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Copper-hydroxyapatite catalyst for synthesizing methyl glycolate and ethylene glycol and preparation method thereof

A kind of technology of methyl glycolate and hydroxyapatite, applied in the field of chemical industry

Inactive Publication Date: 2013-03-27
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis of methyl glycolate and ethylene glycol by hydrogenation of dimethyl oxalate has the characteristics of environmental protection, economy and energy saving, etc., but most of the catalysts reported in the literature can only achieve one of the products of methyl glycolate or ethylene glycol How to efficiently select and synthesize two different products at the same time by changing the reaction conditions on the same catalyst has important practical significance for the industrial production of methyl glycolate and ethylene glycol

Method used

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  • Copper-hydroxyapatite catalyst for synthesizing methyl glycolate and ethylene glycol and preparation method thereof
  • Copper-hydroxyapatite catalyst for synthesizing methyl glycolate and ethylene glycol and preparation method thereof
  • Copper-hydroxyapatite catalyst for synthesizing methyl glycolate and ethylene glycol and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: Preparation of carrier hydroxyapatite

[0021] 23.52 g Ca(NO 3 ) 2 4H 2 O was dissolved in 300 mL water, and the pH was adjusted to 11~12 with ammonia water to make a calcium nitrate solution (about 0.33 M), and 200 mL containing 7.89 g (NH 4 ) 2 HPO 4 The aqueous solution (about 0.30 M, Ca / P=1.67 (mol / mol)) was slowly dropped into the above calcium nitrate solution, and stirred and heated at 50°C for 16 h to obtain a suspension containing apatite carrier for use. The mass fraction of hydroxyapatite in the suspension is about 2%.

[0022] Active metal copper and auxiliary metal loading: 13.10 g Cu(NO 3 ) 2 ·3H 2 O and 3.01 g Fe(NO 3 ) 3 9H 2 Add O to the carrier suspension at the same time, adjust the pH of the suspension to 11~12 with ammonia water, stir and react in a water bath at 30°C for 14 hours, then increase the temperature of the water bath, and continue stirring at 80°C until the suspension The pH value is 9~10, the reaction is stopped, ...

Embodiment 2

[0024] Example 2: Preparation of carrier hydroxyapatite

[0025] 23.52 g Ca(NO 3 ) 2 4H 2 O was dissolved in 300 mL of water, and the pH was adjusted to 11~12 with ammonia water to make a calcium nitrate solution (about 0.33 M), and 200 mL containing 4.39 g (NH 4 ) 2 HPO 4 The aqueous solution (about 0.20 M, Ca / P=3.0 (mol / mol)) was slowly dropped into the above calcium nitrate solution, and stirred and heated at 50°C for 16 h to obtain a suspension containing apatite carrier for use. The mass fraction of hydroxyapatite in the suspension is about 2%.

[0026] Active metal copper and auxiliary metal loading: 13.10 g Cu(NO 3 ) 2 ·3H 2 O and 7.56 g Mn(NO 3 ) 2 4H 2 Add O to the suspension containing the carrier hydroxyapatite at the same time, adjust the pH of the suspension to 10~11 with ammonia water, stir and react in a water bath at 50 °C for 6 h, increase the temperature of the water bath, and continue to stir and react at 80 °C , until the pH value of the suspens...

Embodiment 3

[0028] Embodiment 3: The preparation of carrier hydroxyapatite is the same as that in Embodiment 1.

[0029] Active metal copper and auxiliary metal loading: 13.10 g Cu(NO 3 ) 2 ·3H 2 O and 1.91 g Zn(NO 3 ) 2 ·6H 2 Add O to the suspension containing the carrier hydroxyapatite at the same time, adjust the pH of the suspension to 11~12 with ammonia water, stir and react in a water bath at 50°C for 6 h, increase the temperature of the water bath, and continue to stir and react at 80°C , until the pH value of the suspension is 7~7.5, stop the reaction, obtain the suspension containing the catalyst, then filter it, wash it with deionized water for 5 times, bake the filter cake at 120°C, and put it in a muffle furnace for 10 °C / min, the temperature was raised to 600 °C and kept for 5 h to obtain catalyst powder.

[0030] Activity evaluation is the same as in Example 1.

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Abstract

The invention belongs to the technical field of chemical industry, and particularly relates to an efficient catalyst for synthesizing methyl glycolate and ethylene glycol through gas-phase catalytic hydrogenation of dimethyl oxalate and a preparation method thereof. The catalyst is loaded with copper and other auxiliary metals by taking hydroxyapatite as a carrier. The preparation method of the catalyst comprises the following steps of: firstly preparing a hydroxyapatite suspension from calcium nitrate and diammonium hydrogen phosphate; adding soluble copper salt and soluble auxiliary metal slat, and performing metal loading by an ammonia distillation method; filtering; washing and drying the filter cake; and roasting to obtain a powdery catalyst for the gas-phase catalytic hydrogenation of dimethyl oxalate. Through the invention, controllable selectivity is realized on the hydrogenation products including methyl glycolate and ethylene glycol, the yield of methyl glycolate can reach 80% under low-temperature conditions, and the yield of ethylene glycol can reach 99% under high-temperature conditions; and the preparation method of the catalyst is simple and has good stability and relatively broad prospects in industrial application.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a copper-based catalyst for preparing methyl glycolate and ethylene glycol by gas-phase catalytic hydrogenation of dimethyl oxalate and a preparation method thereof. Background technique [0002] Methyl glycolate, also known as methyl glycolate or methyl glycolate, has both the chemical properties of alcohol and ester because its molecule contains α-H, hydroxyl and ester groups. Methyl glycolate is an important intermediate for synthesizing isotricapine and its analogs with anticancer activity, and it is also a raw material for synthesizing some carrier additives that improve the pressure resistance and wear resistance of lubricating oil. In addition, a series of high value-added downstream products can be synthesized from methyl glycolate, such as catalytic hydrogenation to produce ethylene glycol, hydrolysis to produce glycolic acid, carbonylation to produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/18B01J27/185B01J27/187C07C27/04C07C29/149C07C31/20C07C67/31C07C69/675
CPCY02P20/52
Inventor 戴维林温超范康年
Owner FUDAN UNIV
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