Analyzing and monitoring method for circulating mother liquor during production of 1,2-dichloroethane

A technology of circulating mother liquid and dichloroethane, which is applied in the direction of analyzing materials, measuring devices, and material separation, can solve the problems of unsatisfied, unseen, and lack of standards and specific methods for analysis and monitoring, and achieve accurate analysis results and easy operation. Simple process and good reproducibility

Active Publication Date: 2014-11-26
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be found in production that the fresh mother liquor will turn into a turbid dark brown liquid after being put into operation for a short period of time, which makes the analysis and determination of the mother liquor components more difficult, manifested in: the mother liquor cannot be used directly due to the existence of various solid components Chromatography for normal analysis; at the same time, the solid particles in the mother liquor cannot be completely removed by ordinary sedimentation and filtration methods, so simple treatment often cannot meet the conditions for direct analysis by chromatography
So far, there are no relevant standards and specific methods for the analysis and monitoring of the mother liquor of 1,2-dichloroethane production, and no relevant literature reports have been seen.

Method used

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  • Analyzing and monitoring method for circulating mother liquor during production of 1,2-dichloroethane
  • Analyzing and monitoring method for circulating mother liquor during production of 1,2-dichloroethane
  • Analyzing and monitoring method for circulating mother liquor during production of 1,2-dichloroethane

Examples

Experimental program
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Effect test

Embodiment 1

[0054] Embodiment 1: Get production mother liquor 80mL, weigh 108.216g, filter with weighed filter paper, after filtering, weigh the quality of filter paper and residue, obtain the quality of residue 2.651g; Mother liquor after filtration uses distillation range measurement For instrumental distillation, the condensation temperature of the distillation system is set to 0°C in advance, and the receiving bottle is installed so that the liquid outlet at the end of the condenser tube is at the bottom of the receiving bottle, and the bottle mouth is kept airtight. After reaching the set condensation temperature, take the filtered production mother liquor into the distillation flask, insert a thermometer, and adjust the position of the distillation flask to make it stand upright. Connect the branch pipe of the distillation flask to the condensation pipe tightly with a silicone rubber stopper, and the branch pipe goes deep into the condensation pipe 25 ~ 50mm, gradually increase the d...

Embodiment 2

[0068] Example 2: Take 50 mL of the production mother liquor, weigh 67.521 g, filter with weighed filter paper, weigh the quality of the filter paper and the residue after filtration, and obtain the quality of the filter residue of 1.663 g. The filtered mother liquor is distilled using a distillation range tester. Set the condensation temperature of the distillation system to -10°C in advance, install the receiving bottle so that the liquid outlet at the end of the condenser tube is at the bottom of the receiving bottle, and keep the bottle mouth tightly closed. After reaching the set condensation temperature, take the filtered production mother liquor into the distillation flask, insert a thermometer, and adjust the position of the distillation flask to make it stand upright. Connect the branch pipe of the distillation flask to the condensation pipe tightly with a silicone rubber stopper, and the branch pipe goes deep into the condensation pipe 25 ~ 50mm, gradually increase t...

Embodiment 3

[0082] Example 3: Take 80mL of the production mother liquor, weigh 107.932g, filter with weighed filter paper, weigh the quality of the filter paper and the residue after filtration, and obtain the quality of the filter residue 2.638g. The filtered mother liquor is distilled using a distillation range tester. Set the condensation temperature to 8°C, install the receiving bottle so that the liquid outlet at the end of the condenser tube is at the bottom of the receiving bottle, and keep the bottle mouth tightly closed. After reaching the set condensation temperature, take the filtered production mother liquor into the distillation flask, insert a thermometer, and adjust the position of the distillation flask to make it stand upright. Connect the branch pipe of the distillation flask to the condensation pipe tightly with a silicone rubber stopper, and the branch pipe goes deep into the condensation pipe 25-50mm, gradually increase the distillation temperature to 95°C, and closel...

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Abstract

The invention discloses an analyzing and monitoring method for a circulating mother liquor during production of 1,2-dichloroethane. The analyzing and monitoring method comprises the steps of firstly sampling and weighing the mother liquor; carrying out preliminary filtration; weighing the mass of filter residues; distilling the filtered mother liquor; pre-setting a condensing temperature of a distillation system at -10 DEG C-20 DEG C; starting a heating device of the distillation device when a temperature reach the set condensing temperature; raising a distillation temperature to 80 DEG C-120 DEG C gradually; stopping distillation when the temperature stops increasing and starts to decrease under a continuously heating state; cooling to a room temperature; weighing the mass of the distilled residues; sampling and injecting a distillate into a gas chromatograph; normalizing corrected area to obtain chromatographic analysis results of various low-boiling point components; and converting by substituting the masses of the filter residues and the distilled residues into a formula to obtain the content of the various low-boiling point components in the mother liquor. The method provided by the invention is simple to operate and accurate in analysis results, and has good repeatability. The method is helpful to take measures in advance so as to prevent deterioration of ethylene chlorination.

Description

technical field [0001] The invention relates to a method for analyzing and monitoring the circulating mother liquor of 1,2-dichloroethane production. Background technique [0002] Ethylene or dilute ethylene and chlorine can generate 1,2-dichloroethane through direct chlorination reaction, and the direct chlorination of liquid phase method to produce 1,2-dichloroethane is based on 1,2-dichloroethane with solid catalyst Carried out in the ethane circulation mother liquor, the addition reaction of ethylene and chlorine is completed in the 1,2-dichloroethane mother liquor circulation system to generate 1,2-dichloroethane, and the 1,2-dichloroethane is simultaneously realized Vaporization and separation, the gaseous 1,2-dichloroethane is then condensed to obtain the product. Since the mother liquor of 1,2-dichloroethane circulates in the reaction system, various side reaction products accumulate to a certain extent in the mother liquor, which will lead to "deterioration" of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/14
Inventor 刘建路刘霞薛林梁金龙袁敬明迟庆峰
Owner CHINA NAT OFFSHORE OIL CORP
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