CN101734623B - Method for preparing fluorine gas in organic fluorine residual liquid - Google Patents

Method for preparing fluorine gas in organic fluorine residual liquid Download PDF

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Publication number
CN101734623B
CN101734623B CN 200910258152 CN200910258152A CN101734623B CN 101734623 B CN101734623 B CN 101734623B CN 200910258152 CN200910258152 CN 200910258152 CN 200910258152 A CN200910258152 A CN 200910258152A CN 101734623 B CN101734623 B CN 101734623B
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China
Prior art keywords
fluorine gas
fluorine
residual liquid
organic
electric arc
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Expired - Fee Related
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CN 200910258152
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CN101734623A (en
Inventor
谢学端
王家贵
曾本忠
张金刚
张劲松
徐美燚
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Zhonghao Chenguang Research Institute of Chemical Industry Co Ltd
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Zhonghao Chenguang Research Institute of Chemical Industry Co Ltd
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Abstract

The invention provides a method for preparing fluorine gas in organic fluorine residual liquid, which comprises the following steps: under the condition of no oxygen, directly cracking the organic fluorine residual liquid under the action of high temperature electric arc, thereby breaking the chemical bonds, such as C, F, H Cl and the like, in the organic substances into C, F2, and small amounts of H2, Cl2, HF, HCL and other substances; and cooling the substances, filtering, rectifying and treating with other methods, thereby obtaining F2 with high purity, which is used as the raw material of SF6, NF3 and the like for cycle use.

Description

Produce the method for fluorine gas in a kind of organic fluorine residual liquid
Technical field
The present invention relates to produce in a kind of organic fluorine residual liquid the method for fluorine gas, specifically, relate to a kind of under oxygen free condition, with organic fluorine residual liquid under the effect of high-temperature electric arc directly cracking produce the method for fluorine gas.
Background technology
Prepare in the process of tetrafluoroethylene at the difluorochloromethane Pintsch process, can generate the octafluoroisobutene of a spot of R 1216, Perfluorocyclobutane and trace.In preparing the process of R 1216, the tetrafluoroethylene cracking also can generate a spot of Perfluorocyclobutane and octafluoroisobutene.Because octafluoroisobutene is a kind of highly toxic substance, also be one of important substance of United Nations's taboo chemical weapons (OPCW) verification, so these two kinds of raffinates can only be handled by high temperature incineration.Nearly all organic fluorine residual liquid all is to carry out Pintsch process, burning in the presence of aerobic at present, handles by washing, alkali cleaning then, and final C element combines with airborne O and generates CO 2Emptying, and the F element combines with H in the water and generates about 30% hydrofluoric acid, just last fluorine element are that the aqueous solution form with hydrofluoric acid exists, and therefore can only sell as low-grade byproduct.
Summary of the invention
The objective of the invention is organic fluorine residual liquid under oxygen free condition, with fluorine gas as plasma striking medium, at high temperature carry out cracking, C-F key in the organic fluorine residual liquid, C-C key are disconnected, generate nano level carbon black and fluorine gas, sell as byproduct by behind the cold filtration fluorine gas and carbon black being separated directly then.
The objective of the invention is to adopt following technical scheme to realize.According to the method for producing fluorine gas in a kind of organic fluorine residual liquid provided by the invention, it comprises step: 1) under oxygen free condition, organic fluorine residual liquid is directly carried out cracking under the effect of high-temperature electric arc; 2) lysate obtains fluorine gas at last through overcooling, filtration, dedusting and rectification process.
The object of the invention to solve the technical problems can also be further achieved by the following technical measures.
Aforesaid high-temperature electric arc is as plasma striking medium with fluorine gas.
Arc (bundle) heart temperature of high-temperature electric arc is more than 7000 ℃ during aforesaid cracking.
Plasma body is that the plasma square or the beam-plasma that utilize between electrode to be produced produce pyritous, produces plasma square or beam-plasma and can use methods such as interchange, direct current, power frequency and high frequency.
Aforesaid lysate comprises C, F 2And H 2, Cl 2, HF and/or HCl.
Aforesaid lysate enters quencher and cools off under the drive of hot gas flow and fluorine gas.
Water coolant in the aforesaid process of cooling becomes low-pressure steam and recycles.
Aforesaid lysate enters water cooler and is chilled to 140~160 ℃.
Aforesaid lysate makes it successively by primary dust removing device, secondary ash collector, isolates carbon black and fluorine gas.
By technique scheme, the present invention has following advantage and beneficial effect at least:
(1) by the waste heat boiler recovery waste heat, makes low-pressure steam and recycle.
(2) subsequent disposal does not adopt washing to separate, and is to handle by filtration, dedusting, rectifying fully, and that obtain at last is the very high F of added value 2With the byproduct carbon black.
(3) by product HF, HCl have made water acid and have sold as byproduct.
(4) principal product F 2Can be used as SF 6, NF 3Deng the synthesis material of material, the raw material of fluoridizing that also can be used as fluorine-containing fine chemicals uses.
Description of drawings
Fig. 1 is the schematic flow sheet of preferred embodiment of the present invention.
Embodiment
Following examples are used to illustrate the present invention, but are not used for limiting the scope of the invention.
Embodiment
1, principle of work:
Plasma body is that the plasma square or the beam-plasma that utilize between electrode to be produced produce pyritous, produce plasma square or beam-plasma and can use methods such as interchange, direct current, power frequency and high frequency, arc (bundle) heart temperature can reach more than 7000 ℃, but and moment realization high temperature.
Hazardous wastes can be broken down into one ion and atomic structure rapidly in the plasma heating furnace of energy-intensive.As organism being decomposed into element and CO equimolecular structures such as carbon, hydrogen, chlorine.
The raffinate of the raffinate of preparation tetrafluoroethylene and preparation R 1216 all is the organic mixture based on C, F element.These organic chemical bonds all disconnect under the effect of plasma high-temperature electric arc, the final mixture that generates based on carbon black and fluorine gas.Mixture is isolated nano level carbon black and fluorine gas after cooling, filtration.
2, operating process:
Open the cooling deionized water of plasma gun earlier, the flow control of cooling deionized water is imported and exported the temperature difference and is controlled at 10 ℃ at 3~4 tons/h.Feed refining fluorine gas then in plasma gun, fluorine gas flow is controlled at 20m 3About/h (acting as of fluorine gas is blown into high-temperature electric arc in the incinerator, protected electrode simultaneously again).Power-on then, electric current forms 7000 ℃ of high-temperature electric arcs in the striking of plasma gun place, and the high temperature that electric arc produces is heated to fluorine gas about 6000 ℃, and the high temperature fluorine gas enters into incinerator then, and whole burner hearth is heated to about 4000 ℃.And then with raffinate intensification, vaporization, be pressed in the incinerator, flow control is at 50kg/h, and pressure-controlling is about 0.15MPa.Under the high temperature oxygen free condition, there is machine residue cracking in pyrolyzer to generate carbon black and fluorine gas.Because the particle diameter of carbon black is very tiny, mixed gas enters quencher and cools off under the drive of hot gas flow and fluorine gas, water coolant becomes low-pressure steam and recycles, mixed gas enters water cooler again and is chilled to about 150 ℃, enter one-level sack cleaner, secondary sack cleaner then successively, carbon black is separated from mixed gas the most at last.Carbon black, the fluorine gas separated are sold as byproduct.
Though above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.

Claims (5)

1. produce the method for fluorine gas in the organic fluorine residual liquid, it is characterized in that it comprises step:
1) under oxygen free condition, organic fluorine residual liquid is directly carried out cracking under the effect of high-temperature electric arc;
2) lysate obtains fluorine gas at last through overcooling, filtration, dedusting and rectification process;
Wherein, described high-temperature electric arc be with fluorine gas as plasma striking medium, the arc core temperature of high-temperature electric arc is more than 7000 ℃ during cracking.
2. method according to claim 1 is characterized in that wherein said lysate comprises C, F 2, H 2, C1 2, HF and HCl.
3. method according to claim 1 and 2 is characterized in that lysate enters quencher and cools off under the drive of hot gas flow and fluorine gas.
4. method according to claim 1 and 2 is characterized in that water coolant in the process of cooling becomes low-pressure steam and recycles.
5. method according to claim 1 and 2 is characterized in that lysate enters water cooler and is chilled to 140~160 ℃.
CN 200910258152 2009-12-21 2009-12-21 Method for preparing fluorine gas in organic fluorine residual liquid Expired - Fee Related CN101734623B (en)

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Application Number Priority Date Filing Date Title
CN 200910258152 CN101734623B (en) 2009-12-21 2009-12-21 Method for preparing fluorine gas in organic fluorine residual liquid

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Application Number Priority Date Filing Date Title
CN 200910258152 CN101734623B (en) 2009-12-21 2009-12-21 Method for preparing fluorine gas in organic fluorine residual liquid

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CN101734623A CN101734623A (en) 2010-06-16
CN101734623B true CN101734623B (en) 2011-08-17

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CN107226773A (en) * 2017-06-16 2017-10-03 临海市利民化工有限公司 A kind of synthetic method of o-difluoro-benzene

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Owner name: ZHONGHAO CHENGUANG RESEARCH INSTITUTE OF CHEMICAL

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Address after: 643201 Zigong County, Sichuan Province, Chenguang Road, No. 135, Fushun

Patentee after: Zhonghao Chenguang Chemical Institute Co., Ltd.

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CF01 Termination of patent right due to non-payment of annual fee