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A kind of mesoporous molecular sieve loaded heteropolyacid catalyzed method for synthesizing medicinal triethyl citrate

A technology of triethyl citrate and loaded heteropoly acid, applied in molecular sieve catalysts, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of short validity period, low product purity, low product yield and the like, and achieve repeatability. The effect of improving usability, improving catalytic efficiency, and increasing specific surface area

Active Publication Date: 2016-08-24
HUNAN ER KANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional esterification reaction uses concentrated sulfuric acid as a catalyst. Although the catalytic effect is good, concentrated sulfuric acid has strong acidity and strong oxidizing properties, which is highly corrosive to equipment and requires high requirements. At the same time, side reactions are prone to occur, such as carbonization of organic matter by concentrated sulfuric acid , ethanol itself condenses into ether, etc., resulting in low product yield and product quality problems: low product purity, poor color, easy acidification, and short validity period
Although the preparation method has a simple process, is easy to control, and has warm reaction conditions, in fact, using mixed solid acids as a catalyst not only cannot realize the effective recovery and reuse of the catalyst, but also causes loss and waste, thereby further increasing the production cost; In addition, the preparation of triethyl citrate through a three-step reaction is not easy to control the occurrence of side reactions, and the comprehensive reaction efficiency is not high
[0010] CN102659591A discloses a method for preparing triethyl citrate by continuous catalysis, aiming at technical problems such as easy loss of catalyst and complex post-treatment process in the above two schemes, it is proposed to use a fixed-bed continuous catalytic reaction device to carry out triethyl citrate For the production of the production, the styrene-based cation exchange resin loaded with Lewis acid is used as a catalyst, and it is packed into a series fixed bed. The reactant enters from the top of the reactor, passes through the middle catalyst layer, and undergoes an esterification reaction under heat preservation conditions, and the reaction product is obtained from the reaction The unreacted ethanol is discharged from the upper part of the gas-liquid separation device, and the crude triethyl citrate is discharged from the lower part, and the final product is refined
[0018] In fact, since the interaction between the heteropolyacid and the surface of the carrier is basically an acid-base reaction, the strength of the acid-base of the hydroxyl group on the surface of the carrier and the strength of the heteropolyacid are different, and the result of the interaction between the two forms the acid strength and loading. Different active bodies affect the activity and elution amount of the supported heteropolyacid catalyst in the reaction

Method used

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  • A kind of mesoporous molecular sieve loaded heteropolyacid catalyzed method for synthesizing medicinal triethyl citrate
  • A kind of mesoporous molecular sieve loaded heteropolyacid catalyzed method for synthesizing medicinal triethyl citrate
  • A kind of mesoporous molecular sieve loaded heteropolyacid catalyzed method for synthesizing medicinal triethyl citrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] 2g P123 is dissolved in the hydrochloric acid that concentration is 2mol / L, after fully dissolving, 40 o C, 10ml

[0064] tetraethyl orthosilicate and 1.3 g of Pd-H 4 SiW 12 o 40 The solution was slowly added dropwise to the P123 solution, and the constant temperature stirring was continued for 5h. then at 80 o Stand at C for 36 hours to crystallize. After taking it out, wash the product until neutral, filter to obtain a solid, and dry it at room temperature. Finally, at 500 o C roasting for a period of time to obtain the finished catalyst.

Embodiment 2

[0066] 4g P123 is dissolved in the hydrochloric acid that concentration is 2mol / L, after fully dissolving, 40 o C, 10ml of tetraethyl orthosilicate and 1.3g of Pd-H 3 PiW 12 o 40 The solution was slowly added dropwise to the P123 solution, and the constant temperature stirring was continued for 5h. then at 80 o Stand at C for 36 hours to crystallize. After taking it out, wash the product until neutral, filter to obtain a solid, and dry it at room temperature. Finally, at 500 o C is roasted for a period of time to obtain the finished catalyst.

Embodiment 3

[0068] 3g P123 is dissolved in the hydrochloric acid that concentration is 2mol / L, after fully dissolving, 40 o C, 10ml of tetraethyl orthosilicate and 3.9g of Pd-H 3 PM o12 o 40The solution was slowly added dropwise to the P123 solution, and the constant temperature stirring was continued for 4h. then at 80 o Stand at C for 36 hours to crystallize. After taking it out, wash the product until neutral, filter to obtain a solid, and dry it at room temperature. Finally, at 500 o C is roasted for a period of time to obtain the finished catalyst.

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Abstract

The invention discloses a method for catalytically synthesizing medicinal triethyl citrate by using mesoporous molecular sieve loaded heteropoly acid and in particular relates to a method for refining and purifying a triethyl citrate coarse product to obtain the triethyl citrate, wherein a mesoporous molecular sieve loaded heteropoly acid catalyst is prepared through a in-situ synthesis method and is used for catalyzing the reaction between citric acid and ethyl alcohol to synthetize the triethyl citrate coarse product. The method is mild in reaction condition, high in product esterification rate, good in purity, short in reaction time and suitable for industrial production. The catalyst can be recycled.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and relates to a method for synthesizing triethyl citrate, in particular to a method for catalytically synthesizing medicinal triethyl citrate with mesoporous molecular sieves loaded with heteropolyacids. Background technique [0002] Triethyl citrate (triethyl citrate, also known as triethyl citrate), the molecular formula is C 12 h 20 o 7 , the chemical structural formula is: [0003] [0004] Triethyl citrate is a colorless transparent liquid at room temperature, and its solubility in water is 6.5g / 100ml (25 o C). Triethyl citrate is non-toxic, has a slightly lemony aroma, is soluble in most organic solvents, and hardly soluble in oils. It has good compatibility with most cellulose, polyvinyl chloride and chlorinated rubber. As a plastic plasticizer, it is widely used in daily necessities, food, pharmaceutical packaging, cosmetics, etc. It has high plasticizing efficiency and low volat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/704C07C67/08B01J31/16
CPCB01J29/0341B01J2229/20C07C67/08C07C67/54C07C67/56C07C69/704Y02P20/50Y02P20/584
Inventor 帅放文章家伟王向峰
Owner HUNAN ER KANG PHARMA