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Method for preparing dichloropropanol by recycling impurity-containing phosphate flame retardant industrial byproduct HCl

A technology for industrial by-product, dichloropropanol, is applied in the field of preparing dichloropropanol from resources, can solve the problem of high production cost, and achieve the effects of reducing environmental protection expenditure, reducing environmental pollution and high product yield

Pending Publication Date: 2022-04-01
ZHEJIANG WANSHENG
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, the preparation method of dichloropropanol in China is mainly based on the glycerin method, but basically high-purity HCl gas is used as the raw material, and the production cost is relatively high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The impurities contained in bisphenol A-bis (diphenyl phosphate) BDP by-product HCl are phosphorus impurities and phenolic impurities, and the phosphorus impurities are mainly POCl 3 and a small amount of other phosphorus compound impurities, the total phosphorus content is 5000ppm. The phenolic impurities in the BDP production process are basically phenol, that is, the content of phenol in the by-product HCl is 1000ppm.

[0025] Add 12kg of glycerin into a 30L glass reactor and raise the temperature to 130±5°C, add 1.8kg of adipic acid and stir for 15min until the mixture is uniform. Excessive BDP by-product HCl gas (contained impurity content: total phosphorus 5000ppm, phenol 1000ppm) is sequentially passed into chlorinated paraffin and saturated hydrochloric acid aqueous solution, and then continuously passed into the glass reactor. The condensable steam at 20°C evaporated at high temperature was condensed and collected in the fraction collection bottle, and the rea...

Embodiment 2

[0028] Some phosphate ester flame retardant production processes also use ethanol as a solvent. At this time, the impurities contained in the by-product HCl are phosphorus impurities and alcohol impurities. In TEP by-product HCl, phosphorus impurities are mainly POCl 3 and a small amount of other phosphorus compound impurities, the total phosphorus content is 5500ppm, and the ethanol content is 2000ppm.

[0029] Add 12kg of glycerin into a 30L glass reactor and raise the temperature to 130±5°C, add 1.8kg of adipic acid and stir for 15min until the mixture is uniform. Continuously and stably pass excess TEP by-product HCl (contained impurity content: total phosphorus 5500ppm, ethanol 2000ppm) into saturated hydrogen chloride glycerin solution, saturated hydrochloric acid aqueous solution, and then continue to pass into the glass reactor. The condensable vapor at 20°C evaporated at ±5°C was condensed and collected in the fraction collection bottle, and the reaction was continue...

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Abstract

The invention discloses a method for preparing dichloropropanol by recycling an impurity-containing phosphate flame retardant industrial byproduct HCl, the impurity-containing phosphate flame retardant industrial byproduct HCl is an impurity-containing HCl gas, and the impurities contained in the impurity-containing HCl gas comprise one or a mixture of more than two of phosphorus impurities, phenol impurities and alcohol impurities; the method comprises the following steps: introducing an impurity-containing flame retardant industrial byproduct HCl gas into an impurity-soluble but insoluble or indissolvable HCl gas solution or solvent, removing impurities to obtain high-purity HCl, and reacting the high-purity HCl with glycerol under the catalysis of adipic acid at 130-135 DEG C for 15-20 hours to prepare dichloropropanol. According to the method disclosed by the invention, the industrial byproduct HCl of the flame retardant is reasonably recycled, the hydrogen chloride after impurity removal can be used as high-purity HCl gas to be directly applied to preparation of downstream high-added-value products, the treatment process is simplified, the treatment cost is reduced, the environmental pollution caused by the industrial byproduct HCl of the flame retardant is reduced, the environmental protection expenditure is reduced, the product yield is high, and the purity is high; the energy consumption is low, and the green goal of sustainable production is achieved.

Description

technical field [0001] The invention relates to a method for preparing dichloropropanol from resource recovery of impurity-containing phosphoric acid ester flame retardant industrial by-product HCl. Background technique [0002] Flame retardants produce a lot of by-product HCl gas in the industrial production process. In the prior art, the treatment method is usually to produce by-product hydrochloric acid with a concentration of 10-37% after absorption. Because the acid contains some organic impurities, it cannot be used as an industrial product. The direct reuse of hydrochloric acid has caused a large environmental protection expenditure and polluted the environment to a certain extent. However, if the hydrochloric acid is prepared into high-purity HCl gas through absorption and then desorption, a large economic expenditure will be generated. If the by-product HCl of the flame retardant can be removed by this method to obtain high-purity HCl gas, the environmental protecti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/62C07C31/36C01B7/07
Inventor 李旭锋褚昭宁朱嘉德斯鑫磊田克乐杨爱丽
Owner ZHEJIANG WANSHENG
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