Preparation method of delta-valerolactone

A technology of valerolactone and alkyl acetate, which is applied in the field of preparation of δ-valerolactone, can solve problems such as disastrous consequences, difficulty in obtaining, sensitive reaction conditions, etc., achieve good physical properties, avoid safety hazards, and react The effect of mild conditions

Active Publication Date: 2019-04-19
WANHUA CHEM GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wherein in the Baeyer-Villiger oxidation reaction, cyclopentanone is limited to petrochemical products, and the source of raw materials is narrow; Oxidation, because organic peroxyacids are expensive and the by-product organic acids produced after the reaction pollute the environment, post-treatment requires a large amount of alkaline reagents such as sodium carbonate, which will undoubtedly increase production costs
In addition, due to the existence of peroxides, if misoperation occurs in the reaction process, it may lead to disastrous consequences. Therefore, the preparation of valerolactone by Baeyer-Villiger method has not been widely used in industry.
In the method of dehydrogenating 1,5-pentanediol as a raw material to generate δ-valerolactone, the by-product n-valeric acid in the reaction product corrodes the reactor, increases the input cost of the reaction equipment, and is difficult to separate the product
[0007] It can be seen that the existing methods cannot meet the demand of industrial mass production of high-quality δ-valerolactone
Therefore need to seek a kind of preparation method of the delta-valerolactone that is suitable for industrialized production, be used to solve low product yield in the prior art, raw material source is limited difficult to obtain and expensive and reaction conditions are sensitive and difficult to control, safety factor is low And other issues

Method used

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  • Preparation method of delta-valerolactone
  • Preparation method of delta-valerolactone
  • Preparation method of delta-valerolactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Catalyst preparation:

[0051] Weigh 102g of Al 2 o 3 (1mol), mix it with 100ml of aqueous urea (CO(NH 2 ) 2 : 0.005mol) mixed evenly, placed in a 2L autogenous autoclave, kept at 90°C for 24h, then added 700ml of Mg(NO 3 ) 2 (0.02mol) aqueous solution, and heated up to 130°C, kept for 24h, washed with deionized water, dried at 120°C, and then roasted at 450°C for 8h to obtain LDHs-modified alumina composite MaterialLDHs-Al 2 o 3 .

[0052] Prepare a certain concentration of sodium phosphate (wherein the amount of sodium phosphate substance is 0.1mol) aqueous solution, then 100g of the LDHs-Al prepared above 2 o 3 Put it into the sodium phosphate aqueous solution, shake it well, put it into the constant temperature oscillator in the water bath for 24 hours, keep the temperature of the water bath at about 70°C during this period, and the shaking rate is 130-140r / min. Then keep this temperature and continue to shake, add dropwise lithium chloride aqueous solutio...

Embodiment 2

[0062] Catalyst preparation:

[0063] With embodiment 1, difference is that alkaline substance CO(NH 2 ) 2 The dosage is 0.014mol, Mg(NO 3 ) 2 The dosage is 0.08mol, the dosage of sodium phosphate is 0.58mol, the dosage of lithium chloride is 1.77mol, the prepared catalyst is 166.53g, and the loading capacity of the active component lithium phosphate is 39.95%.

[0064] Preparation of δ-valerolactone:

[0065] Reactor and catalyst loading mode, loading amount are the same as embodiment 1.

[0066] Keep the reaction section of the catalytic rectification tower and the jacket temperature of the stripping section at 250°C, and continuously feed ethyl acetate and propylene oxide through the feed pump, wherein the liquid space velocity of propylene oxide WHSV=5.0g / gcat / h, acetic acid The molar ratio of ethyl ester to propylene oxide is 1.05:1, and the reflux ratio of the catalytic rectification tower is 10. The feed in the tower is used, and low-boiling compounds such as ethan...

Embodiment 3

[0072] Catalyst preparation:

[0073] With embodiment 1, difference is that alkaline substance CO(NH 2 ) 2 The dosage is 0.01mol, Mg(NO 3 ) 2 The dosage is 0.05mol, the dosage of sodium phosphate is 0.39mol, the dosage of lithium chloride is 1.18mol, the prepared catalyst is 145.07g, and the loading capacity of the active component lithium phosphate is 31.07%.

[0074] Preparation of δ-valerolactone:

[0075] Reactor and catalyst loading mode, loading amount are the same as embodiment 1.

[0076] Keep the reaction section of the catalytic rectification tower and the jacket temperature of the stripping section at 215°C, continuously feed propyl acetate and propylene oxide through the feed pump, wherein the liquid space velocity of propylene oxide WHSV=3.0g / gcat / h, acetic acid The molar ratio of methyl ester to propylene oxide is 1.03:1, the reflux ratio of the catalytic rectification tower is 5, the feed in the tower is adopted, the low boiling point compounds such as prop...

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Abstract

The invention relates to a preparation method of delta-valerolactone. The preparation method comprises the following steps: alkyl acetate and propylene oxide are subjected to an isomeric addition cyclization reaction in the presence of a catalyst, and the delta-valerolactone is obtained by one step, wherein the catalyst is a supported catalyst; a carrier is aluminium oxide; and the active component is lithium phosphate. The process has the following advantages: the raw materials are easily available; the reaction steps are simple; environmental pollution is less; yield is high; and the productis easy to purify. The preparation method is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of δ-valerolactone, which belongs to the field of organic synthesis. Background technique [0002] δ-valerolactone, also known as 1,5-valerolactone, delta-valerolactone, tetrahydro-2H-2-pyrone, tetrahydro-o-pyrone, tetrahydrocoumarin, the English name is δ -Valerolactone, abbreviated as DVL, is a cyclic lactone compound similar to caprolactone, with a molecular weight of 100.12, a boiling point of 230°C, and a molecular formula of C 5 h 8 o 2 , a colorless transparent liquid at room temperature. The specific structural formula is as follows. [0003] [0004] δ-valerolactone is a multi-purpose chemical intermediate, and it is used in different fields, mainly used to replace caprolactone in ink and coating additives, and valerolactone is used in the production of ink and coating additives instead of caprolactone Compared with the products produced only with caprolactone, the inks and coatings of our ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D309/30
CPCC07D309/30Y02P20/10
Inventor 刘运海胡江林宋延方杨洋曾伟杨恒东丁可王坤赵欣陈长生黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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