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Method for separating and refining isobomyl acetate

A technology of isobornyl acetate and refined ester, which is applied in the field of chemical technology, can solve the problems of reducing the yield of isobornyl acetate, increasing by-products, and increasing the circulation volume, etc., so as to improve selectivity, catalyst life, and product The effect of stable quality and easy production

Active Publication Date: 2012-01-25
福建南平青松化工有限公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

And this part of membrane acid is recycled, due to entrainment of isobornyl acetate, the circulation volume increases, the energy consumption increases, and the yield decreases
In addition, when the crude isobornyl acetate is whitened, due to the excessively long residence time in the evaporator, the by-products increase, which reduces the yield of isobornyl acetate

Method used

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  • Method for separating and refining isobomyl acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Composition in the feed crude ester (1) is water: 0.6%, acetic acid: 9.7%; Camphene: 11.5%; Isobornyl acetate: 73.6%; Miscellaneous ester: 3.6% heavy oil: 1%, crude ester rectification tower T-101 The theoretical plate number is 30 grades, the feed is at the 15th grade, the membrane acid (5) taken out from the side line is at the 8th grade, the vacuum at the top of the tower is -0.093MPa, the reflux ratio is 6, and the acid water (3 ) consists of: water: 7.6%, acetic acid 92.1%, amphene 0.3%; the membrane acid (4) extracted from the side line consists of water: 0.9%, acetic acid: 25.9%, amphene: 71.7%, isoborneol acetate Esters: 1.3%, miscellaneous esters: 0.4%; the crude ester (7) extracted from the tower kettle is composed of: isobornyl acetate: 94.1%, miscellaneous esters: 4.6%, heavy oil: 1.3%.

[0025] The crude ester in the tower kettle is sent to the whitening process, and the evaporator E-102 The vacuum degree of the evaporator is controlled at -0.095MPa, the ...

Embodiment 2

[0028] The separation device of embodiment 2 is the same as that of embodiment 1, and the only difference is that the feed composition and operating conditions have changed.

[0029] When amphene esterification conversion ratio was low, the composition in the feed crude ester (1) was water: 0.4%, acetic acid: 13.0%; Amphene: 15.4%; Isobornyl acetate: 67.4%; Miscellaneous ester: 3.0% heavy oil: 0.8%, crude ester rectification tower T-101 The vacuum at the top of the tower is-0.093MPa, and the reflux ratio is 7, and the acid water (3) produced at the top of the tower consists of: water: 4.6%, 95.2% acetic acid, 0.3% camphene; the membrane acid (4) produced by the side line ) is composed of water: 0.6%, acetic acid: 32.0%, camphene: 67.5%, and the crude ester (7) extracted from the tower kettle is composed of: isobornyl acetate: 94.7%, miscellaneous ester: 4.2%, heavy oil: 1.1% %.

[0030] The crude ester in the tower kettle is sent to the whitening process, and the evaporator ...

Embodiment 3

[0034] The crude ester enters the crude ester rectification tower T-101 , the top temperature of the rectification tower is controlled at 40°C, the vacuum at the top of the tower is controlled at -0.093MPa, the temperature of the bottom of the tower is controlled at 140°C, and the reboiler E-101 The temperature is controlled at 140°C, and the tower bottom liquid (7) is sent to the refined ester evaporator E-102 Perform whitening operation, E-102 The temperature is controlled at 130°C, E-102 The vacuum degree is controlled at -0.095MPa, from E-102The vapor-liquid mixture that comes out enters the refined ester vapor-liquid separation tank V-101 to separate, V-101 A part (11) is sent to the refined ester stripper T-102 Separation of heavy components, T-102 The temperature at the top of the tower is controlled at 130°C, and the temperature at the bottom of the tower is controlled at 140°C. T-102 The vacuum at the top of the tower is controlled at -0.098MPa.

[0035] A...

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Abstract

The invention relates to a method for separating and refining isobomyl acetate. The method is characterized in that: an acetic acid solution containing water is produced on the top of a crude ester rectification tower; a mixture of camphene and acetic acid is mainly obtained through side take-off; a crude product of the isobomyl acetate is produced from the tower; and the crude product enters a refined ester evaporator, is whitened and then enters a refined ester vapor-liquid separation tank for separation so as to obtain high-purity isobomyl acetate. The disadvantages of high energy consumption of batch separation, low product yield and the like existing in the prior art are overcome; acid water is produced from the top of the crude ester rectification tower, crude ester is produced fromthe tower, the clear segmentation is realized by using a single tower, teichoic acid is produced from one side and only contains the acetic acid and the camphene, and when the teichoic acid is used for the circular reaction, the selectivity of the reaction is improved and the service life of a catalyst is prolonged, so the process is advanced and the energy consumption is low; and the method has the advantages of continuous production, compact flow, low energy consumption and the like, and the product is high in yield and has stable quality.

Description

technical field [0001] The invention belongs to the field of chemical technology, and more specifically relates to a method for separating and refining isobornyl acetate. Background technique [0002] Isobornyl acetate, also known as white ethyl ester, is used as a fragrance because of its fragrance and pine leaf smell, mainly used in cosmetics, soaps and indoor disinfectants, indoor air fresheners, indoor spray essences, bath essences and body refreshers Powder raw materials, etc. At the same time, isobornyl acetate is also an important intermediate for the production of synthetic camphor by esterification, and has a large production scale. [0003] Isobornyl acetate is generally produced with camphene and acetic acid as raw materials under the action of a catalyst. The product contains a small amount of water, unreacted raw materials, isobornyl acetate, isomerized by-products and polymerization by-products. After the product needs to be separated, the satisfactory isobor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/14C07C67/54C07C67/52
Inventor 陈尚和危景波王志林高赣闽
Owner 福建南平青松化工有限公司
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