Process for preparing and extracting tert-butyl acetate

A technology of tert-butyl acetate and acetic acid, which is applied in the field of preparation and purification of tert-butyl acetate, can solve problems such as failure and difficulty in separation and purification of tert-butyl acetate, and achieve reduction of production costs, continuous esterification reaction and separation and purification, and overcome Difficult water separation effect

Active Publication Date: 2009-07-01
HUNAN CHANGLING PETROCHEM SCI & TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantage of this method is that (isobutylene) dimer accumulation and catalyst failure often occur in the tower during the reaction, resulting in the formation of muddy deposits and the need to shut down and clean out the tower, and the dimer of olefins increases The separation and purification of tert-butyl acetate is difficult
So far, the use of acetic acid and C containing a certain amount of isobutylene 4 The reaction obtains crude ester, and the method of obtaining tert-butyl acetate with a purity of more than 99.5% through deacidification, dehydrocarbonation and dealcoholization has not been reported

Method used

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  • Process for preparing and extracting tert-butyl acetate
  • Process for preparing and extracting tert-butyl acetate
  • Process for preparing and extracting tert-butyl acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Acetic acid and C 4 The reaction is acid catalyzed and can be operated in batch or continuous mode. The inner diameter of the reaction tube is 16mm. The catalyst is a strong-acid ion-exchange resin. The loading amount of the catalyst is 30ml to 90ml. The acetic acid is metered in with an advection pump, and the temperature is controlled by a temperature control device. The raw materials used in experiments T-1, T-2, T-3, and T-4 were acetic acid and C 4 , acetic acid is fed into the esterification tower equipped with ion-exchange resin catalyst at a certain rate to maintain a stable C 4 Tail gas flow rate (60ml / min), pressure 0.8MPa, change reaction temperature, react for 6-7 hours and take samples for analysis. The crude ester is deacidified at 85-100°C, dehydrocarbonized at 70-85°C, dealcoholized at 78-90°C, and finally rectified at 90-100°C to obtain tert-butyl acetate product. The results are shown in Table 1.

[0018] Table 1, change the result of reaction temp...

Embodiment 2

[0022] The raw materials used in experiments T-5, T-6, T-8, T-10 and T-11 are acetic acid, water and C 4 , the raw materials used in experiment T-7 were acetic acid, alcohol and C 4 , experiment T-9 with acetic acid and C 4 Be raw material, keep reaction temperature be 65 ℃, change acetic acid space velocity and reaction pressure, other conditions are the same as embodiment 1. The crude ester is deacidified at 85-100°C, dehydrocarbonized at 70-85°C, dealcoholized at 78-90°C, and finally rectified at 90-100°C to obtain tert-butyl acetate product. The results are shown in Table 2.

[0023] Table 2, change the result of acetic acid space velocity and reaction pressure synthesis thick tert-butyl acetate

[0024]

[0025]

Embodiment 3

[0027] The tert-butyl acetate crude product (containing tert-butyl acetate 18.97%) that is obtained by the first esterification tower circulates into the second esterification tower, and supplemented C 4 Esterification occurs, controlling C 4 Exhaust gas flow 60ml / min. Keep the reaction temperature at 65°C, change the reaction pressure and the crude tert-butyl acetate injection space velocity to carry out experiments T-12, 13, 14, 15, and 16, and other conditions are the same as in Example 1, and react for 3 hours and take samples for analysis. The crude ester is deacidified at 85-100°C, dehydrocarbonized at 70-85°C, dealcoholized at 78-90°C, and finally rectified at 90-100°C to obtain tert-butyl acetate product. The results are shown in Table 3.

[0028] Table 3, change reaction pressure and the result of tert-butyl acetate crude product injection space velocity synthetic tert-butyl acetate cyclic reaction

[0029]

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Abstract

The invention discloses a method for preparing and purifying tert-butyl acetate. Acetic acid and C4 containing isobutene are continuously added to an esterification tower equipped with a strong acid ion exchange resin catalyst, and the molar ratio of acetic acid and isobutene is 1:0.30 to 1:0. 5.00, the feed space velocity of acetic acid is 0.5~5.0h-1, the amount of catalyst is 30~90ml, the pressure is 0.5~2.0MPa, and the reaction temperature is 30~110℃, the esterification reaction is carried out to obtain the crude ester; the crude ester is sent to The separation tower is obtained by controlling the reflux temperature of the top gas phase at 85-100°C for deacidification, 70-85°C for dehydrocarbonation, 78-90°C for alcohol removal, and finally rectification at 90-100°C tert-butyl acetate product. The invention uses abundant C4 in refinery as raw material, which can greatly reduce the production cost of the product, and also overcomes the problem of water separation in the traditional acid / alcohol process, which leads to increased energy consumption; realizes continuous esterification and separation Purification, the product content of tert-butyl acetate can reach more than 99.5%.

Description

1. Technical field: [0001] The present invention relates to a kind of method for preparing tert-butyl acetate, particularly relate to a kind of method with acetic acid and C 4 A method for preparing and purifying tert-butyl acetate as a raw material. 2. Background technology: [0002] Tert-butyl acetate is a colorless liquid that can be mixed with alcohol and ether, soluble in acetic acid, almost insoluble in water, is an excellent gasoline anti-shock agent, and can be used as a solvent for nitrocellulose, etc. [0003] At present, the methods for industrially producing tert-butyl acetate include: 1. acetic anhydride method: taking tert-butyl alcohol and acetic anhydride as raw materials to synthesize tert-butyl acetate, wherein the catalysts used include zinc chloride, lithium chloride, lithium perchlorate, nitric acid Cerium ammonium, pyridine, triethylamine, 4-dimethylaminopyridine (DMAP), tin tetrachloride, etc., but zinc chloride is easy to absorb moisture, organic ami...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/04C07C67/08C07C69/14
Inventor 徐斌黄华谢琼玉胡莲佑赵映王伟余忠波
Owner HUNAN CHANGLING PETROCHEM SCI & TECH DEV CO LTD
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