The preparation method of monoglyceride butyrate

A technology of butyric acid monoglyceride and glycerol is applied in the field of preparation of butyric acid monoglyceride, can solve the problems of low yield of butyric acid monoglyceride, poor quality of butyric acid glyceride, difficult industrialized production, etc. The effect of reaction time, avoiding poor quality, and reducing the generation of by-products

Active Publication Date: 2016-01-06
HUBEI XINZHOU CHEM
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Problems solved by technology

[0004] Then, in the experimental research, it was found that in the above-mentioned synthetic process, the whole reaction rate was relatively slow, and it was difficult to promote to industrial production; after the completion of the reaction, a large amount of alkali-containing saturated brine was needed to wash to remove phosphoric acid, resulting in the production of butyric acid mono- and diglycerides. The rate is low, and produce a large amount of waste water; Use mineral acid as the catalyzer of esterification reaction, can produce the side reaction of butyric acid glyceride poor quality; In addition, because the water-carrying agent carbon tetrachloride used is poisonous substance, consumption is larger Purification is required to obtain the final product, and the steps are cumbersome

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  • The preparation method of monoglyceride butyrate

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Embodiment 1

[0016] The preparation method of monoglyceride butyrate comprises the following steps:

[0017] 1) Preparation of sulfonic acid mesoporous molecular sieve: Dissolve 4g of template agent P123 in 130mL of 2mol / L hydrochloric acid solution at 35°C, stir to mix evenly, then add 8.4g of tetraethyl orthosilicate, 10g For p-toluenesulfonic acid, continue to stir for 24h, crystallize at 130°C for 24h, filter, wash and dry, and finally calcinate at 500°C for 6h to remove the template agent, then filter, wash and dry to obtain mesoporous molecular sieve SBA-15- SO 3 H.

[0018] 2) Mix 18.4 grams (200 mmol) of glycerin and 17.8 grams (200 mmol) of n-butyric acid, add a total of 1.78 grams of a mixed catalyst of sulfonic acid mesoporous molecular sieve and ZSM-5 acidic zeolite, heat and stir to 100 ° C, the sulfonic acid mesoporous The weight ratio of pore molecular sieve to ZSM-5 acidic zeolite is 3:1, heat to reflux, and use liquid chromatography for central control detection from the...

Embodiment 2

[0020] The preparation method of monoglyceride butyrate comprises the following steps:

[0021] 1) Preparation of sulfonic acid mesoporous molecular sieve: Dissolve 4g of template agent P123 in 130mL of 2mol / L hydrochloric acid solution at 40°C, stir to mix evenly, then add 8.4g of tetraethyl orthosilicate, 10g For p-toluenesulfonic acid, continue to stir for 28h, crystallize at 130°C for 36h, filter, wash and dry, and finally calcinate at 500°C for 8h to remove the template agent, then filter, wash and dry to obtain mesoporous molecular sieve SBA-15- SO 3 H.

[0022] 2) Mix 18.4 grams (200 mmol) of glycerin and 17.8 grams (200 mmol) of n-butyric acid, add a total of 1.07 grams of a mixed catalyst of sulfonic acid mesoporous molecular sieve and ZSM-5 acidic zeolite, heat and stir to 110 ° C, and the sulfonic acid media The weight ratio of pore molecular sieve to ZSM-5 acidic zeolite is 3:1, heat to reflux, and use liquid chromatography for central control detection from the ...

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Abstract

The invention discloses a preparation method for glyceryl tributyrate. The preparation method comprises: taking glycerin and n-butyric acid as raw materials, adding a catalyst and heating to 100-110 DEG C with stirring, performing heating reflux as well as dropwise adding butyric anhydride, stopping reaction until no water is generated in the reaction solution during dropwise adding, cooling to room temperature, and filtering, so as to obtain glyceryl tributyrate. The catalyst is a mixture of sulfonic-acid mesoporous molecular sieve and ZSM-5 acidic zeolite, and the usage amount of the catalyst is 2-10% by weight of the sum of glycerin and n-butyric acid. By taking sulfonic-acid mesoporous molecular sieve and ZSM-5 acidic zeolite as the catalyst, the selectivity is high, the reaction time is shortened, the generation of by-products is reduced and the catalyst is reusable. By employing the method, the reaction system does not need a water-carrying agent, so that the reaction cost and safe hidden trouble are reduced, the purification step of the product is simplified, the post-processing process is simple, environment is protected and energy is saved. The obtained glyceryl tributyrate is high in purity and high in yield, the reaction speed is fast, and industrial production is easy to realize.

Description

technical field [0001] The invention relates to a synthesis method of a pharmaceutical intermediate, in particular to a preparation method of monoglyceride butyrate. Background technique [0002] Butyrate monoglyceride (glyceryltributyrate) is the chemical formula C 15 h 26 o 6 The short-chain fatty acid esters are esterified products of butyric acid and glycerol, and are polyol-type nonionic surfactants. From its molecular structure, it can be used as both W / O emulsifier and O / W emulsifier. [0003] According to domestic and international document reports, the synthetic method of existing butyric acid monooleyl: take glycerin and butyric acid as raw material, carbon tetrachloride is as water-carrying agent, phosphoric acid is as catalyst, after mixing, heating reflux, purification, make butyric acid Monoglycerides, of which the content of butyric monoglycerides is 60.2%. (See Liao Hejing et al. Synthesis of glyceryl butyrate and its application in oil microencapsulatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/30C07C67/08B01J29/40B01J29/03
CPCB01J29/03B01J29/40B01J2229/37C07C67/08C07C69/30
Inventor 闵江华黄剑雄
Owner HUBEI XINZHOU CHEM
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