Method for synthesizing acetyl tributyl citrate by using ion type catalyst

A technology of acetyl tributyl citrate and tributyl citrate, applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve the problem of low yield of acetyl tributyl citrate, The problems of difficult catalyst recovery and long product purification time can shorten the washing time, avoid emulsification, and shorten the purification time.

Active Publication Date: 2008-02-20
李祥庆
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Problems solved by technology

The shortcoming of this method is that the recovery of catalyst is difficult, easy emulsification during dealcoholization and dehydration in tributyl citrate synthesis, product purification time is long; When acetyl tributyl citrate is synthesized, the by-product acetic

Method used

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Experimental program
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Embodiment Construction

[0021] One, the synthesis of tributyl citrate

[0022] In a 500ml four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and an oil-water separator, add 0.60mol of citric acid, add sodium bisulfate monohydrate (3.0%, citric acid mass percent) and n-butanol (2.4- 3.8mol); stirring, heating, and dissolving, when the temperature reaches 50°C, take the reaction solution to measure the initial acid value, record the time when the system starts to reflux and divide water in time, the reflux temperature is 110-140°C, and react for 2-5 hours ( The temperature is not higher than 170°C), and the acid value is measured by sampling every 30 minutes. According to the national standard GB1668-81 method, the acid value change before and after the reaction is measured, and the esterification rate is calculated according to the following formula:

[0023] Esterification rate=(reaction initial acid value-reaction end acid value) / reaction initial acid value.

[0024] After...

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Abstract

The invention relates to a method for synthesizing acetyl tributyl citrate through electrophoretic catalyst. The method comprises the steps: step one: citric acid, butanol and sodium bisulfate monohydrate are added into a reactor, and the catalyst is recycled and filtered after the cooling of the stirring reflux reaction, filtrate is neutralized by adding alkaline solution and rinsed till neutral state, then the butanol is distilled and recycled under normal pressure, and the residual water is steamed under reduced pressure to acquire crude tirbutyl citrate, and the compound decolurant of acticarbon and aluminum oxide is added into the crude tirbutyl citrat for decoloring treatment, thereby, the finished tirbutyl citrat is acquired; step two: the finished tirbutyl citrate, acetic anhydride and the sodium bisulfate monohydrate are added into the reactor, and the catalyst is filtered , cooled and recycled after 1.0-3.0 hours of stirring reaction under the temperature of 50-90 DEG C; filtrate is neutralized by adding alkaline solution and rinsed till neutral state; acetyl tributyl citrate is acquired after water phase is separated and n-butyl acetate is distilled under reduced pressure and recycled. The catalyst of the method of the invention is easily separated and recycled, the esterification process is not easily influenced by by-product, emulsification is not easy during the rinsing process and the product yield is high.

Description

technical field [0001] The invention relates to a method for synthesizing a non-toxic plasticizer, in particular to a method for synthesizing acetyl tributyl citrate with an ionic catalyst. It belongs to the field of fine chemical technology. Background technique [0002] At present, most commonly used plasticizers are phthalate plasticizers. Because they may induce cancer, foreign countries have legislated to restrict their use, and are actively looking for non-toxic plasticizers that can replace phthalates. Acetyl tributyl citrate is a promising non-toxic plasticizer, and the US Food and Drug Administration (FDA) considers it to be one of the safest plasticizers. Acetyl tributyl citrate has excellent cold resistance, light resistance and water resistance, good compatibility with polyvinyl chloride, polypropylene and various fiber resins, high plasticizing efficiency, non-toxic, low volatility, etc., especially in food Packaging, medical products, children's toys and othe...

Claims

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Application Information

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IPC IPC(8): C07C69/704C07C67/08B01J27/053
CPCY02P20/584
Inventor 李祥庆王向辉冯文
Owner 李祥庆
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