obtained product was extracted with n-heptane. The oil phase was located in the upper layer, and the water phase was located in the lower layer. The yield of isoprene was 53%, and 232 g of the aqueous phase containing tert-butanol was obtained. Take 100 g of the aqueous phase, add potassium bicarbonate solution, adjust the pH to 8, and distill under reduced pressure at a water bath temperature of 60°C to obtain a colorless and clear solution. Analyzed by gas chromatography, it was calculated that the mass of tert-butanol in the water phase was 3.68g, and the concentration was 3.68%.

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Abstract

The invention relates to the technical field of analytic chemistry, and especially relates to a method of measuring water phase C4 alcohols in the isoprene synthesis industry (olefin aldehyde method).The method is characterized in that a C4 alcohol containing water phase is taken as the processing object; an alkaline solution is added into the water phase to adjust the pH value to 8-14, precipitates are generated in the solution; through distillation, the C4 alcohol containing water phase is separated from a precipitating agent, excess alkalis, and soluble acidic salts generated during the process of acid-base neutralization; and finally gas chromatography is used to measure the accurate content of C4 alcohols in the water phase through an external standard method. The method is simple and easy to perform, the results are accurate, the influence of acid catalysts and multiple metal ions in the water phase on C4 alcohol measurement is eliminated, and the method is suitable for popularization and application.

Description

(1) Technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a method for measuring water-phase carbon tetraol in the industry of synthesizing isoprene by enal method. (2) Background technology [0002] Isoprene is an important raw material for the production of isoprene rubber. Isoprene rubber is used more and more widely because its structure and properties are close to natural rubber. The current production methods of isoprene include C5 fraction extraction distillation method, dehydrogenation method, and chemical synthesis method, wherein chemical synthesis method includes isobutylene-formaldehyde method, acetylene-acetone method, and propylene dimerization method. The acetylene-acetone method and the propylene dimerization method have long been used. The enaldehyde method is the most important isoprene synthesis method, which has been industrialized in Russia and Japan. [0003] The alkenal method can be divided into...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/12
CPCG01N30/02G01N30/12G01N2030/047G01N2030/067G01N2030/122
Inventor 景文赵存胜肖博崔春生侯红霞王建伟王胜伟
Owner SHANDONG YUHUANG CHEM CO LTD
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