Continuous treatment process and device of neopentyl glycol condensed washing mother liquor

A technology of neopentyl glycol and mother liquor, which is applied in the separation/purification of hydroxyl compounds, organic chemistry, etc., can solve the problems of long operation period, low production efficiency, and large loss of neopentyl glycol, so as to reduce production costs, Effects of increasing processing efficiency and improving appearance characteristics

Active Publication Date: 2015-08-19
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing steam equilibrium distillation process has the following problems: first, the loss of neopentyl glycol is large during the treatment process, and the mass fraction of neopentyl glycol in the wastewater produced from the top of the tank is 2 to 3%, and every ton of neopentyl glycol is processed Alcohol condensation water washing mother liquor, the loss of neopentyl glycol is 20-30 kg; second, the operation period is long, and it takes 20-22 hours to process a batch of 20 tons of neopentyl glycol condensation water washing mother liquor, and the production efficiency is low; third , the color of the treated neopentyl glycol solution is yellowish, and it needs to be decolorized by activated carbon before it can be recycled. The existing process adopts intermittent treatment, and the solution in the tank is kept at high temperature for a long time, resulting in partial carbonization of the organic matter in the solution, and the color is yellowish. 4. Scaling easily occurs in the neopentyl glycol distillation tank, which leads to deviation of heat transfer effect. The neopentyl glycol condensation washing mother liquor contains a small amount of calcium sulfate. After a large amount of water is steamed out by balanced distillation, the calcium sulfate in the tank gradually Accumulation leading to scaling inside the retort walls

Method used

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  • Continuous treatment process and device of neopentyl glycol condensed washing mother liquor

Examples

Experimental program
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Effect test

Embodiment 1

[0031]Implementation example 1: The feed rate of neopentyl glycol condensation water washing mother liquor is 4000 kg / h, the temperature rises from 20°C to 70°C after passing through the primary preheater, and the temperature rises to 90°C after passing through the secondary preheater , The temperature of the bottom material of the rectification tower dropped from 109°C to 75°C, and the steam consumption was 450 kg / hour. The treatment time of 20 tons of neopentyl glycol solution is about 5 hours, the volume of dichloromethane produced at the top of the tower is 800 liters, and the volume of petroleum ether is 500 liters. After the water produced at the top of the tower passes through the water separator, the neopentyl glycol content is 8ppm and the COD is 236 mg / liter, and the mass fraction of neopentyl glycol produced at the bottom of the tower is 70%, wherein dichloromethane and petroleum ether Not detected.

Embodiment 2

[0032] Implementation example 2: The feed rate of neopentyl glycol condensation water washing mother liquor is 4000 kg / h, the temperature rises from 20°C to 75°C after passing through the first-stage preheater, and the temperature rises to 95°C after passing through the second-stage preheater , The temperature of the bottom material of the rectification tower dropped from 108°C to 70°C, and the steam consumption was 400 kg / hour. The treatment time of 20 tons of neopentyl glycol solution is about 5 hours, the volume of dichloromethane extracted from the tower top is 830 liters, and the volume of petroleum ether is 550 liters. After the water produced at the top of the tower passes through the water separator, the content of neopentyl glycol is 9ppm and the COD is 156 mg / liter, and the mass fraction of neopentyl glycol produced at the bottom of the tower is 68%, of which dichloromethane and petroleum ether The concentration is 1ppm.

Embodiment 3

[0033] Implementation example 3: The feed rate of neopentyl glycol condensation water washing mother liquor is 5000 kg / hour, the temperature rises from 20°C to 65°C after passing through the primary preheater, and the temperature rises to 92°C after passing through the secondary preheater , The temperature of the bottom material of the rectification tower dropped from 108°C to 72°C, and the steam consumption was 550 kg / hour. The treatment time of 20 tons of neopentyl glycol solution is about 4 hours, the volume of dichloromethane extracted from the tower top is 850 liters, and the volume of petroleum ether is 520 liters. After the water produced at the top of the tower passes through the water separator, the neopentyl glycol content is 5ppm and the COD is 221 mg / liter, and the concentrated mass fraction of neopentyl glycol produced at the bottom of the tower is 67%, of which dichloromethane and petroleum The ether concentration was 1 ppm.

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Abstract

The invention relates to a continuous treatment device of neopentyl glycol condensed washing mother liquor. The device is characterized by comprising a filter, a primary preheater, a secondary preheater, a rectifying tower, a chromatographic device and a cyclone hydraulic separator, wherein the filter is arranged at the front end of the primary preheater, the primary preheater is connected with the secondary preheater through a pipeline, the rectifying tower is arranged at the rear end of the secondary preheater, a return tank and the chromatographic device are arranged on the top of the rectifying tower, and the cyclone hydraulic separator and a reboiler are arranged on the bottom of the rectifying tower. The invention relates to a continuous treatment process flow of neopentyl glycol condensed washing mother liquor capable of continuously and stably removing organic impurities in the neopentyl glycol condensed washing mother liquor and condensing neopentyl glycol.

Description

technical field [0001] The invention belongs to the separation field of the pharmaceutical industry, and in particular relates to a continuous treatment process and device for neopentyl glycol condensation water washing mother liquor. Background technique [0002] Neopentyl glycol, referred to as NPG, is a white crystalline solid, easily soluble in water, low-carbon alcohols, low-carbon ketones, ethers and aromatic compounds. At present, the synthesis methods of neopentyl glycol mainly include hydrogenation method and methanol method. Neopentyl glycol molecule has a specific neopentyl structure, which contains two primary carbonyl groups, and there is no α-hydrogen atom on the central carbon atom. These characteristics make neopentyl glycol have high thermal and chemical stability , Therefore, it is often used in the production fields such as medicine, chemical industry, paint, pesticide, plastic and petroleum. Among them, in the pharmaceutical industry, neopentyl glycol c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/76
CPCC07C29/76C07C31/20
Inventor 王英龙张震朱兆友张青马艺心
Owner QINGDAO UNIV OF SCI & TECH
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