Process for preparing and extracting tert-butyl acetate

A technology of tert-butyl acetate and acetic acid, applied in the field of preparation and purification of tert-butyl acetate, can solve problems such as difficulty in separation and purification of tert-butyl acetate, ineffectiveness, etc., achieve continuous esterification reaction and separation and purification, reduce production costs, overcome The effect of difficult water separation

Active Publication Date: 2006-12-27
HUNAN CHANGLING PETROCHEM SCI & TECH DEV CO LTD
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  • Abstract
  • Description
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  • 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

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Acetic acid and C 4 The reaction is an acid-catalyzed reaction, which can be a batch or continuous operation mode. The inner diameter of the reaction tube is 16mm, the catalyst adopts a strong acid type ion exchange resin, the catalyst filling amount is 30ml~90ml, the acetic acid is metered in with a flat flow pump, and temperature control equipment is used for temperature control. The raw materials used in experiments T-1, T-2, T-3, and T-4 are 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 The exhaust gas flow rate (60ml / min), the pressure is 0.8MPa, the reaction temperature is changed, and the reaction takes 6-7 hours to sample 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] ...

Embodiment 2

[0020] The raw materials used in experiments T-5, T-6, T-8, T-10, T-11 are acetic acid, water and C 4 , The raw materials used in experiment T-7 are acetic acid, alcohol and C 4 , Experiment T-9 uses acetic acid and C 4 As the raw material, keep the reaction temperature at 65°C, change the acetic acid space velocity and the reaction pressure, and other conditions are the same as in Example 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.

[0021] Test number

Embodiment 3

[0023] The crude tert-butyl acetate product (containing 18.97% tert-butyl acetate) obtained from the first esterification tower is recycled into the second esterification tower, and supplemented C 4 Esterification reaction occurs, control C 4 The exhaust gas flow rate is 60ml / min. Keep the reaction temperature at 65°C, change the reaction pressure and the injection space velocity of the crude product of tert-butyl acetate to perform experiments T-12, 13, 14, 15, 16, and other conditions are the same as in Example 1, and take samples for analysis after 3 hours of reaction. 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.

[0024] Test number

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Abstract

The invention discloses a preparing and extracting method of tert-butyl acetate, which is characterized by the following: adding acetate and C4 with isobutene continuously at 1:0.30-1:5.00 molar rate in the esterification tower with strong acid ionic exchange resin catalyst; setting inlet air-speed of acetate at 0.5-5.0 h-1 and catalyst quantity at 30-90 ml and pressure at 0.5-2.0 Mpa at 30-110 deg.c; obtaining coarse ester; sending ester in the separating tower; controlling top-gas reflux temperature at 85-100 deg.c to deacidify; dehydrocarbylating at 70-85 deg.c; dealcoholizing at 78-90 deg.c; rectifying between 90 and 100 to obtain the product.

Description

1. Technical Field: [0001] The invention relates to a method for preparing tert-butyl acetate, in particular to a method for preparing acetic acid and C 4 It is a method for preparing and purifying tert-butyl acetate as raw materials. 2. Background technology: [0002] Tert-butyl acetate is a colorless liquid that can be mixed with alcohol and ether, soluble in acetic acid, and almost insoluble in water. It is an excellent gasoline shockproof agent and can be used as a solvent for nitrocellulose. [0003] At present, the industrial production methods of tert-butyl acetate include: ①Acetic anhydride method: Use tert-butanol and acetic anhydride as raw materials to synthesize tert-butyl acetate. The catalysts used are zinc chloride, lithium chloride, lithium perchlorate, and nitric acid. Cerium ammonium, pyridine, triethylamine, 4-dimethylaminopyridine (DMAP), tin tetrachloride, etc., but zinc chloride is easy to absorb moisture, organic amines have irritating odor and certain toxi...

Claims

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Application Information

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Patent Type & Authority Applications(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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