Method for mass producing butyl acetate by reactive distillation method and using sulfuric acid as catalyst

A technology of butyl acetate and reactive distillation, applied in the direction of chemical instruments and methods, physical/chemical process catalysts, carboxylate preparation, etc., can solve problems such as difficult to achieve, poor product quality, high cost of use, etc., to achieve corrosion Lightening, good separation effect, and the effect of solving corrosion problems

Active Publication Date: 2006-10-11
NANTONG BAICHUAN NEW MATERIAL CO LTD +1
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Problems solved by technology

Adopt such intermittent reaction technique, the one, production efficiency can't be improved, and production capacity is difficult to improve, and energy consumption is big, and production cost is high; 》Requirements for superior products
[0004] In the 1990s, with the development and application of reactive distillation technology, some units in China began to study the use of this technology to produce butyl acetate, but generally solid acids such as heteropoly acids were used as catalysts, which have not been used. The technology combining liquid as catalyst and reactive distillation has been applied to industrial production
[0005] The use of solid acid as a catalyst has many disadvantages: first, this catalyst is very expensive, and its catalytic activity will decrease after a period of use, it is very troublesome to replace, and the cost of use is very high; , and it is easy to cause impurities to accumulate in the esterification tank or reactive distillation tower, which affects the evaporation of the material and ultimately affects the quality of the product; the third is that the solid catalyst is not like a liquid catalyst, it is difficult to achieve homogeneous catalysis, and the solid It is difficult to achieve a uniform heat transfer effect, and it is easy to cause local overheating, coking of reactants, etc., which affects product quality and production efficiency; fourth, if solid acid is used as a catalyst, it is difficult to increase production capacity, and the annual cost of a single set of equipment The output is basically less than 10,000 tons, and it is difficult to form a large-scale production capacity
[0007] Chinese patent ZL 94108405.1 discloses a method and equipment for producing n-butyl acetate by continuous catalytic rectification, but its reactive distillation equipment adopts a tower-type device, and the content of n-butyl acetate generated by it is only (95-97 )%, which is only equivalent to the requirements of qualified products in the GB / T 3729-91 standard, far below the requirements of contemporary butyl acetate users
[0008] Chinese patent ZL 97121674.6 discloses a continuous process for the production of butyl acetate, using heteropolyacids as catalysts, and does not use reactive distillation
[0009] The method for continuously producing butyl acetate disclosed in Chinese patent ZL 00107970.0, although sulfuric acid is also used as a catalyst, does not adopt the reactive distillation method

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  • Method for mass producing butyl acetate by reactive distillation method and using sulfuric acid as catalyst

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specific Embodiment approach

[0031] see figure 1, the whole production system is mainly composed of four towers, namely reactive distillation tower 6, azeotropic tower 9, recovery tower 12 and ester rectification tower 14. The reactive distillation column and the azeotropic column can be combined into one column, that is, the azeotropic column is placed above the reactive distillation column, which is a reactive distillation column in the classical sense. But in this case, the tower will be made very high, and corresponding auxiliary facilities need to be built to protect the tower and maintain its normal operation, which is not very economical. For this reason, the present invention divides the reactive distillation column in the classical sense into two columns—a reactive distillation column and an azeotropic column in practical applications. The specific embodiment of the present invention is as follows:

[0032] The raw material acetic acid is pumped into the acetic acid preheater 1 for preheating, ...

Embodiment 1

[0069] Acetic acid adopts the first-class product with a main content of about 99.5%, and the flow rate is 4.3T / h; n-butanol adopts the superior product with a content greater than 99.5%, and the flow rate is 5.4T / h; concentrated sulfuric acid adopts the superior product with a content greater than 98%. The flow rate is 0.05T / h.

[0070] The temperature of the acetic acid and butanol preheaters are both 108°C and the pressure is 155kPa, 1 # and 2 # The temperature of the pre-reactor is 110°C, the pressure is 150kPa; the top temperature of the reactive distillation tower is 100°C, the pressure is 130kPa, the bottom temperature is 130°C, and the pressure is 150kPa; The temperature at the bottom of the tower is 98°C and the pressure is 130kPa; the temperature at the top of the recovery tower is 98°C and the pressure is 100kPa; the temperature at the bottom of the tower is 103°C and the pressure is 120kPa; The discharge temperature of n-butyl acetate finished product is 126.5 DE...

Embodiment 2

[0072] The flow rate of raw material acetic acid is 4.0T / h, the flow rate of n-butanol is 5.0T / h, and other process conditions are all constant, and the content of n-butyl acetate in the 5 bottom initial esters of reactive distillation column is 98.3%, and the extraction The n-butyl acetate is 7.7T / h, the content of n-butyl acetate is 99.91%, and other indicators meet the requirements of superior products.

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Abstract

The refers to a mass production method of isobutyl acetate which uses hydric sulphate as accelerant by reaction fractional distillation, using ethyl acetate and butyl alcohol as raw material, concentrated sulfuric acid as accelerant, continue producing isobutyl acetate by reaction fractional distillation, the whole production system contains three towers, reaction fractionating tower, azeotropy tower and eater fractionating tower, the reaction fractionating tower, azeotropy tower are setted side by side. The ethyl acetate, butyl alcohol and concentrated sulfuric acid are drived into feeder column plate of reaction fractionating tower after esterification prereaction, the gas phase of prereactor going into feeding phase of reaction fractionating tower, the gas phase on top of reaction fractionating tower going into column plate of cellar of azeotropy towder, the liquid phase of towder bottom going into mesomere of eater fractionating tower, the butyl product is continue discharged from side tower. This invention combines the technique which using sulfuric as accelerant by mean improvement of reaction fractional distillation technique, not only ustilizing the advanced technology of reaction fractional distillation, but also making the liquid accelerant's characters of convenience to operate, easy to enlarge production scale getted adequate use.

Description

Technical field: [0001] The present invention relates to a kind of method of producing butyl acetate, especially relate to a kind of continuous, large-scale production method of butyl acetate that combines sulfuric acid as catalyst and reactive distillation method. Background technique: [0002] Butyl acetate is an environmentally friendly ester solvent that is easily degraded in nature and can replace aromatic solvents such as toluene and xylene. It is widely used in coatings, paints, inks, adhesives and medicines. [0003] The early production method of butyl acetate generally uses sulfuric acid as a catalyst, and performs intermittent esterification first. After the reaction is completed, it is neutralized with soda ash, and then refined by distillation. Adopt such intermittent reaction technique, the one, production efficiency can't be improved, and production capacity is difficult to improve, and energy consumption is big, and production cost is high; 》Requirements for...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08B01J27/02C07C67/52C07C69/14
CPCY02P20/10
Inventor 郑铁江
Owner NANTONG BAICHUAN NEW MATERIAL CO LTD
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