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Heat-insulation reaction system and process for preparing glycolate through oxalate hydrogenation

An adiabatic reaction, glycolic acid ester technology, applied in the preparation of carboxylate, the preparation of organic compounds, organic chemistry and other directions, can solve the problems of inappropriate proportion of hot materials, insufficient utilization of catalysts, uneven mixing and air flow, etc. Achieve the effect of improving conversion rate, inhibiting side reactions and reducing energy consumption

Active Publication Date: 2016-02-24
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in actual industrial production, there is often an inappropriate proportioning ratio between the cold shock material injected between the stages and the hot material reacted in the upper stage, and the material mixing and air flow between the stages in the reactor are not uniform, so that the catalyst cannot be fully utilized, resulting in product selection. low sex problem

Method used

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  • Heat-insulation reaction system and process for preparing glycolate through oxalate hydrogenation
  • Heat-insulation reaction system and process for preparing glycolate through oxalate hydrogenation
  • Heat-insulation reaction system and process for preparing glycolate through oxalate hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The process of using a single-layer axial adiabatic fixed-bed reactor figure 1 Shown. The hydrogenation reactor is a cylindrical body with an inner diameter of 160 mm and a height of 600 mm. Load 4LAg / SiO in the middle of the hydrogenation reactor 2 The catalyst is filled with stainless steel magnetic rings with the same particle size at the top and bottom, diethyl oxalate is used as the raw material, the reaction pressure is set to 3.0Mpa, and the molar ratio of hydrogen to oxalate in the hydrogenation reactor inlet is 120.

[0029] Hydrogen mixed gas 1 (hydrogen: 95v%, ethanol: 4v%, the rest is inert gas), flow rate 30Nm3 / h, temperature 84°C, pressure 3.12MPa(A), preheated to 152°C by circulating gas preheater E1 The hot stream 2 enters the vaporization tower T1, and is mixed with the raw material oxalate liquid 8 at a temperature of 160°C, and the liquid raw material feed rate is 1.55 kg / h to vaporize the liquid oxalate. The vaporized oxalate ester steam and hydrogen m...

Embodiment 2

[0031] The process of using a single-layer axial adiabatic fixed-bed reactor figure 1 Shown. The reactor is a cylindrical body with an inner diameter of 160 mm and a height of 600 mm. The 4LAg / SiO2 catalyst is filled in the middle of the hydrogenation reactor, and the upper and lower parts are filled with stainless steel magnetic rings with the same particle size. Diethyl oxalate is used as the raw material. The reaction pressure is set to 3.0MPa. The hydrogen and oxalate are in the inlet of the reactor. The molar ratio is 80.

[0032] Hydrogen mixed gas 1 (hydrogen: 95v%, ethanol: 4v%, the rest is inert gas), flow rate 20Nm3 / h, temperature 84°C, pressure 3.12MPa(A), preheated to 168°C by circulating gas preheater E1 The hot stream 2 enters the vaporization tower T1, and is mixed with the raw material oxalate liquid 8 at a temperature of 160°C. The liquid raw material feed rate is 1.55 kg / h to vaporize the liquid oxalate. The vaporized steam and hydrogen mixed gas 1 form a mixt...

Embodiment 3

[0034] The process of using a single-layer radial adiabatic fixed-bed reactor is as follows: figure 1 As shown, see the reactor type image 3 . The reactor is a cylindrical body with an inner diameter of 200mm and a height of 600mm. The catalyst is packed in an annulus formed by concentric circles. The gas is blown out by the distributor and passes through the catalyst bed in the radial direction. The 4LAg / SiO2 catalyst is loaded in the middle of the hydrogenation reactor, and the upper and lower parts are filled with stainless steel magnetic rings of equivalent particle size. Diethyl oxalate is used as the raw material. The reaction pressure is set to 3.0Mpa. The molar ratio of the acid ester is 100. The specific reaction process is the same as in Example 1.

[0035] The composition and mass fraction of the product are: ethanol 32.3%, ethyl acetate 1.00%, water 0.55%, ethylene glycol monoethyl ether 0.18%, ethyl glycolate 65.3%, ethylene glycol 0.54%, and others 0.13%. The co...

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Abstract

The invention relates to a heat-insulation reaction system for preparing glycolate through oxalate hydrogenation, belonging to the technical field of glycolate preparation. The system comprises a circulating gas preheater, a vaporization tower, a reaction gas preheater and a hydrogenation reactor communicated in sequence, wherein an outlet of the hydrogenation reaction is communicated with the reaction gas preheater, and the reaction gas preheater is communicated with the circulating gas preheater. The invention also relates to a process for preparing glycolate by using the heat-insulation reaction system. By using the system and process disclosed by the invention, the exothermic reaction temperature rise can be favorably controlled, side reaction can be inhibited, the activity of a catalyst can be improved, the service life of the catalyst can be prolonged, the problems of low oxalate conversion rate, low selectivity of glycolate serving as a product and the like are solved, and the energy consumption is reduced because heating is realized by virtue of system reaction heat. The heat-insulation reaction system and process for preparing glycolate through oxalate hydrogenation have the advantages that the oxalate conversion rate is high, the selectivity of glycolate serving as the product is high, waste heat of the system can be sufficiently utilized, and the energy consumption and the cost can be reduced.

Description

Technical field [0001] The invention belongs to the technical field of glycolic acid ester preparation, and specifically relates to an adiabatic reaction system and process for preparing glycolic acid ester by hydrogenation of oxalic acid ester. Background technique [0002] Glycolic acid ester is an important chemical product, which is widely used in many fields such as chemical industry, medicine, pesticide, feed, dye and perfume. Such as improved solvents for fibers, resins and rubber; hydrogenation to produce ethylene glycol, carbonylation to produce malonate, aminolysis to produce glycine, and hydrolysis to produce glycolic acid. At present, foreign technology mainly adopts formaldehyde carbonylation route to prepare glycolic acid esters, but formaldehyde carbonylation technology requires high-pressure conditions, and will cause huge corrosion, high equipment requirements, large investment, and difficult industrial production. In China, the process route of re-esterificatio...

Claims

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Application Information

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IPC IPC(8): C07C69/675C07C67/31
CPCC07C67/31C07C69/675
Inventor 胡玉容范鑫李扬王科袁小金夏伟许红云董玲玉
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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