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A kind of production method of vanillin-1,2-propanediol acetal

A technology of propylene glycol acetal and production method, which is applied in the direction of organic chemistry, can solve the problems of long reaction time, pollution of the environment and food, and achieve the effects of shortened reaction time, low cost and high product yield

Active Publication Date: 2020-05-08
CHONGQING THRIVE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of this, the purpose of this invention is to provide a kind of production method of vanillin-1,2-propanediol acetal, to solve existing method production vanillin-1,2-propanediol acetal exists reaction time is long, uses Benzene as a solvent has problems such as polluting the environment and food

Method used

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Embodiment Construction

[0029] The present invention will be further described below in conjunction with embodiment.

[0030] The production method of present embodiment vanillin-1,2-propanediol acetal comprises the following steps:

[0031] 1) Clean the reactor, and remove water from the reactor and its condensing device so that the water content is lower than 500ppm. The effect of this step on removing water in the reaction system is to increase the reaction rate, and the presence of water will reduce the reaction rate. Since the reaction medium in the production method of vanillin-1,2-propanediol acetal in this embodiment is acidic, it will produce corrosion, and the product will turn red when it encounters iron, so the material of the reaction kettle in contact with the material needs to be 316L or 904, Or materials such as Hastelloy plates with better acid resistance.

[0032] 2) The raw material vanillin and the raw material 1,2-propanediol are sequentially added in proportion to the reactor....

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Abstract

The invention discloses a production method of vanillin-1,2-propylene glycol acetal. The production method comprises the following steps: firstly, cleaning a reaction still, dehydrating the reaction still and a condensing device thereof so as to enable the water content of the reaction still to be lower than 500 ppm; secondly, adding raw materials vanillin and 1,2-propylene glycol into the reaction still; thirdly, adding an acidic substance as a catalyst into the reaction still and uniformly stirring; fourthly, vacuumizing the reaction still and enabling the reaction still to be in a certain negative pressure state; fifthly, raising the temperature of the reaction still to required temperature and reacting at the required temperature for a certain time; sixthly, carrying out sampling detection on a reaction product, adding a certain amount of alkaline raw materials into the reaction still to neutralize the catalyst after the reaction product is qualified by detecting; seventhly, carrying out reduced pressure distillation on the unreacted 1,2-propylene glycol and finally distilling and collecting to obtain qualified vanillin-1,2-propylene glycol acetal. The reaction time of the production method disclosed by the invention is 3 to 8 hours; compared with the prior production method, the production method disclosed by the invention has the advantages that reaction time is greatly shortened; in addition, the use of an organic solvent benzene is avoided and further environment friendliness is realized.

Description

technical field [0001] The invention relates to the technical field of ethyl vanillin, in particular to a production method of vanillin-1,2-propanediol acetal. Background technique [0002] Vanillin-1,2-propanediol acetal is a new type of raw material commonly used in the fragrance industry in the past ten years. The domestic fragrance industry first discovered that this compound should pass through the essence containing vanillin and 1,2-propanediol. Detected by GC / MS. In 1998, the American Flavor and Extract Manufacturers Association (FEMA) announced the FEMA number of vanillin-1,2-propanediol acetal as 3905, and suggested the dosage in food as 2-999mg / kg. Since then, it has been used more and more widely in the spice industry, and there are more studies on it. [0003] Vanillin 1,2-propanediol is a spice with vanillin smell, it is colorless to light yellow or yellow viscous liquid, it is stable and does not change color in neutral or alkaline solution, but it is easy to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/22
CPCC07D317/22
Inventor 兰军汪洋姚皖川赵华文唐凌
Owner CHONGQING THRIVE CHEM
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