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Method for continuously preparing glyceryl triacetate with phenyl phosphate biomimetic catalyst

A technology of glyceryl acetate and phenyl phosphate, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of low triacetin content, biodiesel Complicated components, high cost of ionic liquids, etc., to achieve the effects of low acidity, high yield, and good mass and heat transfer effects

Inactive Publication Date: 2017-09-26
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Patents CN 105087087 A and CN 103159622 A propose a new method for preparing glyceryl acetate, that is, biodiesel (animal and vegetable glyceride) and short-chain alcohol undergo transesterification reaction under the action of alkaline ionic liquid to obtain three Acetate, this method is another method for preparing triacetin, but due to the complexity of biodiesel components, after the transesterification reaction, the product components are more, and the content of triacetin is less, and the purity is not high. high
Patent CN102675095 A improves the previous method, using acidic ionic liquid instead of liquid acid as a catalyst, but after the reaction, the product is difficult to separate, and the cost of ionic liquid is high, and the reaction temperature is also high

Method used

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  • Method for continuously preparing glyceryl triacetate with phenyl phosphate biomimetic catalyst
  • Method for continuously preparing glyceryl triacetate with phenyl phosphate biomimetic catalyst
  • Method for continuously preparing glyceryl triacetate with phenyl phosphate biomimetic catalyst

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Experimental program
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Embodiment 1

[0032] Preparation of phenyl phosphate biomimetic catalysts: diphenyl phosphate (DPP), diphenyl phosphoric acid (DPA) can be purchased from Aladdin reagents, and the preparation of diphenyl phosphoryl trifluoromethanesulfonate imide (PAA): In an anhydrous and oxygen-free environment, take 2 mmol of diphenyl chlorophosphate in a 50 ml flask, add 3 mmol of ammonium trifluoromethanesulfonate to it at -78°C, and react for 2 hours. After the reaction is completed, remove the cooling bath and vacuum the product Dry and purify by column chromatography (dichloromethane as eluent).

[0033] Preparation of pyrophosphoric acid catalyst (IDPA): first synthesize diphenyl ester phosphoramide, take 3 mmol of diphenyl chlorophosphate in a 50ml flask in an anhydrous and oxygen-free environment, pass ammonia gas into it at -78°C, and react for 2 hours , After the reaction, the cold bath was removed, the product was vacuum-dried, and purified by column chromatography to obtain the product (dichl...

Embodiment 2

[0035] Configure 100ml of glycerol benzene solution of 4mol / L as material tank 1, configure 100ml of acetic acid solution of 12mol / L, 16mol / L, and 20mol / L respectively as material tank 2, and add bionic catalyst pyrophosphoric acid catalyst (IDPA) 0.4mol therein , the material tank 1 and the material tank 2 are pumped into the microchannel reactor according to the flow rate ratio of 1:1, and kept at 70°C for 30 minutes. After the reaction, the effluent is taken for liquid phase detection to determine the content of each component.

[0036] Table 1 Effect of acetic acid concentration on glycerol conversion and acetate selectivity in acylation reaction

[0037] Acetic acid concentration

Embodiment 3

[0039] 100ml of glycerol benzene solution of 4mol / L is configured as material tank 1, 100ml of acetic acid solution of 20mol / L is configured as material tank 2, and 0.4mol of biomimetic catalyst pyrophosphoric acid catalyst (IDPA) is added thereto, material tank 1 and material tank 2 according to Pump into the microchannel reactor at a flow rate ratio of 1:1, and retain at 60, 70, and 80°C for 30 minutes (Example 5, 6, 7). After the reaction, take the effluent for liquid phase detection to determine the content of each component.

[0040] Table 2 Effect of microchannel reactor temperature on glycerol conversion and acetate selectivity in acylation reaction

[0041]

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Abstract

The invention provides a method for continuously preparing glyceryl triacetate with a phenyl phosphate biomimetic catalyst, and belongs to the field of synthesis of chemical products. Glycerinum, acetic acid, a catalyst and a solvent are pumped into a microchannel reactor and are subjected to an esterification reaction under the catalytic action of the phenyl phosphate catalyst, and an obtained product and acetic anhydride are subjected to an acylation reaction to obtain glyceryl triacetate. The phenyl phosphate biomimetic catalyst is adopted, the acidity of the phenyl phosphate biomimetic catalyst is relatively low as compared with that of a liquid acid, the equipment is less corroded, and the phenyl phosphate biomimetic catalyst is a bifunctional small-molecule catalyst and is higher in catalytic efficiency under the action of a hydrogen bond, the conversion rate of glycerinum is up to 100%, and the yield of glyceryl triacetate is up to more than 95%.

Description

technical field [0001] The invention belongs to the field of chemical product synthesis, and in particular relates to a method for continuous production using a microchannel reaction device and small molecule catalysis of a bionic catalyst phenyl phosphate. Background technique [0002] Glycerol Triacetate (Glycerol Triacetate) is a colorless, odorless, oily liquid, non-toxic and non-irritating. Glyceryl acetate is soluble in alcohol, benzene, ethers, castor oil and other organic solvents, and can dissolve nitrocellulose, acrylic resin, polyvinyl acetate, etc. Glyceryl acetate has good gelling effect and physiological inertness, and is widely used as a plasticizing and curing agent for cellulose acetate in cigarette filters, food additives, spice fixatives, cosmetic fixatives and lubricating bases. Glyceryl acetate is widely used in tobacco, food and metallurgical industries as a safe and non-toxic plasticizer. [0003] The traditional synthetic method of glycerol triaceta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/18B01J31/02B01J19/00
CPCB01J19/0093C07C67/08B01J31/0271C07C69/18
Inventor 朱晨杰郭凯沈涛唐成伦应汉杰欧阳平凯
Owner NANJING UNIV OF TECH
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