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A method for preparing tributyl citrate by immobilizing tungsten oxide on attapulgite clay

A technology of attapulgite clay and tributyl citrate, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve the problems of complex post-processing, large waste liquid, and high energy consumption, and achieve Environmentally friendly, high activity, and simple preparation method

Active Publication Date: 2021-10-08
安徽新鸿药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention provides an economical and green tributyl citrate preparation method, the process is environmentally friendly, the conditions are mild, and the catalyst can be reused to overcome the serious pollution, high energy consumption, large waste liquid and complicated post-treatment in the prior art and other shortcomings

Method used

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  • A method for preparing tributyl citrate by immobilizing tungsten oxide on attapulgite clay
  • A method for preparing tributyl citrate by immobilizing tungsten oxide on attapulgite clay
  • A method for preparing tributyl citrate by immobilizing tungsten oxide on attapulgite clay

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Preparation of the catalyst: Take 1.5g of attapulgite clay, add the prepared solution containing 0.1g of ammonium metatungstate, stir at 30°C for 52h, let stand for aging for 12h, dry in a blast drying oven for 12h, and then Slowly raise the temperature to 300°C in a muffle furnace for activation for 3 hours to obtain the desired catalyst.

[0029] (2) Preparation of tributyl citrate: get catalyzer 0.1g obtained in step (1), citric acid 100g, n-butanol 150ml, 110 ℃ of reaction 240min, reaction process reflux; The water that reaction produces divides from water separator Go out, react to anhydrous and stop reaction when entering water separator again, obtain tributyl citrate crude product. Filter the crude tributyl citrate, wash the crude citric acid 2-3 times with 5% sodium bicarbonate solution, and then distill under reduced pressure to remove impurities such as water and n-butanol to obtain a colorless and transparent tributyl citrate product , The product yield ...

Embodiment 2

[0033] Change the amount of ammonium metatungstate, prepare the catalyst with reference to the method in step (1) in Example 1, then prepare the tributyl citrate product according to the method in step (2) in Example 1, and the reaction esterification rate can basically reach 100% , wherein the tributyl citrate product yield results are shown in Table 2.

[0034] Table 2 Catalyst preparation results of tributyl citrate catalyzed by different ammonium metatungstate dosages

[0035]

Embodiment 3

[0037] Change catalyst roasting temperature, prepare catalyzer with reference to the method for step (1) among the embodiment 1, then prepare tributyl citrate product according to the method in embodiment 1 step (2), reaction esterification rate can reach 100% substantially, Wherein the tributyl citrate product yield result is as shown in table 3.

[0038] Table 3 Catalysts prepared at different calcination temperatures catalyze the preparation of tributyl citrate results

[0039]

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Abstract

The invention discloses a method for preparing tributyl citrate by immobilizing tungsten oxide on attapulgite clay, which belongs to the technical field of chemical catalysts. The solid acid catalyst of the invention is obtained by using natural attapulgite clay as a carrier and immobilizing tungsten oxide. The solid acid catalyst of the present invention can efficiently catalyze the esterification of citric acid and butanol to generate tributyl citrate, and the yield of the product reaches more than 95%. With advantages such as easy separation and reusability, the industry has broad prospects.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysts, and in particular relates to a method for preparing tributyl citrate by immobilizing tungsten oxide on attapulgite clay. Background technique [0002] At present, the commonly used plasticizers in the plastics industry are phthalates. Due to their potential carcinogenicity, the research and development of new green plasticizers has become a top priority. Tributyl citrate is a green catalyst with good compatibility, high plasticizing efficiency, non-toxic, low volatility, good biodegradability and mechanical properties, and can replace phthalic acid as a plasticizer Widely used in food packaging, daily necessities and children's toys and other fields. [0003] Traditional tributyl citrate mainly uses highly corrosive liquid sulfuric acid as a catalyst. Under the catalysis of sulfuric acid, citric acid and butanol undergo dehydration reaction to produce crude n-butyl citrate. After a se...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/30C07C69/704C07C67/08
CPCB01J23/30C07C67/08C07C69/704
Inventor 杨可武杨凤丽宋烨航梁国斌林伟庄苍伟
Owner 安徽新鸿药业有限公司