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Method for preparing 2, 2-dimethyl-1, 3-epoxypropane

A technology of propylene oxide and dimethyl group, which is applied in the field of preparation of organic chemical intermediates, can solve the problems of difficult solid-liquid separation operation, insufficient saponification reaction, and high impurity boiling point, achieves good mass transfer and heat transfer effect, and suppresses side effects. Simple effect of product generation and solid-liquid separation

Active Publication Date: 2019-11-22
QINGDAO UNIV OF SCI & TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the saponification reaction is insufficient in the existing operation, and the yield of 2,2-dimethyl-1,3-epoxypropane is low (<50%)
And because contain 30~40% impurity in still raffinate, the boiling point of impurity is higher, color is deep, viscosity is big
After the saponification reaction, the raffinate has dark color, complex composition and high viscosity; the raffinate is divided into oil phase, water phase and solid salt.

Method used

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  • Method for preparing 2, 2-dimethyl-1, 3-epoxypropane
  • Method for preparing 2, 2-dimethyl-1, 3-epoxypropane

Examples

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Effect test

Embodiment 1

[0038] (1) Refining and purifying of the by-product 2,2-dimethyl-3-chloropropanol produced by ibuprofen:

[0039] use figure 1For the shown rectification device, use a vacuum pump to evacuate, control the absolute pressure in the four-necked flask one at 20kPa, put cooling water into the condenser one, heat the four-necked flask one, and keep the rectifying temperature at 150°C. After 1 hour, the temperature was raised to 180°C for 0.5 hours, and 2,2-dimethyl-3-chloropropanol was evaporated from the top of the device into the receiving bottle 1 with a purity of 95%; when the temperature at the top of the device reached 130°C , turn off the vacuum pump, open the vent valve, balance the internal and external pressure of the system, and put the residual liquid into the waste liquid bucket.

[0040] (2) Saponification reaction of 2,2-dimethyl-3-chloropropanol:

[0041] The mass concentration is 35% sodium hydroxide solution and phase transfer catalyst dodecyltrimethylammonium br...

Embodiment 2

[0045] (1) Refining and purifying of the by-product 2,2-dimethyl-3-chloropropanol produced by ibuprofen:

[0046] use figure 1 For the shown rectification device, use a vacuum pump to evacuate, control the absolute pressure in the four-necked flask one at 10kPa, feed cooling water into the condenser one, heat the four-necked flask one, and keep the rectification temperature at 13°C. After 2 hours, the temperature was raised to 160°C for 1 hour, and 2,2-dimethyl-3-chloropropanol was evaporated from the top of the device into the receiving bottle 1 with a purity of 96%; when the temperature at the top of the device reached 120°C , turn off the vacuum pump, open the vent valve, balance the internal and external pressure of the system, and put the residual liquid into the waste liquid bucket.

[0047] (2) Saponification reaction of 2,2-dimethyl-3-chloropropanol:

[0048] Get the waste lye 680g after the filtration that embodiment one obtains, record its sodium hydroxide content ...

Embodiment 3

[0053] (1) Refining and purifying of the by-product 2,2-dimethyl-3-chloropropanol produced by ibuprofen:

[0054] use figure 1 For the shown rectification device, use a vacuum pump to evacuate, control the absolute pressure in the four-necked flask one at 30kPa, put cooling water into the condenser one, heat the four-necked flask one, and keep the rectification temperature at 120°C. After 2.5 hours, the temperature was raised to 170°C for 1 hour, and 2,2-dimethyl-3-chloropropanol was evaporated from the top of the device into the receiving bottle 1 with a purity of 95.6%; when the temperature at the top of the device reached 125°C , turn off the vacuum pump, open the vent valve, balance the internal and external pressure of the system, and put the residual liquid into the waste liquid bucket.

[0055] (2) Saponification reaction of 2,2-dimethyl-3-chloropropanol:

[0056] Get the filtered waste lye 600g that embodiment one obtains, record its sodium hydroxide content 37.5%, a...

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Abstract

The invention discloses a method for preparing 2, 2-dimethyl-1, 3-epoxypropane, which comprises the following steps of (1) refining and purifying a byproduct 2, 2-dimethyl-3-chloropropanol in the ibuprofen production; (2) carrying out the saponification reaction of 2, 2-dimethyl-3-chloropropanol, mixing a sodium hydroxide solution with a phase transfer catalyst, conveying the mixture and the 2, 2-dimethyl-3-chloropropanol into a tangential flow tubular reactor at the same time, starting stirring for continuous reaction, and discharging a 2, 2-dimethyl-1, 3-epoxypropane crude product after thereaction is completed; and (3) purifying the 2, 2-dimethyl-1, 3-epoxypropane crude product. According to the method disclosed by the invention, the high yield of the 2, 2-dimethyl-propylene oxide is realized, the excessive sodium hydroxide solution can be recycled, the reaction process is continuous, and the production safety is improved; the method is suitable for the continuous saponification reaction and is good in mass and heat transfer effect and high in production efficiency.

Description

technical field [0001] The invention relates to a method for preparing an organic chemical intermediate, in particular to a method for preparing 2,2-dimethyl-1,3-propylene oxide by using a by-product produced by ibuprofen. Background technique [0002] The molecule of 2,2-dimethyl-1,3-epoxypropylene contains four-membered rings, and there is a dimethyl structure, and there is no hydrogen atom at the β position, which makes it have high chemical stability and thermal stability , Under the catalysis of protonic acid, it can be hydrolyzed to generate neopentyl glycol. Neopentyl glycol (NPG) is widely used in the production of unsaturated resins, oil-free alkyd resins, plasticizers for polyurethane foams and elastomers, surfactants, insulating materials, polymerization inhibitors, synthetic aviation lubricants At the same time, neopentyl glycol is also an excellent solvent, which can be used for the selective separation of cycloalkyl hydrocarbons and aromatic hydrocarbons; neop...

Claims

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Application Information

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IPC IPC(8): C07D305/06
CPCC07D305/06
Inventor 岳金彩杨安明杨霞郑世清钟洁水秦利涛寇祖兴孙科
Owner QINGDAO UNIV OF SCI & TECH
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