Catalyst of hydrogenation synthesis of ethylene glycol from dimethyl oxalate and preparation method of the catalyst

A technology of dimethyl oxalate and catalyst, which is applied in the field of selective hydrogenation catalyst and its preparation, can solve the problems that the life of the catalyst cannot meet the requirements of industrialization, the catalyst reaction temperature and pressure are high, and the heat and power consumption are high, so as to achieve long life and selectivity High performance and good stability

Inactive Publication Date: 2015-08-12
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction temperature and pressure of the above-mentioned catalysts are high, and the selectivity of ethylene glycol is low, which leads to high heat and power consumption and increased by-products. In addition, the copper-based catalysts are prone to grain agglomeration and deactivation, which makes the life of the catalyst difficult to meet the requirements of industrialization.

Method used

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  • Catalyst of hydrogenation synthesis of ethylene glycol from dimethyl oxalate and preparation method of the catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A kind of synthetic method of the catalyst that prepares ethylene glycol by hydrogenation of dimethyl oxalate: its steps are as follows:

[0021] (1) 13.4g copper nitrate, 0.05g neodymium nitrate are dissolved in 43g distilled water respectively, obtain mixed salt solution;

[0022] (2) Add 100 g of ethanol and 70 g of tetraethyl orthosilicate to the mixed salt solution obtained in step (1), mechanically stir the mixed solution and place it in a water bath at 70° C. for 1–2 hours to form a sol-gel; After the gel was aged at room temperature for 24 hours, it was dried in an oven with programmed temperature, at 70°C for 17 hours, then at 90°C for 40 hours, and finally at 120°C for 4 hours;

[0023] (3) The catalyst precursor prepared in step (2) is crushed and screened with a stainless steel sieve for 10-20 mesh;

[0024] (4) preparing 200ml of pH in a beaker is 11 aqueous ammonia solution, then the catalyst precursor screened by step (3) is added in the beaker;

[0025...

Embodiment 2

[0030] Catalyst preparation is the same as in Example 1, except that 0.05g of neodymium nitrate is changed to 0.3g of neodymium nitrate in step (1). Above operation obtains catalyzer, and the content of metal copper in this catalyzer is 13.1% through ICP measurement, and the content of auxiliary agent neodymium is 0.95%, and the specific surface (m) of catalyzer is measured through BET 2 / g) is 453, the pore volume (cm 3 / g) was 0.60.

Embodiment 3

[0032] Catalyst preparation is the same as in Example 1, except that 0.05g of neodymium nitrate is changed to 0.05g of lanthanum nitrate in step (1). Above operation obtains catalyzer, and the content of metal copper in this catalyzer is measured through ICP and is 14.6%, and the content of auxiliary agent lanthanum is 0.12%, and the specific surface (m 2 / g) is 515, the pore volume (cm 3 / g) was 0.81.

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Abstract

The invention provides a catalyst of hydrogenation synthesis of ethylene glycol from dimethyl oxalate and a preparation method of the catalyst, wherein the catalyst is prepared with metal copper as a main active component, lanthanum, cerium, neodymium or samarium as additives and tetraethoxysilane as a silicon source through combination of a sol-gel method, an ammonia evaporation method and a microwave method. In the catalyst, the content of the metal copper is 5-30%, the content of the transition metal additives is 0.05-5%, and the balanced being a carrier, SiO2. The catalyst is 300-550 m<2>/g in specific surface area and is 0.4-1 cm<3>/g in pore volume. When the catalyst is used in a process of producing ethylene glycol from dimethyl oxalate through hydrogenation synthesis, the conversion rate of the dimethyl oxalate can reach not less than 99.5% and the selectivity of ethylene glycol can reach 93-97.6% at a reaction temperature of 180-190 DEG C and under a reaction pressure of 2 MPa. After a service life test for 1000 h, the average conversion rate of the dimethyl oxalate is basically maintained to be 99% and the selectivity of ethylene glycol can reach not less than 96% without any obvious decreasing tendency.

Description

technical field [0001] The invention relates to a selective hydrogenation catalyst and a preparation method thereof, in particular to a catalyst for preparing ethylene glycol (EG) by hydrogenation of dimethyl oxalate (DMO) and a preparation method thereof. Background technique [0002] Ethylene glycol is an important chemical raw material, mainly used in the synthesis of polyester (PET) fibers (polyester), PET bottles, cellophane, adhesives, glyoxal, polyols, explosives and other chemical products, and as antifreeze , Plasticizers, hydraulic fluids, solvents, etc., are widely used in many aspects such as polymer materials, organic synthesis, pharmaceuticals, and spices. In recent years, the world's demand for ethylene glycol has been increasing year by year, especially in my country's domestic production, which is far from meeting the demand. Therefore, how to produce ethylene glycol more economically, more environmentally friendly, and more effectively has become more reali...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/83C07C31/20C07C29/147
CPCY02P20/52
Inventor 姚元根杨德亮林凌杨锦霞孙明玲覃业燕潘鹏斌周张锋
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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