A method for synthesizing tri-n-butyl citrate with acid-modified h-zms-5 type molecular sieve

A technology of H-ZMS-5 and tri-n-butyl ester, which is applied in the direction of molecular sieve catalysts, carboxylate preparation, chemical instruments and methods, etc., can solve the problems of unsatisfactory catalytic effect of molecular sieves, difficult treatment of reaction waste liquid, and high production costs. , to achieve high yield, reduce the amount of acid, and reduce the effect of corrosion

Active Publication Date: 2021-02-19
GUANGDONG IND TECHN COLLEGE
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  • Abstract
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AI Technical Summary

Problems solved by technology

The traditional esterification reaction generally uses sulfuric acid as a catalyst. Although the catalyst is cheap and has high catalytic activity, this method has disadvantages such as serious equipment corrosion, many side reactions, difficult disposal of reaction waste liquid, and high production cost.
Molecular sieves are widely used as catalysts. Molecular sieves have regular and uniform intracrystalline pores, and the pore size is close to the molecular size, so that the catalytic performance of molecular sieves varies significantly with the geometric size of reactant molecules, product molecules or reaction intermediates. However, the catalytic effect of simple molecular sieves is not ideal.

Method used

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  • A method for synthesizing tri-n-butyl citrate with acid-modified h-zms-5 type molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0023]In this example, the H-ZMS-5 molecular sieve was modified by sulfuric acid of 5 groups of different concentrations set in Table 1, and then used to catalyze the esterification reaction to prepare tri-n-butyl citrate, to study the effect of different sulfuric acid concentrations on the esterification rate influences.

[0024]The synthesis steps of tri-n-butyl citrate are as follows: H-ZMS-5 molecular sieve (silica-aluminum ratio 25) is dried in a blast drying oven at 300°C for 2 hours to activate it, and the activated H-ZMS-5 molecular sieve is activated with different concentrations of sulfuric acid Soak for 15h (see Table 1 for sulfuric acid concentration), then put it in a blast drying box for drying for two hours, then grind into powder to obtain acid-modified H-ZMS-5 molecular sieve; add 0.538g anhydrous citric acid, 1.24g n-butyl The acid-modified H-ZMS-5 molecular sieve containing 3% alcohol and anhydrous citric acid by mass was added to a 50ml round bottom flask (the molar...

Embodiment 2

[0028]In this example, the H-ZMS-5 molecular sieve was modified according to the 5 groups of different sulfuric acid soaking times set in Table 2, and then used to catalyze the esterification reaction to prepare tri-n-butyl citrate, and the effect of different sulfuric acid soaking time on esterification was studied. Rate of impact.

[0029]The synthesis steps of tri-n-butyl citrate are as follows: H-ZMS-5 molecular sieve (silica-aluminum ratio 25) is dried in a blast drying oven at 300°C for 2 hours to activate it, and the activated H-ZMS-5 molecular sieve uses 5mol / L Soak in sulfuric acid (see Table 2 for soaking time), then put it in a blast drying box for drying for two hours, and then grind into powder to obtain acid-modified H-ZMS-5 molecular sieve; change anhydrous citric acid, n-butanol, and acid H-ZMS-5 molecular sieve was added to a 50ml round-bottom flask (the molar ratio of anhydrous citric acid and n-butanol was 1:6, and the acid-modified H-ZMS-5 molecular sieve was 3% of ...

Embodiment 3

[0033]In this example, according to the 5 groups of different catalyst addition amounts set in Table 3, the esterification reaction was used to prepare tri-n-butyl citrate, and the effect of different catalyst addition amounts on the esterification rate was studied.

[0034]The synthesis steps of tri-n-butyl citrate are as follows: H-ZMS-5 molecular sieve (silica-aluminum ratio 25) is dried in a blast drying oven at 300°C for 2 hours to activate it, and the activated H-ZMS-5 molecular sieve uses 5mol / L Soak in sulfuric acid for 15 hours, then put it in a blast drying box for drying for two hours, and then grind into powder to obtain acid-modified H-ZMS-5 molecular sieve; anhydrous citric acid, n-butanol, acid-modified H-ZMS-5 The molecular sieve was added to a 50ml round-bottom flask (the molar ratio of anhydrous citric acid to n-butanol was 1:6, and the amount of acid-modified H-ZMS-5 molecular sieve added was shown in Table 3), and the esterification reaction was carried out (the rea...

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Abstract

The invention belongs to the field of tri-n-butyl citrate synthesis, in particular to a method for synthesizing tri-n-butyl citrate with an acid-modified H-ZMS-5 molecular sieve. The method comprises the following steps: soaking the H-ZMS-5 molecular sieve with sulfuric acid after activation, the concentration of the sulfuric acid is 1-18mol / L, and the soaking time is 1-18h; after suction filtration, the solid is dried and ground into powder to obtain Acid-modified H-ZMS-5 molecular sieve; Anhydrous citric acid, n-butanol, acid-modified H-ZMS-5 molecular sieve are added to a reaction vessel for esterification to obtain tri-n-butyl citrate; the esterification reaction temperature The temperature is 110-140°C, and the reaction time is 1-9h. The invention combines the advantages of high catalysis of concentrated sulfuric acid and molecular sieve, and has the characteristics of high yield, easy purification, reduced environmental pollution and the like.

Description

Technical field[0001]The invention belongs to the field of synthesis of tri-n-butyl citrate, and specifically relates to a method for synthesizing tri-n-butyl citrate by an acid-modified H-ZMS-5 molecular sieve.Background technique[0002]In recent years, China has gradually become the country with the largest plasticizer production and consumption in Asia. Compared with foreign countries, my country's plasticizer varieties are slightly single, and the product structure is unreasonable. In addition, there are more synthetic units and poor yield. Discharge pollution of high and acid-base waste is serious, forcing many domestic plasticizer companies to reduce or suspend production. In addition, in recent years, more and more studies and reports have publicly demonstrated the negative effects of dioctyl phthalate DOP and other phthalic plasticizers. Due to the lack of raw material sources such as isononanol and decanol in my country, the production and sales structure of plasticizers in ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/704B01J29/40
CPCB01J29/40B01J2229/18C07C67/08C07C69/704
Inventor 黎彧邹训重冯安生游遨
Owner GUANGDONG IND TECHN COLLEGE
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