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Preparation method of acetyl tri-n-butyl citrate and catalyst used in preparation method

A technology of acetyl tri-n-butyl citrate and citric acid, which is applied to the preparation of carboxylic acid esters, the preparation of organic compounds, and physical/chemical process catalysts, etc., to achieve high production efficiency, high catalytic activity, and low corrosion effects

Active Publication Date: 2013-09-25
宁波永顺精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And the solid superacid SO used in the present invention 4 2- / ZrO 2 -WO 3 (SZW) None reported

Method used

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  • Preparation method of acetyl tri-n-butyl citrate and catalyst used in preparation method
  • Preparation method of acetyl tri-n-butyl citrate and catalyst used in preparation method
  • Preparation method of acetyl tri-n-butyl citrate and catalyst used in preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Embodiment 1, a kind of preparation method of organic compound---acetyl tri-n-butyl citrate, take citric acid, n-butanol as raw material, carry out following steps successively:

[0034] 1) Solid superacid SO as a catalyst 4 2- / ZrO 2 -WO 3 (SZW) preparation, carry out following steps successively:

[0035] ①. Weigh 5g of ZrOCl 2 ·8H 2 O is dissolved in deionized water (about 20ml), and the mass ratio M(ZrOCl 2 ): M(H 2 O)=1:8 ZrOCl 2 Aqueous solution; slowly add ammonia water to the above solution to adjust the pH to 9.

[0036] ②. Stir the mixture obtained in step ① for 25 min at room temperature, put it in an oven, and age it at 80°C for 36 h; filter, and wash the obtained filter cake with water until it is free of Cl - Then, it was placed in a muffle furnace and fired at 550 °C for 12 h.

[0037] ③. After cooling the roasted product obtained in step ② to room temperature, grind it into a powder that can pass through 100 mesh (pass through a 100 mesh sieve)...

Embodiment 2

[0043] Embodiment 2, a kind of preparation method of organic compound---acetyl tri-n-butyl citrate, with citric acid, n-butanol is raw material, carries out following steps successively:

[0044] 1) Solid superacid SO as a catalyst 4 2- / ZrO 2 -WO 3 (SZW) preparation:

[0045] With embodiment 1.

[0046] 2) React 0.1mol of citric acid, 0.3mol of butanol, 0.10g of SZW and 100ml of toluene in a 250ml three-neck flask under the condition of reflux and water separation, and continuously separate water during the reaction. After 3 h of reaction, the reaction was stopped, and the reaction solution was cooled to room temperature.

[0047] 3) Add 0.1 mol of acetic anhydride and 0.05 g of SZW to the reaction solution cooled to room temperature, and react at room temperature for 1 hour. Filter out the catalyst and reuse it. The filtrate was distilled under reduced pressure to remove toluene, a small amount of unreacted n-butanol and acetic acid produced in the reaction, and the s...

Embodiment 3

[0048] Embodiment 3, a kind of preparation method of organic compound---acetyl tri-n-butyl citrate, with citric acid, n-butanol is raw material, carries out following steps successively:

[0049] 1), solid superacid SO 4 2- / ZrO 2 -WO 3 (SZW) catalyst preparation:

[0050] With embodiment 1.

[0051] 2) React 0.1mol citric acid, 0.35mol n-butanol, 0.20g SZW and 100ml toluene in a 250ml three-necked flask under the condition of reflux and water separation, and continuously separate water during the reaction. After 5 hours of reaction, the reaction was stopped, and the reaction solution was cooled to room temperature.

[0052] 3) Add 0.1 mol of acetic anhydride and 0.05 g of SZW to the reaction solution cooled to room temperature, and react at room temperature for 2 hours. Filter out the catalyst and reuse it. The filtrate was distilled under reduced pressure to remove toluene, a small amount of unreacted n-butanol and acetic acid produced in the reaction, and the still l...

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Abstract

The invention discloses a preparation method of acetyl tri-n-butyl citrate. The solid super acid SO-42- / ZrO2-WO3 prepared in the invention is used as a catalyst in the preparation method. The preparation method comprises the following steps sequentially: 1), reacting citric acid and n-butyl alcohol which are used as the raw material with the catalyst for 3-4hours in a solvent under the condition of circumfluence to repel water; 2), reducing the temperature of the reactant obtained in the step 1) to normal temperature, adding acetic anhydride with the amount that is equal to the molar weight of the citric acid used in the step 1) and adding catalyst, reacting for 1-3hours at normal temperature; after the reaction is finished, firstly filtering to remove the catalyst, and then subjecting the filtrate to reduced pressure distillation in order to remove the solvent, the n-butyl alcohol which does not participate in the reaction and the acetic acid generated during the reaction, so as to obtain the acetyl tri-n-butyl citrate. The acetyl tri-n-butyl citrate prepared by the method disclosed by the invention has the characteristics of high production efficiency, easy and convenient operation, environment-friendly production and the like.

Description

technical field [0001] The invention relates to a preparation method of an organic compound---acetyl tri-n-butyl citrate and a used catalyst. Background technique [0002] Acetyl tri-n-butyl citrate, referred to as ATBC, its molecular formula is C 20 h 34 o 8 , its structural formula is shown in S-1, and its pure product is a colorless, odorless oily liquid with a boiling point of 343°C; it is a new type of non-toxic and environmentally friendly plasticizer, which has the characteristics of non-toxic, tasteless, good compatibility, plasticizing It has the advantages of high efficiency, easy biodegradation and low volatility, excellent cold resistance, light resistance and water resistance, and can replace traditional phthalate-based plasticizers. It can be used as a plasticizer for polyvinyl chloride, cellulose resin and synthetic rubber, for non-toxic PVC granulation, food packaging containers, children's toys, medical products, films, plates, cellulose coatings and othe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053C07C69/716C07C67/08
Inventor 贾银霞陈新发韦隆武张小莲
Owner 宁波永顺精细化工有限公司
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