CN204198414U - The device of Separation and Recovery hydrofluoric acid in a kind of difluorochloromethane production - Google Patents

The device of Separation and Recovery hydrofluoric acid in a kind of difluorochloromethane production Download PDF

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Publication number
CN204198414U
CN204198414U CN201420504588.XU CN201420504588U CN204198414U CN 204198414 U CN204198414 U CN 204198414U CN 201420504588 U CN201420504588 U CN 201420504588U CN 204198414 U CN204198414 U CN 204198414U
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China
Prior art keywords
hydrofluoric acid
distillation column
extractive distillation
acid extractive
difluorochloromethane
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CN201420504588.XU
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Chinese (zh)
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王卫国
孙忠英
柳存林
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JIANGSU MEILAN CHEMICAL CO Ltd
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JIANGSU MEILAN CHEMICAL CO Ltd
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Abstract

The utility model discloses the device of Separation and Recovery hydrofluoric acid in the production of a kind of difluorochloromethane, the top of hydrofluoric acid extractive distillation column (2) is provided with condenser (6), the delivery port at hydrofluoric acid extractive distillation column (2) top is connected with the input aperture of condenser (6), the delivery port of condenser (6) is connected with falling-film absorber (3), HCL knockout tower (1) is connected with the input aperture at hydrofluoric acid extractive distillation column (2) middle part, the delivery port of hydrofluoric acid extractive distillation column (2) top-side is connected with water wash column (5), the discharge port of chloroform feeding pump (4) is connected with the input aperture on the top of hydrofluoric acid extractive distillation column (2), the discharge port of the tower reactor (11) that hydrofluoric acid extractive distillation column (2) bottom is provided with is connected with fluoridation still (12), the gas delivery port of tower reactor reboiler (14) is connected with tower reactor (11) inside of hydrofluoric acid extractive distillation column (2).

Description

The device of Separation and Recovery hydrofluoric acid in a kind of difluorochloromethane production
Technical field
The utility model relates to the device of Separation and Recovery hydrofluoric acid in the production of a kind of difluorochloromethane.
Background technology
It is for raw material with chloroform and hydrofluoric acid that difluorochloromethane is produced, both react by certain proportioning and generate difluorochloromethane in fluoridation still, for ensureing discharging component, reactor top is provided with reactive distillation column, because of difluorochloromethane and hydrofluoric acid azeotropic, containing 3-3.5% hydrofluoric acid (the nearly 28-32kg hydrofluoric acid of difluorochloromethane per ton) in reaction gas, the dichloromonofluoromethane of 600-1000PPm, after dry method is separated HCL, in liquid phase material, hydrofluoric acid is only absorbed by the water in water wash column, (12% has water hydrofluoric acid to generate 123 acid, 3% has water HCL), dichloromonofluoromethane at the tired knot of rectifying tower to a certain extent, discharge system, original flow process is surprising to waste of raw materials, and environmental pollution is serious.
Summary of the invention
The utility model provides the device of Separation and Recovery hydrofluoric acid in the production of a kind of difluorochloromethane, and not only structure is simple for it, and simple operation, energy consumption is low, and separation efficiency is high.
The utility model have employed following technical scheme: the device of Separation and Recovery hydrofluoric acid in a kind of difluorochloromethane production, it comprises HCL knockout tower, hydrofluoric acid extractive distillation column, falling-film absorber, chloroform feeding pump, water wash column and fluoridation still, the top of described hydrofluoric acid extractive distillation column is provided with condenser, the delivery port of hydrofluoric acid extracting rectifying top of tower is connected with the input aperture of condenser, the delivery port of condenser is connected with falling-film absorber, flowrate control valve is provided with between described condenser and falling-film absorber, described HCL knockout tower is connected with the input aperture in the middle part of hydrofluoric acid extractive distillation column, Liquid level adjusting valve is provided with between HCL knockout tower and the middle part of hydrofluoric acid extractive distillation column, the delivery port of described hydrofluoric acid extractive distillation column top-side is connected with water wash column, rewinding variable valve is provided with between described hydrofluoric acid extractive distillation column and water wash column, the discharge port of described chloroform feeding pump is connected with the input aperture on the top of hydrofluoric acid extractive distillation column, flow control valve is provided with between chloroform feeding pump and hydrofluoric acid extractive distillation column, the discharge port of the tower reactor that described hydrofluoric acid extracting rectifying tower bottom is provided with is connected with fluoridation still, volume pump II is provided with between the discharge port and fluoridation still of the tower reactor of hydrofluoric acid extractive distillation column, the tower reactor of described hydrofluoric acid extractive distillation column is connected with tower reactor reboiler, the gas delivery port of tower reactor reboiler is connected with the tower reactor inside of hydrofluoric acid extractive distillation column.
Described flowrate control valve connects volume pump I, volume pump I is frequency conversion volume pump.Described rewinding variable valve is connected with rewinding flow meter I.Described flow control valve is connected with flow meter II.The side of described hydrofluoric acid extractive distillation column is provided with pressure-detecting device, and the detecting end of pressure-detecting device is positioned at hydrofluoric acid extractive distillation column, and the output terminal of pressure-detecting device is connected with return valve and return flow meter successively.The side of described hydrofluoric acid extractive distillation column is provided with temperature-detecting device, and the detecting end of temperature-detecting device is positioned at hydrofluoric acid extractive distillation column, and the output terminal of temperature-detecting device is connected with rewinding variable valve and rewinding under meter successively.The gas delivery port place of described tower reactor reboiler is provided with steam regulating valve.The tower top of described hydrofluoric acid extractive distillation column is provided with emptying variable valve.
The utility model has following beneficial effect: after have employed above technical scheme, the reboiler of the utility model hydrofluoric acid extractive distillation column leads to steam heating, difluorochloromethane is vaporized, tower top difluorochloromethane liquid adjusts valve by rewinding, accurate control rewinding amount, steam consumption and pressure in effective adjustment recovery tower reboiler, make bottom temperature and the pressure-stabilisation of hydrofluoric acid extractive distillation column, separation accuracy is high, the difluorochloromethane that tower top is sent is through returning the full liquid backflow of condenser condenses post liquefaction, after backflow makes to form certain pressure in tower repeatedly, rewinding under meter is coordinated to carry out rewinding by rewinding variable valve, the isolated difluorochloromethane precision of HF recovery tower can be improved further.The utility model structure is simple, use cost is low, hydrofluoric acid can not only be reclaimed, simultaneously dichloromonofluoromethane can also be reclaimed and separating feed, heating, condensing reflux, rewinding accurately control by variable valve, simple operation, be separated precision high, whole process does not contact with water, guarantees again to put into production use without impact.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model.
Embodiment
In FIG, the utility model provides the device of Separation and Recovery hydrofluoric acid in the production of a kind of difluorochloromethane, it comprises HCL knockout tower 1, hydrofluoric acid extractive distillation column 2, falling-film absorber 3, chloroform feeding pump 4, water wash column 5 and fluoridation still 12, the top of described hydrofluoric acid extractive distillation column 2 is provided with condenser 6, the delivery port at hydrofluoric acid extractive distillation column 2 top is connected with the input aperture of condenser 6, the delivery port of condenser 6 is connected with falling-film absorber 3, flowrate control valve 7 is provided with between described condenser 6 and falling-film absorber 3, described flowrate control valve 7 connects volume pump I 15, volume pump I 15 is frequency conversion volume pump, described HCL knockout tower 1 is connected with the input aperture in the middle part of hydrofluoric acid extractive distillation column 2, Liquid level adjusting valve 8 is provided with between HCL knockout tower 1 and the middle part of hydrofluoric acid extractive distillation column 2, the delivery port of described hydrofluoric acid extractive distillation column 2 top-side is connected with water wash column 5, rewinding variable valve 9 is provided with between described hydrofluoric acid extractive distillation column 2 and water wash column 5, described rewinding variable valve 9 is connected with rewinding flow meter I 16, the discharge port of described chloroform feeding pump 4 is connected with the input aperture on the top of hydrofluoric acid extractive distillation column 2, flow control valve 10 is provided with between chloroform feeding pump 4 and hydrofluoric acid extractive distillation column 2, described flow control valve 10 is connected with flow meter II 17, the discharge port of the tower reactor 11 be provided with bottom described hydrofluoric acid extractive distillation column 2 is connected with fluoridation still 12, volume pump II 13 is provided with between the discharge port and fluoridation still 12 of the tower reactor 11 of hydrofluoric acid extractive distillation column 2, the tower reactor 11 of described hydrofluoric acid extractive distillation column is connected with tower reactor reboiler 14, the gas delivery port of tower reactor reboiler 14 is connected with tower reactor 11 inside of hydrofluoric acid extractive distillation column 2, the gas delivery port place of tower reactor reboiler 14 is provided with steam regulating valve 18, the side of described hydrofluoric acid extractive distillation column 2 is provided with pressure-detecting device, the detecting end of pressure-detecting device is positioned at hydrofluoric acid extractive distillation column 2, the output terminal of pressure-detecting device is connected with return valve and return flow meter successively, the side of described hydrofluoric acid extractive distillation column 2 is provided with temperature-detecting device, the detecting end of temperature-detecting device is positioned at hydrofluoric acid extractive distillation column 2, the output terminal of temperature-detecting device is connected with rewinding variable valve and rewinding under meter successively, the tower top of hydrofluoric acid extractive distillation column 2 is provided with emptying variable valve.

Claims (8)

1. a difluorochloromethane produce in the device of Separation and Recovery hydrofluoric acid, it is characterized in that it comprises HCL knockout tower (1), hydrofluoric acid extractive distillation column (2), falling-film absorber (3), chloroform feeding pump (4), water wash column (5) and fluoridation still (12), the top of described hydrofluoric acid extractive distillation column (2) is provided with condenser (6), the delivery port at hydrofluoric acid extractive distillation column (2) top is connected with the input aperture of condenser (6), the delivery port of condenser (6) is connected with falling-film absorber (3), flowrate control valve (7) is provided with between described condenser (6) and falling-film absorber (3), described HCL knockout tower (1) is connected with the input aperture at hydrofluoric acid extractive distillation column (2) middle part, Liquid level adjusting valve (8) is provided with between HCL knockout tower (1) and the middle part of hydrofluoric acid extractive distillation column (2), the delivery port of described hydrofluoric acid extractive distillation column (2) top-side is connected with water wash column (5), rewinding variable valve (9) is provided with between described hydrofluoric acid extractive distillation column (2) and water wash column (5), the discharge port of described chloroform feeding pump (4) is connected with the input aperture on the top of hydrofluoric acid extractive distillation column (2), flow control valve (10) is provided with between chloroform feeding pump (4) and hydrofluoric acid extractive distillation column (2), the discharge port of the tower reactor (11) that described hydrofluoric acid extractive distillation column (2) bottom is provided with is connected with fluoridation still (12), volume pump II (13) is provided with between the discharge port of the tower reactor (11) in hydrofluoric acid extractive distillation column (2) and fluoridation still (12), the tower reactor (11) of described hydrofluoric acid extractive distillation column is connected with tower reactor reboiler (14), the gas delivery port of tower reactor reboiler (14) is connected with tower reactor (11) inside of hydrofluoric acid extractive distillation column (2).
2. difluorochloromethane according to claim 1 produce in the device of Separation and Recovery hydrofluoric acid, it is characterized in that described flowrate control valve (7) is upper and connect volume pump I (15), volume pump I (15) is frequency conversion volume pump.
3. difluorochloromethane according to claim 1 produce in the device of Separation and Recovery hydrofluoric acid, it is characterized in that described rewinding variable valve (9) is connected with rewinding flow meter I (16).
4. difluorochloromethane according to claim 1 produce in the device of Separation and Recovery hydrofluoric acid, it is characterized in that described being provided with on flow control valve (10) is connected with flow meter II (17).
5. difluorochloromethane according to claim 1 produce in the device of Separation and Recovery hydrofluoric acid, it is characterized in that the side of described hydrofluoric acid extractive distillation column (2) is provided with pressure-detecting device, the detecting end of pressure-detecting device is positioned at hydrofluoric acid extractive distillation column (2), and the output terminal of pressure-detecting device is connected with return valve and return flow meter successively.
6. difluorochloromethane according to claim 1 produce in the device of Separation and Recovery hydrofluoric acid, it is characterized in that the side of described hydrofluoric acid extractive distillation column (2) is provided with temperature-detecting device, the detecting end of temperature-detecting device is positioned at hydrofluoric acid extractive distillation column (2), and the output terminal of temperature-detecting device is connected with rewinding variable valve and rewinding under meter successively.
7. difluorochloromethane according to claim 1 produce in the device of Separation and Recovery hydrofluoric acid, it is characterized in that the gas delivery port place of described tower reactor reboiler (14) is provided with steam regulating valve (18).
8. difluorochloromethane according to claim 1 produce in the device of Separation and Recovery hydrofluoric acid, it is characterized in that the tower top of described hydrofluoric acid extractive distillation column (2) is provided with emptying variable valve.
CN201420504588.XU 2014-09-03 2014-09-03 The device of Separation and Recovery hydrofluoric acid in a kind of difluorochloromethane production Active CN204198414U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107382662A (en) * 2016-05-14 2017-11-24 江西理文化工有限公司 A kind of method of difluoromethane dry production
CN107382656A (en) * 2016-05-14 2017-11-24 江西理文化工有限公司 A kind of method of monochlorodifluoromethane dry production

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107382662A (en) * 2016-05-14 2017-11-24 江西理文化工有限公司 A kind of method of difluoromethane dry production
CN107382656A (en) * 2016-05-14 2017-11-24 江西理文化工有限公司 A kind of method of monochlorodifluoromethane dry production

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