Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for controlling the catalytic hydrogenation of 1,4-butynediol via the content of co and/or ch4 in the exhaust gas stream

A waste gas flow and content technology, applied in chemical instruments and methods, hydrogenation preparation, preparation of organic compounds, etc.

Inactive Publication Date: 2020-05-01
BASF SE
View PDF22 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Furthermore, complex off-line measurements of the butanol concentration of the hydrogenation output are required

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0123] Embodiment 1: (measure CO content and control by reducing the substrate load per unit catalyst)

[0124] 100g of Raney nickel-molybdenum catalyst was charged into a 2L autoclave filled to 1L and heated to 160°C while stirring and injecting H 2 to 45 bar. An approximately 50% by weight aqueous butynediol solution is operated into the autoclave at a feed rate of 800 to 1000 g (butynediol solution) / h, and a correspondingly high product flow rate is withdrawn from the reactor. h 2 Feed rate with about 2.2 moles of H per mole of butynediol 2 correspond. After about 400 hours of operation at a feed rate of 800 g (butynediol solution) / h, about 60 ppm of CO, 1600 ppm of CO were found in the exhaust gas 2 and 14% by volume of CH 4 . GC analysis of the liquid gave 1.54% Methanol, 1.26% Propanol, 0.94% Butanol, 95% 1,4-Butanediol (BDO), 1000 ppm at a pH of 7.2 and an APHA value of 120 (measured according to ASTM D1209) 2-methyl-1,4-butanediol (MBDO), 310 ppm acetal and 130 ...

Embodiment 2

[0125] Embodiment 2 (hydrogenated butynediol, measure CH 4 content and control by reducing the hydrogenation temperature)

[0126] The reaction conditions correspond to those in Example 1. The butynediol feed rate was 900 g (butynediol solution) / h. On the first day, at a temperature of 160 °C, the amount of methane in the exhaust gas was 30% by volume, while the CO content in the exhaust gas was 0.1 ppm. The propanol content in the product was 2%. After a temperature drop of 10° C., the methane content in the exhaust gas can be reduced to 15% by volume. At the same time, the propanol content in the product dropped to 1.5%, and thus the butanediol content rose from 95% to 95.5%. The remainder consists essentially of methanol (from formaldehyde), butanol, GBL, and other by-products.

Embodiment 3

[0127] Example 3 (hydrogenation of butynediol, measurement of CO content and control by temperature increase)

[0128] The reaction conditions correspond to those in Example 2. At a temperature of 150° C., the butynediol feed rate was 900 g (butynediol solution) / h. After 300 hours of operation, the CO content in the exhaust gas increased from 0.1 ppm to 170 ppm, while CH 4 The content was reduced from 15% by volume to 11% by volume. The butenediol content in the output increased from <5 ppm to 140 ppm and the acetal content increased from 300 ppm to 600 ppm. After the temperature had increased from 150° C. to 152° C., the CO content in the exhaust gas decreased from 170 ppm to 30 ppm, while the methane content increased from 11 to 12 vol. %. The butenediol content in the output was reduced from 140 ppm to 10 ppm and the acetal content from 600 ppm to 250 ppm. Once the limit of 170 ppm for CO in the exhaust gas is exceeded, the temperature increases by 2 °C.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The present invention relates to a method for producing 1,4-butanediol by catalytic hydrogenation of 1,4-butynediol in a reaction zone with hydrogen in the presence of a heterogeneous hydrogenation catalyst, in which method the content of at least one gas in the exhaust gas stream, selected from CO and CH4, is measured and the content of the measured gas in the exhaust gas stream is used for controlling the hydrogenation.

Description

[0001] Background of the invention [0002] The present invention relates to a process for the preparation of 1,4-butanediol by catalytic hydrogenation of 1,4-butynediol with hydrogen in a reaction zone in the presence of a heterogeneous hydrogenation catalyst, wherein at least one selected from CO and CH in the exhaust stream 4 and using the gas content measured in the off-gas stream to control the hydrogenation in a closed loop. [0003] current technology [0004] In the chemical industry, catalytic hydrogenation is one of the most important reactions for producing chemical products. The hydrogenation is preferably carried out in the presence of a heterogeneous catalyst, which, in contrast to a homogeneous catalyst, is easier to separate from the reaction mixture. A very important process on an industrial scale is the hydrogenation of butynediol to butanediol. Butanediol is used to prepare tetrahydrofuran (THF), polyTHF, polyester, etc. The hydrogenation of butynediol to...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/17
CPCC07C29/172C07C31/207
Inventor R·萍克斯J·韦古尼J·巴尔达姆斯M·施瓦茨
Owner BASF SE