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Green method for preparing pinacolone

A green and formaldehyde-based technology, applied in the preparation of heterocyclic compounds, sustainable manufacturing/processing, chemical industry, etc., can solve the problems of increasing environmental protection costs and environmental pollution, uneconomical use of hydrochloric acid, large equipment investment, etc., to achieve equipment investment and the reduction of the site area, the obvious reduction of environmental protection costs and investment, and the effect of saving the exhaust gas recovery device

Active Publication Date: 2019-05-28
上海旭流化学科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The use of hydrochloric acid in the whole reaction is very uneconomical. A large amount of hydrochloric acid is used in the front, and a large amount of hydrochloric acid is released in the back. Tail gas absorption and alkali neutralization are required, resulting in large investment in equipment and increased use of alkali; the use

Method used

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  • Green method for preparing pinacolone
  • Green method for preparing pinacolone
  • Green method for preparing pinacolone

Examples

Experimental program
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Effect test

Embodiment 1

[0037] A 1L four-neck flask for the reaction was connected with a 1m packing column, the top of the packing column was connected to a condenser, a peristaltic pump was used for feeding and discharging, the cooling medium of the condenser was 20°C circulating water, and the four-necked flask was kept at 100°C. Before the reaction, 500 ml of reaction solution was added to the four-neck flask (reaction solution using 80 g of isoamylene raw material, the process was as in Comparative Example 1, and it was started as a full kettle) and the temperature was raised to 100°C. Isopentene (relative specific gravity 0.65, cooled to 10° C.) was fed at a speed of 2 g / min, and after 10 minutes, the paraformaldehyde solution was added with 255 grams of trioxane at a speed of 2.6 g / min (500 grams of 25% hydrochloric acid solution). POM is kept at 60°C, the relative specific gravity is 1.2) feeding, and the material is continuously discharged after 5 minutes. The water phase obtained by separati...

Embodiment 2

[0039] A 200L reactor is used for the reaction, connected to a packed tower with three sections of 2 meters and a diameter of 0.2 meters, and a square condenser is connected externally, and a metering pump is used for feeding and discharging. The condenser is fed with water at 20°C, and the temperature of the reactor is controlled at 100°C. Before the reaction, first add 100L of reaction solution (reaction solution with isoamyl content of 16KG, the process is the same as that of Comparative Example 1) in the reaction kettle and heat up to 100°C. After stabilizing for 1 hour, feed 400 g / min of isoamyl with a pump . After 20 minutes, feed paraformaldehyde / hydrochloric acid solution (300 kilograms of 25% hydrochloric acid, 153 kilograms of paraformaldehyde) at 520 g / min, and discharge continuously at the bottom of the reactor after 10 minutes. The aqueous phase obtained by separation at the discharge port was detected to have a hydrochloric acid concentration of 24.9%. After addi...

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Abstract

The invention discloses a green method for preparing pinacolone, and belongs to the technical field of a fine chemical engineering intermediate. A trioxymethylene (or paraformaldehyde) hydrochloric acid water solution and isoamylene is continuously fed in different positions in a reaction rectifying tower; pinacolone crude products and a hydrochloric acid mixed solution are continuously dischargedat the bottom; organic phases and water phases are continuously separated; the organic phases are distilled to obtain a pinacolone finished product; previous fractions enter trioxymethylene (or paraformaldehyde) and acid water phases return for preparing a trioxymethylene (or paraformaldehyde) acid solution. A set of reaction rectifying tower is used; three-step reaction is controlled to be performed in different positions in one system; three wastes (waste water, waste gas and waste solid) are reduced; the number of personnel is reduced; the equipment utilization rate is improved; the methodbelongs to a green, environment-friendly safe novel process.

Description

technical field [0001] The invention relates to a method for preparing pesticides and organic intermediates, in particular to a green method for synthesizing pinacolone, which belongs to the technical field of fine chemical intermediates. Background technique [0002] Pinacolone, the abbreviation of 3,3-dimethyl-2-butanone, CAS: 75-97-8, is a very important organic fine chemical intermediate, mainly used in pesticides, pharmaceuticals, rubber and other fine In the synthesis of chemicals, there are dozens of triazole pesticides synthesized from pinacolone. [0003] At present, the production process of pinacolone mainly adopts batch reaction, which is carried out in two steps: [0004] The first step is the addition reaction of isopentene and hydrochloric acid at low temperature. The reaction temperature is 5-30°C and it takes 6 hours. High-concentration hydrochloric acid is used to synthesize chloropentane. The oil-water phase is separated, and the water The acid-containin...

Claims

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Application Information

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IPC IPC(8): C07C45/60C07C49/04
CPCY02P20/10
Inventor 杨智深周留扣王岩吴镝
Owner 上海旭流化学科技有限公司
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