Method for preparing salicylate through green synthesis process

A technology of salicylates and methyl salicylate, which is applied in the field of green synthesis of salicylates, can solve the problems of treatment, large amounts of waste water and waste salt, achieve smooth reaction, improve quality and yield rate, reduce the effect of side effects

Pending Publication Date: 2021-02-05
马鞍山科思化学有限公司
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Problems solved by technology

[0004] There are few reports about the synthesis of protofilm loose esters, and the existing preparation methods mainly exist in the following ways: salicylic acid and isophorol are directly esterified and synthesized. After the reaction, a large amount of water washing is required to remove the catalyst. A large amount of waste water and waste salt need to be treated; salicylates and isophorol are synthesized by transesterification under the catalysis of alkali metals. This method also requires a large amount of water washing to remove the catalyst after the reaction, resulting in a large amount of waste water and Waste salt needs to be treated

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  • Method for preparing salicylate through green synthesis process

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preparation example Construction

[0044] According to the present invention, one aspect is to provide a preparation method of salicylate green synthesis process, said method comprising the following steps:

[0045] Step 1, mixing salicylate compounds and isophorol, optionally adding a catalyst.

[0046] In step 1, the salicylate compound is a salicylate, preferably an alkyl salicylate, preferably selected from methyl salicylate, ethyl salicylate, isopropyl salicylate, One or more of isobutyl salicylate and isoamyl salicylate.

[0047] Preferably, the salicylate compound is methyl salicylate.

[0048] In the present invention, methyl salicylate has the advantages of simple structure among salicylate compounds, small steric hindrance, low toxicity, environmental friendliness, simple and mature synthesis process, and low requirements for equipment. More importantly, under the action of a catalyst, methyl salicylate is easily decomposed under heating conditions, and the products are salicylic acid and methanol. ...

Embodiment 1

[0092] In a 1000ml four-necked flask with a rectification tower, 152g of methyl salicylate, 426g of isophorol, and 14g of potassium carbonate were fed.

[0093] Turn on the water circulation vacuum pump, adjust the vacuum pressure to -0.085MPa, start stirring and raise the temperature to 115-120°C; continue to produce methanol, when the methanol production slows down, add 100g of toluene, slowly increase the vacuum degree to -0.095MPa, the large reflux is small The final small amount of methanol is taken out until the reaction is completed, the total reaction time is 3 hours, the conversion rate is greater than 99%, and the selectivity is greater than 99%.

[0094] After the reaction, the temperature was lowered to 70-80°C, potassium carbonate was removed by filtration, and the recovered potassium carbonate was directly used in the transesterification step, and the filtrate was transferred into a four-neck flask.

[0095] Add a small amount of acetic acid to adjust the pH of t...

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Abstract

The invention discloses a method for preparing salicylate through a green synthesis process. The method comprises the following steps: carrying out ester exchange on salicylate compounds and isophorone which are used as raw materials under the catalysis of a potassium carbonate weak base catalyst, directly conducting filtering after the ester exchange is finished, directly applying the obtained weak base catalyst to the next batch of reaction, and directly rectifying and purifying the obtained filtrate to obtain the salicylate, thereby obtaining a finished homosalate product meeting requirements. After the process is used for improving an original process, the whole system does not generate waste water and waste residues any more, so corresponding cost for treating the waste water and thewaste residues is saved, raw material cost is correspondingly saved due to continuous application of the catalyst, the product has a cost advantage, and the current demand for a green and environment-friendly process is better met.

Description

technical field [0001] The present invention relates to the field of chemical engineering, in particular to a preparation method of salicylic acid esters with a green synthesis process. Background technique [0002] Original film loose ester (HMS), CAS number: 118-56-9, molecular formula: C 16 h 22 o 3 , molecular weight: 262.34. This product is a colorless to light yellow oily liquid with a density of 1.05g / cm 3 , boiling point 141-165°C (12torr), refractive index 1.516-1.519, flash point 132.3°C, water solubility <0.1g / 100ml (26°C). [0003] The original film loose ester has good compatibility with resin and is not colored. It is widely used in plastics such as soft and rigid polyvinyl chloride and coatings such as nitrocellulose, acrylic resin and polyurethane as a light stabilizer; it is irritating to the skin. It is very small and can be added to high-end cosmetics as a sunscreen agent. As an important daily chemical product, it is often found in the formulation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/84C07C67/03C07C67/54
CPCC07C67/03C07C67/54C07C69/84
Inventor 王荣刘启发王中孝
Owner 马鞍山科思化学有限公司
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