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Method for preparing 1,3-propylene glycol by means of methyl 3-methoxypropionate

A technology of methyl methoxy propionate and methoxy propanol, which is applied in the field of chemical synthesis, can solve problems such as unfavorable industrialization, harsh reaction conditions, and complicated operation, and achieve short synthesis routes, low environmental impact, and high reaction selectivity Good results

Inactive Publication Date: 2018-09-28
深圳市前海博扬研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process has harsh reaction conditions, the separation of product and water involves tower equipment, and the operation is complicated, which is not conducive to industrialization

Method used

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  • Method for preparing 1,3-propylene glycol by means of methyl 3-methoxypropionate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Preparation of hydrogenation catalyst

[0031] Dissolve 1 mole of copper nitrate in water, add 40% sodium hydroxide solution and stir, and ensure that the number of moles of sodium hydroxide is twice that of copper nitrate. Then add silica sol with a concentration of 30% and stir, and the addition amount of silica sol is measured according to the weight content of Cu in the final catalyst being 45%. After the mixture was evenly stirred, it was dried at 90°C for 4 hours, then calcined at 550°C for 5 hours, and pressed into tablets to obtain a hydrogenation catalyst. The pressed tablet is crushed and sieved to obtain a 20-40 mesh supported nano-copper-based catalyst. The catalyst can be reduced for 10 hours in a nitrogen atmosphere containing 5% hydrogen at 300 degrees before use, and the purpose of the reduction is to reduce the copper oxide to the active component of the elemental copper catalyst.

[0032] Reduction reaction principle:

[0033] CuO+H 2 → Cu 2 O+H ...

Embodiment 2

[0047]Preparation of hydrogenation catalyst: the specific method is the same as example 1, except that copper acetate is replaced by copper nitrate, and its advantage is that copper acetate is decomposed into carbon dioxide during high-temperature roasting, while copper nitrate is decomposed into nitrogen dioxide during high-temperature roasting, polluted environment.

[0048] Hydrogenation reaction: the specific method is the same as example 1, and the catalyst prepared by adopting copper acetate is compared with copper nitrate, and the reaction conversion rate and selectivity are not much different.

[0049] Demethylation: the specific method is the same as Example 1

Embodiment 3

[0051] Preparation of hydrogenation catalyst: the specific method is the same as Example 1, except that copper oxalate is used instead of copper nitrate. Copper oxalate is a light blue-green powder at room temperature, soluble in ammonia, almost insoluble in water, ethanol and acetic acid. Therefore, in the catalyst preparation process, it should be prepared in an ammonia water system.

[0052] Its advantage is that copper oxalate decomposes into carbon dioxide during high-temperature roasting, while copper nitrate decomposes into nitrogen dioxide during high-temperature roasting, polluting the environment. However, due to the use of ammonia water, ammonia volatilizes during the drying process, which is not as good as copper acetate from the perspective of environmental protection.

[0053] Hydrogenation reaction: the specific method is the same as Example 1, the hydrogen pressure is 4.0MPa, and the catalyst prepared by adopting copper acetate is compared with copper nitrate,...

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Abstract

The invention provides a method for preparing 1,3-propylene glycol by means of methyl 3-methoxypropionate, and relates to the field of chemical synthesis. Aiming at the problems that for an existing method, the technology condition is high, a reaction is harsh, and operation is complex, methyl 3-methoxypropionate serves as the main raw material, methyl 3-methoxypropionate is obtained through a hydrogenation reaction, demethylation is conducted, and reaction is conducted with hydroiodic acid, a target product 1,3-propylene glycol and methyl iodide are obtained, methyl iodide is subjected to catalytic cracking finally, and hydroiodic acid is obtained, wherein hydroiodic acid is reused in the demethylation process. For the whole scheme, the synthetic route is short, reaction selectivity is good, the cost is low, the yield is high, the quality is high, raw material resources are simple, the method does not refer to high temperature and high pressure, the technology is safe and reliable, operability is high, and the influence on the environment is low.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for preparing 1,3-propanediol by using methyl 3-methoxypropionate. Background technique [0002] 1,3-propanediol is a kind of diol, its structural formula is: [0003] [0004] 1,3-Propanediol is a chemical substance with the molecular formula C 3 h 8 o 2 , can undergo oxidation and esterification reactions, can be miscible with water, and can be miscible with ethanol and ether. It is widely used as an organic solvent in industrial production. It can be used in the synthesis of various drugs, new polyester PTT, pharmaceutical intermediates and new antioxidants. [0005] At present, the synthesis process of 1,3-propanediol is reported internationally. One method is the ethylene oxide carbonylation method of Shell Company; the other method is the acrolein hydration oxidation method of Degussa Company. Among them, the equipment investment of the ethylene oxide car...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/10C07C31/20C01B7/13
CPCC01B7/135C07C29/10C07C41/26C07C31/205C07C43/13
Inventor 董研徐辑亮肖增钧肖阳傅兵
Owner 深圳市前海博扬研究院有限公司
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