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Catalyzer for oxalic ester hydrogenation synthesizing of glycolate and method of preparing the same

A glycolic acid ester and catalyst technology, which is applied in the field of glycolic acid ester preparation, can solve environmental problems and other problems, and achieve the effects of easy control, stable reaction performance, and long life

Active Publication Date: 2008-03-12
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of Cr / Cu catalysts in gas-phase catalytic hydrogenation of oxalate poses environmental concerns

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take by weighing two parts of silica sol 100g carrier, one part is modified (recorded as SiO 2 (M)), one unmodified (denoted as SiO 2 (W). According to 15wt%Cu+5wt%Ag / SiO 2 content preparation catalyst, the steps are as follows: select copper nitrate, prepare impregnation solution according to the Cu loading amount, prepare the impregnation solution according to the loading amount, and prepare the modified SiO 2 After the carrier was soaked in the solution for 24 hours, it was vacuum-dried for 8 hours to obtain a solid. Select Ag(NO 3 ) 3 , according to the loading of Ag, the impregnating solution is prepared. In order to prevent metal ions from being hydrolyzed to form hydroxides or oxides, a small amount of nitric acid is added to the impregnating solution to make the pH of the impregnating solution = 5-6, and then the above solids are in the impregnating solution. Soak for 10 hours, dry it in a water bath to become a solid after fully absorbed, then dry the soli...

Embodiment 2

[0017] Weigh two parts of 100g modified silica sol carrier, according to 20wt%Cu+6wt%Ag / SiO 2 Content preparation catalyst, its steps are as follows: select cupric chloride, prepare impregnating liquid according to Cu loading amount, load amount is formulated into impregnating liquid, after immersing the prepared modified silica sol carrier in this solution for 10 hours, vacuum-dry for 6 hours. hours to get solids. Select Ag(NO 3 ) 3 , according to the loading capacity of Ag, the impregnating solution was formulated. In order to prevent metal ions from being hydrolyzed to form hydroxide or oxide precipitation, a small amount of nitric acid was added to the impregnating solution to make the pH of the impregnating solution = 6.5, and then the modified silica sol carrier was impregnated Soak in the liquid for 10 hours, dry it in a water bath after being fully absorbed, and then dry the solid at 120°C for 6 hours, and roast it at 500°C for 6 hours, and use nitrogen and hydrogen ...

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Abstract

A catalyst for hydrogenated synthesis of glycollate with oxalate and a preparation method for the catalyst belong to the glycollate preparation technical field. The catalyst of the present invention uses the copper metal as the main active component, and silver as the promoter, and is manufactured with the method of immersion. A carrier of the catalyst is the modified silica sol. The select content of the copper metal is 5 to 45 percent of the carrier weight, and the optimal content of the copper metal is 10 to 40 percent. The content of silver metal is 0.1 to 15 percent of the carrier weight, and the optimal content of silver metal is 1 to 8.0 percent. The select carrier is the silica sol with a double peak pore distribution structure and the specific surface area of the carrier is 100-300m2 / g; and the optimal specific surface area of the carrier is 120-240m2 / g. The present invention settles the problem of applying a Cr / Cu catalyst in the oxalate gas-phase catalytic hydrogenation. Proven by experiments, the catalyst is provided with the very high reaction activity and glycollate selectivity in the reaction to synthesize glycollate with oxalate and hydrogen Moreover, the catalyst is provided with the long usable life and the stable reaction performance, and can be easily controlled.

Description

technical field [0001] The invention belongs to the technical field of glycolate ester preparation, and further relates to a catalyst for hydrogenating oxalate to synthesize glycolate and a preparation method thereof. Background technique [0002] Glycolate has its unique molecular structure: it has α-H, hydroxyl and ester functional groups at the same time, which makes it have the chemical properties of alcohol and ester, and can undergo carbonylation reaction, hydrolysis reaction, oxidation reaction, etc., and has become an important Chemical raw materials. Glycolate is an excellent solvent for many celluloses, resins, and rubbers. Its downstream products such as glycolic acid, glycine, dimethyl malonate and glyoxylic acid also have extensive application value. [0003] At present, there is no mature production process of environmentally friendly glycolic acid ester in China. It is still produced by the chloroacetic acid method, and the process is to mix and stir the ch...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C69/675C07C67/31
Inventor 王保伟张旭马新宾许根慧
Owner TIANJIN UNIV
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