Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Catalyst used for hydrogenation of oxalate for preparing ethylene glycol and preparation method thereof

A catalyst and ethylene glycol technology, applied in chemical instruments and methods, preparation of hydroxyl compounds, organic compounds, etc., can solve pollution hazards and other problems, achieve environmental friendliness, enhance anti-sintering ability, high activity and ethylene glycol selective effect

Active Publication Date: 2012-08-22
TIANJIN UNIV +1
View PDF7 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since Cr is extremely harmful to human body and environmental pollution, the research on Cr-free catalysts has gradually become the research trend of oxalate hydrogenation catalysts.

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

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Catalyst used for hydrogenation of oxalate for preparing ethylene glycol and preparation method thereof
  • Catalyst used for hydrogenation of oxalate for preparing ethylene glycol and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Preparation of Zirconium Glue

[0032] Weighing 30g Zr(NO 3 ) 4 ·5H 2 O was added to a 200ml beaker, and 100ml of 70% nitric acid was added to dissolve it and adjust the Zr(NO 3 ) 4 The concentration is 2M. Under the stirring state, ammonia water was slowly added dropwise in the solution until the pH was 4.0-5.0, at this time Zr(NO 3 ) 4 The solution is transformed into a translucent zirconium sol, and deionized water is added to adjust the concentration of the zirconium sol to 1 mol / L, and then aged under air atmosphere for 24-48 hours with stirring.

[0033] Catalyst preparation

[0034] Weigh 15.25g of copper nitrate pentahydrate and dissolve it in 120ml of water, slowly add 52ml of 25% ammonia water to dissolve it and mix well. The zirconium colloid and silica sol (silicon oxide content is 30wt. %) prepared before are added dropwise in this solution, and the volumes of zirconium colloid and silica sol are respectively 113ml and 6ml. The temperature is then ...

Embodiment 2

[0048] Preparation of Zirconium Glue

[0049] Zirconium glue preparation method is the same as embodiment 1

[0050] Catalyst preparation

[0051] Weigh 15.25g of copper nitrate pentahydrate and dissolve it in 100ml of water, slowly add 52ml of 25% ammonia water to dissolve it and mix well. 113ml of the previously prepared zirconium glue was added dropwise to the solution, and after the dropwise addition was completed, it was aged for 2 hours under stirring. A total of 6ml of silica sol was added dropwise to the above-mentioned material, and after the dropwise addition was completed, it was aged for 2 hours under stirring. Then the temperature is raised to 95°C to precipitate copper, zirconia and silicon oxide. The precipitate was filtered, washed three times with deionized water, dried at 120°C for 12 hours, and calcined at 450°C for 4 hours to form a copper content of 20wt.%, SiO 2 10wt.% Cu / ZrO 2 / SiO 2 Catalyst ready for use.

[0052] Catalyst evaluation

[0053] T...

Embodiment 3

[0055] Preparation of Zirconium Glue

[0056] Weighing 12.0g Zr(OH) 4 Add it into a 200ml beaker and add water to make a suspension, slowly add nitric acid dropwise under stirring to dissolve it, add ammonia water dropwise until the pH is 4.0-5.0, at this time a translucent zirconium sol is formed, add deionized water to adjust the zirconium The concentration of the sol is 1 mol / L, and then it is stirred and aged in an air atmosphere for 24-48 hours before use.

[0057] Catalyst preparation

[0058] Other is the same as embodiment 1, but adopts the zirconium sol prepared in the present embodiment to replace with Zr(NO 3 ) 4 ·5H 2 O is the zirconium sol prepared by raw material to obtain copper content of 20wt.%, SiO 2 10wt.% Cu / SiO 2 / ZrO 2 Catalyst ready for use.

[0059] Catalyst evaluation

[0060] The catalyst evaluation method is the same as in Example 1, and the results are shown in Table 1.

[0061] Table 1 Cu / SiO prepared using different methods and precursor...

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 invention relates to a catalyst used for hydrogenation of oxalate for preparing ethylene glycol and a preparation method thereof. The catalyst comprises copper, an auxiliary agent and zirconia serving as active ingredients and is characterized in that: the auxiliary agent is one or more of Al2O3, SiO2, TiO2, BaO, La2O3, MnO and ZnO; the active ingredients account for 10 to 45 percent of the weight of the catalyst; the zirconia accounts for 1 to 85 percent of the weight of the catalyst; and the auxiliary agent accounts for 5 to 80 percent of the weight of the catalyst. By using a more stable chemical structure formed by hydroxy of zirconium sol, the copper and other auxiliary agents, the specific surface area and pore size distribution of the catalyst are improved, the copper has high dispersion degree, and the anti-sintering capacity of the copper catalyst is also enhanced at the same time. The catalyst can stably run for over 3,200 hours in a skill-up test in the hydrogenation ofthe oxalate for preparing 300ml of ethylene glycol; the average conversion rate of the oxalate is over 99.9 percent; and the average yield of the ethylene glycol reaches over 94 percent.

Description

technical field [0001] The invention relates to a catalyst and a preparation method for oxalate hydrogenation to ethylene glycol, the catalyst chemical formula is Cu / MO x / ZrO 2 . Among them, copper is the main active component of the catalyst, MO x Composed of main group metal or transition metal oxide, zirconium oxide in the form of zirconium sol and the precursor of the auxiliary agent are added to the copper precursor solution in a step-by-step or synchronous way to finally prepare the catalyst. This preparation method helps to promote high dispersion and thermal stability of the active component copper. The catalyst can be used for gas-phase hydrogenation of oxalate to produce ethylene glycol in a fixed-bed catalytic reactor and can obtain higher ethylene glycol selectivity and yield. Background technique [0002] Ethylene glycol is an important basic organic raw material. Ethylene glycol was first produced by Wurtz in 1859 by hydrolyzing ethylene glycol diacetate ...

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 Patents(China)
IPC IPC(8): B01J23/76B01J23/889B01J23/83C07C31/20C07C29/149
CPCY02P20/52
Inventor 马新宾赵玉军王胜平赵国杰余铭程吕静王保伟李振花
Owner TIANJIN UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com