CN107382660A - Gas phase methods of eliminating acidity in a kind of monochlorodifluoromethane production - Google Patents
Gas phase methods of eliminating acidity in a kind of monochlorodifluoromethane production Download PDFInfo
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- CN107382660A CN107382660A CN201610315253.7A CN201610315253A CN107382660A CN 107382660 A CN107382660 A CN 107382660A CN 201610315253 A CN201610315253 A CN 201610315253A CN 107382660 A CN107382660 A CN 107382660A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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Abstract
Gas phase methods of eliminating acidity in being produced the invention discloses a kind of monochlorodifluoromethane, it is related to technical field of fluorine chemical industry;Its methods of eliminating acidity is as follows:Enter vaporizer storage tank by liquid level regulation from HCl separation tower tower reactor crude product, vaporizer is pumped into by vaporizer conveying, vaporizer automatically controls that maintenance pressure is constant, and the crude product after vaporization enters water scrubber bottom by liquid level and pressure;Industry water delivers to water scrubber top from storage tank by industrial water pump, it is in contact by gas-liquid, the hydrogen fluoride absorbed in crude product forms rare water hydrofluoric acid, and rare water hydrofluoric acid is drained into the hydrogen fluoride absorption system of anhydrous hydrogen fluoride device by Liquid level, externally sold after absorbing into finished acid;Flow of the present invention is short, simple to operate, and alkali lye consumption amount is small, and operating cost is low;Because water scrubber operation temperature is high, the R22 dissolved in diluted acid is reduced, and mixed alkali liquor is free of caustic soda, and amount of hydrolysis of the R22 in mixed alkali liquor is reduced.
Description
Technical field:
Gas phase methods of eliminating acidity in being produced the present invention relates to a kind of monochlorodifluoromethane, belongs to technical field of fluorine chemical industry.
Background technology:
Monochlorodifluoromethane (abbreviation R22) is chloroform and hydrogen fluoride under catalyst action, under the conditions of 60~80 DEG C, 1.0~2.0MPa, fluorine atom substitution chlorine atom generation R22 in the reactor, while a small amount of monofluorodichloromethane of by-product and fluoroform.The mixed gas of reactor outlet is after reflux column, topping still remove heavy constituent, into HCl separation tower.Tower top light component(Mainly HCL)Absorbed through falling-film absorber into fluorine-containing hydrochloric acid, on-condensible gas(Mainly R23)Deliver to incinerator burning.Tower reactor crude product is by after water, caustic wash tower remove acidity, being sent into rectifying column.The qualified R22 of tower top purity delivers to finished product detection groove after further removing micro-moisture.
Liquid phase deacidification operation idiographic flow be:Crude product from HCl separation tower tower reactor enters water scrubber top after trap, cooler.Industry water is sent into water scrubber bottom by water scrubber feed pump from tank after precooling, and water scrubber reclaimed water absorbs the hydrogen fluoride of crude product formed with water hydrofluoric acid, has water hydrofluoric acid to drain into storage tank from tower top.Tower reactor crude product is pumped to alkali separating tank, agglomerator, decanter by mixing, and the crude product for removing acidity completely through fully neutralizing enters rectifying column by decanter bottom liquid phases.Different alkali lye in alkali dosage bunker and alkali feeder trough are sent into alkali neutralization chamber by certain proportion, are then pumped into mixing pump inlet by neutralizing.
Above-mentioned liquid phase acid removal process long flow path, complex operation, alkali consumption is high, and operating cost is high;And the meltage for having R22 in water hydrofluoric acid of water scrubber discharge is big, R22 amount of hydrolysis is big in alkali separating tank, causes raw material consumption higher.
The content of the invention:
A kind of in view of the above-mentioned problems, gas phase methods of eliminating acidity in being produced the technical problem to be solved in the present invention is to provide monochlorodifluoromethane.
Gas phase methods of eliminating acidity in a kind of monochlorodifluoromethane production of the present invention, its methods of eliminating acidity are as follows:It includes R22 carburetion systems, production water and alkali lye feed system, water scrubber and dilute acid recovery system, alkali cleaning Tower System;Described R22 carburetion systems are R22 vaporizers;Described water wash system is in contact the water scrubber of deacidification using gas-liquid;Described caustic washing system is in contact caustic wash tower and the efficient caustic wash tower demister of deacidification using gas-liquid;Enter vaporizer storage tank by liquid level regulation from HCl separation tower tower reactor crude product, vaporizer is pumped into by vaporizer conveying, vaporizer automatically controls that maintenance pressure is constant, and the crude product after vaporization enters water scrubber bottom by liquid level and pressure;Industry water delivers to water scrubber top from storage tank by industrial water pump, it is in contact by gas-liquid, the hydrogen fluoride absorbed in crude product forms rare water hydrofluoric acid, and rare water hydrofluoric acid is drained into the hydrogen fluoride absorption system of anhydrous hydrogen fluoride device by Liquid level, externally sold after absorbing into finished acid;The crude product containing micro acidity that water scrubber ejection comes enters alkali cleaning tower reactor, fully contacted by the alkali lye circulated with NaOH solution circulating pump, neutralize micro acidity, periodic detection circulates alkali concn, salkali waste delivers to sewage plant when concentration reaches lower control limit, and fresh alkali lye is added into tower by alkali lye storage tank and delivery pump.Gas of the tower top without acidity enters demister, after removing the most of moisture in gas, subsequently into rectifying column.
Preferably, the caustic wash tower temperature control of described caustic washing system is at 40-45 DEG C.
Preferably, the water scrubber temperature control of described water wash system is at 35-55 DEG C.
Preferably, described caustic washing system is using the mixed alkali liquor for reducing R22 hydrolysis.
Preferably, the diluted acid recoverable of described water wash system.
Beneficial effects of the present invention are:Flow is short, simple to operate, and alkali lye consumption amount is small, and operating cost is low;Because water scrubber operation temperature is high, the R22 dissolved in diluted acid is reduced, and mixed alkali liquor is free of caustic soda, and amount of hydrolysis of the R22 in mixed alkali liquor is reduced.
Brief description of the drawings:
For ease of explanation, the present invention is described in detail by following specific implementations and accompanying drawing.
Fig. 1 is the flow chart of the present invention.
Embodiment:
To make the object, technical solutions and advantages of the present invention of greater clarity, the present invention is described below by the specific embodiment shown in accompanying drawing.However, it should be understood that these descriptions are merely illustrative, and it is not intended to limit the scope of the present invention.In addition, in the following description, the description to known features and technology is eliminated, to avoid unnecessarily obscuring idea of the invention.
As shown in figure 1, present embodiment uses following technical scheme:Its methods of eliminating acidity is as follows:It includes R22 carburetion systems, production water and alkali lye feed system, water scrubber and dilute acid recovery system, alkali cleaning Tower System;Described R22 carburetion systems are R22 vaporizers;Described water wash system is in contact the water scrubber of deacidification using gas-liquid;Described caustic washing system is in contact caustic wash tower and the efficient caustic wash tower demister of deacidification using gas-liquid;Enter vaporizer storage tank by liquid level regulation from HCl separation tower tower reactor crude product, vaporizer is pumped into by vaporizer conveying, vaporizer automatically controls that maintenance pressure is constant, and the crude product after vaporization enters water scrubber bottom by liquid level and pressure;Industry water delivers to water scrubber top from storage tank by industrial water pump, it is in contact by gas-liquid, the hydrogen fluoride absorbed in crude product forms rare water hydrofluoric acid, and rare water hydrofluoric acid is drained into the hydrogen fluoride absorption system of anhydrous hydrogen fluoride device by Liquid level, externally sold after absorbing into finished acid;The crude product containing micro acidity that water scrubber ejection comes enters alkali cleaning tower reactor, fully contacted by the alkali lye circulated with NaOH solution circulating pump, neutralize micro acidity, periodic detection circulates alkali concn, salkali waste delivers to sewage plant when concentration reaches lower control limit, and fresh alkali lye is added into tower by alkali lye storage tank and delivery pump.Gas of the tower top without acidity enters demister, after removing the most of moisture in gas, subsequently into rectifying column.
Further, the caustic wash tower temperature control of described caustic washing system is at 40-45 DEG C.
Further, the water scrubber temperature control of described water wash system is at 35-55 DEG C.
Further, described caustic washing system is using the mixed alkali liquor for reducing R22 hydrolysis.
Further, the diluted acid recoverable of described water wash system.
Further, described described R22 carburetion systems use special compress control method.
The operation principle of present embodiment is:The mixed gas of reactor outlet is after reflux column, topping still remove heavy constituent, into HCl separation tower.Tower top light component(Mainly hydrogen chloride gas)Absorbed through falling-film absorber into fluorine-containing hydrochloric acid, on-condensible gas delivers to incinerator burning.Tower reactor crude product is vaporized by vaporizer, after water, caustic wash tower remove acidity, is sent into rectifying column;The qualified R22 of tower top purity delivers to finished product detection groove after further removing micro-moisture;Technic acid is removed using gas phase, gas phase scale is washed, and shortens flow, reduces cost of investment;The consumption of the energy and raw material is reduced in process of production, has saved resource.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.It should be understood by those skilled in the art that; the present invention is not limited to the above embodiments; merely illustrating the principles of the invention described in above-described embodiment and specification; without departing from the spirit and scope of the present invention; various changes and modifications of the present invention are possible, and these changes and improvements all fall within the protetion scope of the claimed invention.The scope of the present invention is defined by the appended claims and its equivalents.
Claims (5)
- A kind of 1. gas phase methods of eliminating acidity in monochlorodifluoromethane production, it is characterised in that:Its methods of eliminating acidity is as follows:It includes R22 carburetion systems, production water and alkali lye feed system, water scrubber and dilute acid recovery system, alkali cleaning Tower System;Described R22 carburetion systems are R22 vaporizers;Described water wash system is in contact the water scrubber of deacidification using gas-liquid;Described caustic washing system is in contact caustic wash tower and the efficient caustic wash tower demister of deacidification using gas-liquid;Enter vaporizer storage tank by liquid level regulation from HCl separation tower tower reactor crude product, vaporizer is pumped into by vaporizer conveying, vaporizer automatically controls that maintenance pressure is constant, and the crude product after vaporization enters water scrubber bottom by liquid level and pressure;Industry water delivers to water scrubber top from storage tank by industrial water pump, it is in contact by gas-liquid, the hydrogen fluoride absorbed in crude product forms rare water hydrofluoric acid, and rare water hydrofluoric acid is drained into the hydrogen fluoride absorption system of anhydrous hydrogen fluoride device by Liquid level, externally sold after absorbing into finished acid;The crude product containing micro acidity that water scrubber ejection comes enters alkali cleaning tower reactor, fully contacted by the alkali lye circulated with NaOH solution circulating pump, neutralize micro acidity, periodic detection circulates alkali concn, salkali waste delivers to sewage plant when concentration reaches lower control limit, and fresh alkali lye is added into tower by alkali lye storage tank and delivery pump;Gas of the tower top without acidity enters demister, after removing the most of moisture in gas, subsequently into rectifying column.
- 2. gas phase methods of eliminating acidity in a kind of monochlorodifluoromethane production according to claim 1, it is characterised in that:The caustic wash tower temperature control of described caustic washing system is at 40-45 DEG C.
- 3. gas phase methods of eliminating acidity in a kind of monochlorodifluoromethane production according to claim 1, it is characterised in that:The water scrubber temperature control of described water wash system is at 35-55 DEG C.
- 4. gas phase methods of eliminating acidity in a kind of monochlorodifluoromethane production according to claim 1, it is characterised in that:Described caustic washing system is using the mixed alkali liquor for reducing R22 hydrolysis.
- 5. gas phase methods of eliminating acidity in a kind of monochlorodifluoromethane production according to claim 1, it is characterised in that:The diluted acid recoverable of described water wash system.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111943244A (en) * | 2020-08-12 | 2020-11-17 | 山东昭和新材料科技股份有限公司 | Method for producing low-silicon dry-process aluminum fluoride by using high-silicon fluorite powder |
US11628183B2 (en) | 2018-07-27 | 2023-04-18 | ARC Medical Ine. | Highly purified fucans for the treatment of fibrous adhesions |
Citations (6)
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GB1281822A (en) * | 1969-01-16 | 1972-07-19 | Imp Smelting Corp Ltd | Improved fluorination process |
CN1073423A (en) * | 1992-12-12 | 1993-06-23 | 浙江省化工研究院 | By vinylidene chloride preparation by liquid-phase fluorization 1,1-two chloro-1-fluoroethanes |
CN201873515U (en) * | 2010-09-14 | 2011-06-22 | 昆山化工医药原料有限公司 | Fluorine hydride gas recovery device |
CN102478245A (en) * | 2010-11-29 | 2012-05-30 | 屠国强 | Method for reducing greenhouse effect and treating F23 in difluoro-methane chloride production through environmentally-friendly burning |
CN104119201A (en) * | 2014-07-02 | 2014-10-29 | 常熟三爱富中昊化工新材料有限公司 | Dry separation and purification system and purification method for fluorine-containing alkane |
CN205878191U (en) * | 2016-08-09 | 2017-01-11 | 湖北中油优艺环保科技有限公司 | Energy -efficient incineration treatment device of hazardous waste |
-
2016
- 2016-05-14 CN CN201610315253.7A patent/CN107382660A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1281822A (en) * | 1969-01-16 | 1972-07-19 | Imp Smelting Corp Ltd | Improved fluorination process |
CN1073423A (en) * | 1992-12-12 | 1993-06-23 | 浙江省化工研究院 | By vinylidene chloride preparation by liquid-phase fluorization 1,1-two chloro-1-fluoroethanes |
CN201873515U (en) * | 2010-09-14 | 2011-06-22 | 昆山化工医药原料有限公司 | Fluorine hydride gas recovery device |
CN102478245A (en) * | 2010-11-29 | 2012-05-30 | 屠国强 | Method for reducing greenhouse effect and treating F23 in difluoro-methane chloride production through environmentally-friendly burning |
CN104119201A (en) * | 2014-07-02 | 2014-10-29 | 常熟三爱富中昊化工新材料有限公司 | Dry separation and purification system and purification method for fluorine-containing alkane |
CN205878191U (en) * | 2016-08-09 | 2017-01-11 | 湖北中油优艺环保科技有限公司 | Energy -efficient incineration treatment device of hazardous waste |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11628183B2 (en) | 2018-07-27 | 2023-04-18 | ARC Medical Ine. | Highly purified fucans for the treatment of fibrous adhesions |
CN111943244A (en) * | 2020-08-12 | 2020-11-17 | 山东昭和新材料科技股份有限公司 | Method for producing low-silicon dry-process aluminum fluoride by using high-silicon fluorite powder |
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