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Method for synthesizing n-butyl acetate

A technology of n-butyl acetate and acetic acid, applied in the field of synthesizing n-butyl acetate, can solve the problems of high production cost, large equipment investment, unavailability, etc., achieves good selectivity and yield, high acetic acid conversion rate, and reduces overall The effect of energy consumption

Active Publication Date: 2015-09-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method has the advantages of mature technology, simple equipment and convenient operation, due to the use of concentrated sulfuric acid as a catalyst, this method has the following defects: (1) The selectivity of n-butyl acetate is poor, and it is difficult to refine: concentrated sulfuric acid is used to catalyze the esterification reaction At the same time, it can also catalyze reactions such as oxidation, dehydration, sulfonation, carbonization, and polymerization; (2) The recovery and reuse of raw materials is difficult; (3) The separation of catalysts is difficult: it needs to undergo subsequent processes such as alkali neutralization and water washing, resulting in A large amount of waste water is produced while n-butyl acetate is lost; (4) Concentrated sulfuric acid severely corrodes equipment, resulting in large investment in equipment and high production costs
Since the application of conventional molecular sieves, including catalytic applications, mainly utilizes the space or active centers in the micropore channels, the structure-directing agent contained in the molecular sieve channels must be removed, so that the spaces or active centers in the channels can be released. Utilization, that is, molecular sieves containing structure-directing agents (templates) in the channels are basically unusable or extremely inefficient in conventional molecular sieve applications, including catalytic applications.
However, generally due to the limitation of the channels, the structure-directing agent existing in the channel of the molecular sieve is very stable, and it is difficult to remove it by methods such as washing and extraction; Such as N, P, etc.) are difficult to contact with external molecules, so it is generally believed that the structure-directing agents existing in the pores of molecular sieves cannot be used

Method used

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  • Method for synthesizing n-butyl acetate
  • Method for synthesizing n-butyl acetate
  • Method for synthesizing n-butyl acetate

Examples

Experimental program
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Effect test

Embodiment 1

[0063] 19.4kg of acetic acid and 44.2kg of n-butanol were added to a dry stainless steel pressure reactor, and then 6.4kg of titanium-silicon molecular sieve TS-1 with a structure-directing agent content of 12.5% ​​by weight in the pores was added to the stainless steel pressure reactor; Reactor sealed, at 200r. min -1 The temperature was raised to 50°C at a certain stirring speed, and the reaction was carried out for 2 hours; after the reaction was completed and the sample was analyzed, the product was transferred to the rectification tower; the final result was that the conversion rate of acetic acid was 99.2%, the selectivity of n-butyl acetate was 99.5%, and the selectivity of n-butyl acetate was 99.5%. The yield of butyl ester was 98.7%.

Embodiment 2

[0067] 11.1kg of acetic acid and 50.6kg of n-butanol were added to a dry stainless steel pressure reactor, and then 6.2kg of titanium-silicon molecular sieve HTS with a hollow structure having a structure directing agent content of 3.0% by weight was added to the stainless steel pressure reactor; The stainless steel high-pressure reactor is sealed, at 300r. min -1 The temperature was raised to 80°C at a certain stirring speed, and the reaction was carried out for 1 hour; after the reaction was completed and the sample was analyzed, the product was transferred to the rectification tower; the final result was that the conversion rate of acetic acid was 99.3%, the selectivity of n-butyl acetate was 99.3%, and the acetic acid The yield of n-butyl ester was 98.6%.

Embodiment 3

[0073] 9.1kg of acetic acid and 52.1kg of n-butanol were added to a dry stainless steel pressure reactor, and then 12.2kg of titanium-silicon molecular sieve HTS with a hollow structure with a structure-directing agent content of 3.0% by weight was added to the stainless steel pressure reactor; the stainless steel The pressure reactor is sealed, at 600r. min -1 The temperature was raised to 150°C at a constant stirring speed, and the reaction was carried out for 0.5h; after the reaction was completed and the sample was analyzed, the product was transferred to the rectification tower; the final result was that the conversion rate of acetic acid was 99.6%, and the selectivity of n-butyl acetate was 95.1%. The yield of n-butyl acetate was 94.7%.

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Abstract

The invention relates to a method for synthesizing n-butyl acetate. The method comprises the following steps: contacting acetic acid and n-butyl alcohol under the synthetic reaction conditions of n-butyl acetate and in the presence of a catalyst, and recovering to obtain the n-butyl acetate. The method is characterized in that the active ingredient of the catalyst refers to a molecular sieve which is formed by hydrothermal crystallization synthesis and of which the pore passage contains an organic template agent. The method has the advantages of high acetic acid conversion rate, high n-butyl acetate selectivity, energy conservation and environment friendliness.

Description

technical field [0001] The present invention relates to a kind of method of synthesizing n-butyl acetate, say further that the present invention relates to a kind of method that acetic acid and n-butanol react to generate n-butyl acetate under the action of molecular sieve catalyst. Background technique [0002] N-Butyl Acetate is a colorless, transparent, flammable liquid with a slightly lower fruity aroma than Amyl Acetate. It is miscible with alcohols, ketones, esters and most common organic solvents. In addition, although n-butyl acetate has anesthetic and stimulating effects, its acute toxicity is relatively small. Therefore, n-butyl acetate can be used as an organic solvent, extractant or dehydrating agent and is used in industrial production such as varnish, artificial leather, nitrocellulose, medicine, collodion, spices and plastics, and is an important basic organic chemical raw material . [0003] At present, the main industrial production method of n-butyl acet...

Claims

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Application Information

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IPC IPC(8): C07C69/14C07C67/08B01J31/02
Inventor 王宝荣史春风林民朱斌彭欣欣吴国文舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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