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Method for preparing high-purity potassium tert-butoxide with tert-butanol-water azeotropic solution and potassium hydroxide

A technology of potassium hydroxide and potassium tert-butoxide, applied in the field of preparation of high-purity potassium tert-butoxide, which can solve the problems of high cost, backward technology, dangerous operation, etc.

Inactive Publication Date: 2016-05-04
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Domestic manufacturers all use this method to produce, the technology is backward, the operation is dangerous, and the cost is expensive

Method used

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  • Method for preparing high-purity potassium tert-butoxide with tert-butanol-water azeotropic solution and potassium hydroxide
  • Method for preparing high-purity potassium tert-butoxide with tert-butanol-water azeotropic solution and potassium hydroxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Weigh 150.3g of 88wt% tert-butanol-water azeotropic solution and 15.3g of potassium hydroxide into the mixing tank R1 for mixing, heat and keep the temperature to 40°C, rotate at 200r / min, stir for 2.5h, and enter the separation tank V1 for a minute Floor.

[0035] (2) 10.9 g of the liquid in the lower layer of the separation tank V1, that is, the water layer, enters the drier D1, evaporates and dries under the protection of nitrogen, and recovers 15.1 g of potassium hydroxide.

[0036] (3) After mixing 139.2g of the upper liquid of the separation tank V1, that is, the alcohol layer and 7.5g of potassium hydroxide, it is placed in the still T1 of the batch rectification column, and cyclohexane is pumped into the top of T1 at a rate of 10g / min, and the timing is started. After 15 minutes, stop cyclohexane feed, a total of 150.2g, control tower top temperature 70 ° C, tower bottom temperature 83 ° C; tert-butanol, water and cyclohexane azeotrope distilled from the top...

Embodiment 2

[0039] (1) Weigh 120.1g of 88wt% tert-butanol-water azeotropic solution and 10.8g of potassium hydroxide into the mixing tank R1 for mixing, heat and keep the temperature to 40°C, the rotation speed is 200r / min, stir for 2.5h, and enter the separation tank V1 for a minute Floor.

[0040] (2) 8.2 g of the liquid in the lower layer of the separation tank V1, that is, the water layer, enters the drier D1, evaporates and dries under the isolation of air (under the protection of nitrogen), and recovers 10.4 g of potassium hydroxide.

[0041] (3) After mixing 112.0 g of the upper liquid of the separation tank V1, that is, the alcohol layer and 6.1 g of potassium hydroxide, it is placed in the still T1 of the batch rectification column, and cyclohexane is pumped into the top of the T1 tower at a rate of 10 g / min, and the timing is started. After 15 minutes, the feeding of cyclohexane was stopped, a total of 149.7g of cyclohexane, and the temperature at the top of the tower was contro...

Embodiment 3

[0044] (1) Weigh 350.7g 88wt% tert-butanol-water azeotropic solution and 31.2g potassium hydroxide into the mixing tank R1 for mixing, heat and keep the temperature to 50°C, rotate at 200r / min, stir for 3h, and enter the separation tank V1 for stratification .

[0045] (2) 22.1 g of the liquid in the lower layer of the separation tank V1, that is, the water layer, enters the drier D1, evaporates and dries under the protection of nitrogen, and recovers 30.8 g of potassium hydroxide.

[0046] (3) After mixing 296.1g of the upper liquid of the separation tank V1, that is, the alcohol layer and 20.2g of potassium hydroxide, it is placed in the still T1 of the batch rectification column, and cyclohexane is pumped into the top of T1 at a rate of 10g / min, and the timing is started. After 40min, stop cyclohexane feeding, 401.6g in total, control tower top temperature 72 ℃, tower still temperature 84 ℃; Tertiary butanol, water and cyclohexane azeotrope distill from tower top, obtain to...

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Abstract

The invention discloses a method for preparing high-purity potassium tert-butoxide with a tert-butanol-water azeotropic solution and potassium hydroxide. The potassium hydroxide serves as a salting-out water separating agent to concentrate the tert-butanol-water azeotropic solution, and the concentrated tertiary butanol solution and a certain amount of potassium hydroxide are reacted in a semi-batch rectifying tower kettle; meanwhile, cyclohexane and tertiary butanol serve as water carrying agents, and water generated in the reaction process is separated and brought out in real time. After the reaction is over, the generated tertiary butanol solution of the potassium tert-butoxide is dried to be crystallized under the protection of nitrogen, the potassium tert-butoxide with the purity of 98.2wt% or above can be obtained, and the tertiary butanol with the purity of 99.0wt% or above can be obtained in a vapor condensation mode; overhead products of a semi-batch rectifying tower is layered through standing, the cyclohexane and the tertiary butanol serve as the water carrying agent, returns to the semi-batch rectifying tower and is recycled, and after the tert-butanol-water solution is rectified, the obtained tert-butanol-water azeotropic solution is recycled.

Description

technical field [0001] The invention relates to a preparation method of a fine chemical intermediate, in particular to a preparation method of high-purity potassium tert-butoxide. Background technique [0002] Potassium tert-butoxide is an intermediate widely used in fine chemical industry. It is often used in rearrangement, ring opening, etherification, esterification and various chemical reactions at carbonyl α-position in organic synthesis such as chemical industry, medicine, pesticide, printing and dyeing, etc. reaction. At present, the conventional preparation method of potassium tert-butoxide is to utilize anhydrous tert-butanol to react with metal potassium. Domestic manufacturers all use this method to produce, the technology is backward, the operation is dangerous, and the cost is expensive. [0003] Tert-butanol and water can form a binary azeotrope, which is purified by ordinary rectification, and the product concentration is only about 88wt%. The tert-butanol-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/70C07C31/30C07C29/78C07C31/12C07C29/82
CPCC07C29/70C07C29/78C07C29/82C07C31/30C07C31/12
Inventor 于英民辛坤
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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