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A kind of resource treatment method of fluorinated siloxane waste liquid

A fluorinated siloxane and waste liquid treatment technology, applied in chemical instruments and methods, water/sewage treatment, water/sewage multi-stage treatment, etc., can solve the problem of high equipment requirements, waste of resources, and strong corrosiveness of hydrogen fluoride to equipment and other problems to achieve the effect of reducing energy consumption, saving costs, avoiding environmental pollution and waste of resources

Active Publication Date: 2020-03-06
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The incineration treatment system will produce hydrogen fluoride during the treatment process, which is highly corrosive to the equipment and requires high equipment. At the same time, direct incineration of fluorinated organic silicon waste liquid will cause waste of resources.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Waste liquid hydrolysis:

[0037] Add fluorinated siloxane waste liquid and potassium hydroxide solution with a mass concentration of 8% into the reaction kettle at a mass ratio of 1:3, heat to 30°C, stir and react for 30 minutes, and then enter the layering device for separation to obtain the hydrolyzate and spent lye;

[0038] (2) Catalytic rearrangement:

[0039] Place the hydrolyzate obtained in step (1) in a catalytic rearrangement reactor, heat to 130° C., stir and add the catalyst, the amount of the catalyst added is 0.1% of the weight of the hydrolyzate, and react for 0.5 h at a pressure of 0.06 MPa and a temperature of Distilled under reduced pressure at 140-200°C to obtain dimethylsiloxane mixed rings;

[0040] (3) Regeneration of waste lye:

[0041] Add sodium hydroxide or calcium hydroxide to the spent lye obtained in step (1), stir and react for 10 minutes, filter to obtain fluoride salt and regenerated lye;

[0042] (4) lye recycling:

[0043] The...

Embodiment 2

[0047] (1) Waste liquid hydrolysis:

[0048] Put the fluorinated siloxane waste liquid and the regenerated lye obtained in Example 1 into the reaction kettle at a mass ratio of 1:5, heat to 50°C, stir and react for 55 minutes, and then enter the layering device for separation to obtain the hydrolyzate and spent alkali liquid;

[0049] (2) Catalytic rearrangement:

[0050] Place the hydrolyzate obtained in step (1) in a catalytic rearrangement reactor, heat to 135°C, stir and add the catalyst, the amount of catalyst added is 1.5% of the weight of the hydrolyzate, react for 1.2h, at a pressure of 0.08MPa and a temperature of 140 Distilled under reduced pressure at -200°C to obtain dimethylsiloxane mixed rings;

[0051] (3) Regeneration of waste lye:

[0052] Add sodium hydroxide or calcium hydroxide to the spent lye obtained in step (1), stir and react for 35 minutes, filter to obtain fluoride salt and regenerated lye;

[0053] (4) lye recycling:

[0054] The regenerated ly...

Embodiment 3

[0057] (1) Waste liquid hydrolysis:

[0058]Add fluorinated siloxane waste liquid and potassium hydroxide solution with a mass concentration of 16.5% into the reaction kettle at a mass ratio of 1:4.5, heat to 60°C, stir and react for 45 minutes, and then enter the layering device for separation to obtain the hydrolyzate and spent lye;

[0059] (2) Catalytic rearrangement:

[0060] Place the hydrolyzate obtained in step (1) in a catalytic rearrangement reactor, heat to 130-140°C, stir and add the catalyst, the amount of catalyst added is 1.5% of the weight of the hydrolyzate, react for 1.2h, and the pressure is 0.08MPa, Distillation under reduced pressure at a temperature of 140-200°C to obtain a mixed ring of dimethylsiloxane;

[0061] (3) Regeneration of waste lye:

[0062] Add sodium hydroxide or calcium hydroxide to the spent lye obtained in step (1), stir and react for 25 minutes, filter to obtain fluoride salt and regenerated lye;

[0063] (4) lye recycling:

[0064]...

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PUM

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Abstract

The invention discloses a fluorinated siloxane waste liquor recycling method which comprises the following steps: (1) waste liquor hydrolysis, namely reacting fluorinated siloxane waste liquor and alkali liquor, and separating to obtain a hydrolysis product and waste alkali liquor; (2) catalytic rearrangement, namely carrying out a catalytic reaction on the hydrolysis product, and performing reduced pressure distillation to obtain mixed methylcyclosiloxane of dimethyl siloxane; (3) regeneration of the waste alkali liquor, namely adding solid alkali into the waste alkali liquor, and filtering to obtain a fluoride salt and regenerated alkali liquor; and (4) recycling alkali liquor, namely taking the regenerated alkali liquor as alkali liquor for hydrolysis, and recycling. The fluorinated siloxane waste liquor recycling method disclosed by the invention is simple in process, and the waste liquor is transformed into a basic raw material (mixed methylcyclosiloxane of dimethyl siloxane) in the organosilicon industry, so that waste liquor recycling and cyclic utilization of the waste liquor can be realized.

Description

technical field [0001] The invention relates to the field of waste liquid treatment, in particular to a resource treatment method for fluorinated siloxane waste liquid. Background technique [0002] Fluorinated siloxane waste liquid is the fluorine-terminated polydimethylsiloxane waste liquid produced by the defluorination of octamethylcyclotetrasiloxane (D4) in industrial production (the structural formula is as follows: FSi(CH3)2[OSi (CH3)2]nF (n=0,1,2,3 etc.)). At present, there is no report on the treatment of this waste liquid, so it is necessary to study the treatment method of fluorinated siloxane waste liquid. [0003] Chinese patent CN102532547B discloses a method for preparing silicone oil from organosilicon high boilers, which includes the following steps: 1) adding dropwise a mixture of ethanol and catalyst to the organosilicon high boilers, and refluxing at 50-70°C to obtain the first reaction Materials; 2) placing the first reaction material in a neutralizati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C02F9/10C02F101/36
CPCC02F1/00C02F1/04C02F1/66C02F9/00C02F2101/36
Inventor 黄明星杨仲苗吴奕张品杰
Owner JUHUA GROUP TECH CENT