CN108862197A - With the method and device thereof of by-product hydrogen chloride gas production liquid hydrogen chloride - Google Patents
With the method and device thereof of by-product hydrogen chloride gas production liquid hydrogen chloride Download PDFInfo
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- CN108862197A CN108862197A CN201710345188.7A CN201710345188A CN108862197A CN 108862197 A CN108862197 A CN 108862197A CN 201710345188 A CN201710345188 A CN 201710345188A CN 108862197 A CN108862197 A CN 108862197A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/80—Compositional purity
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Abstract
The present invention relates to liquid hydrogen chlorides, and in particular to a kind of method and device thereof with by-product hydrogen chloride gas production liquid hydrogen chloride.The method be using by-product hydrogen chloride gas as raw material, it is re-liquefied, filling first after condensation and removal high-boiling components.Compared with prior art, the present invention has not only prevented the use of water, has recycled the high-boiling components in by-product hydrogen chloride gas, and reduces the generation of terminal user's waste water, also reduces the discharge of terminal user COD, reduces environmental pollution.Meanwhile a completely new processing mode is provided for the use of industrial by-product hydrogen chloride gas, conceive with the prior art entirely different.Installation cost of the present invention is low, income is high.
Description
Technical field
The present invention relates to liquid hydrogen chlorides, and in particular to a method of liquid hydrogen chloride is produced with by-product hydrogen chloride gas
And its device.
Background technique
In modern chemical industry production, such as the hydrogen chloride gas generated in fluorine chemical industry fluorination reaction process, organic synthesis
The hydrogen chloride gas of chlorination reaction process by-product, common water absorption are made 31% or so hydrochloric acid, are chiefly used in derusting and solid
The preparation of water purification agent aluminium polychloride, iron chloride etc., this part hydrochloric acid include many organic matters, and scale is up to ten million ton.This
Process absorbs the hydrochloric acid for being made 31% or so into downstream use process from upstream with water, is also generated simultaneously using a large amount of water a large amount of
Waste water, and the COD content of waste water is high, and environment protection treating difficulty is big.
102390810 A of Chinese patent CN discloses a kind of from by-product of the chlorination reaction of the organic matter generation containing hydrogen chloride
The technology that hydrogen chloride is separated, extracted in object can use the side of water absorption since most of organic chlorides are insoluble or are insoluble in water
Method separates hydrogen chloride and other components.Mixed gas water obtained by chlorination reaction or 20% or so azeotropic absorption by Hydrochloric Acid chlorination
Hydrogen.When absorbing temperature at 50 DEG C or so, 30%~35% hydrochloric acid is made.Gained crude salt acid can be refined first when necessary,
Then desorption obtains gas chlorination hydrogen and barostat control.Hydrogen chloride is sent to user through drying, and barostat control is recycled back to absorber portion.This work
Skill is reasonable, and production is simple, is the most easy desirable technique of hydrogen chloride preparation.The azeotropic hydrochloric acid that the patent passes through water or 20% or so
Absorbing hydrogen chloride still remains using a large amount of water, also generates the defect of a large amount of waste water.
102445051 A of Chinese patent CN discloses a kind of method that preparation liquid hydrogen chloride is compressed from hydrogen chloride gas, institute
Stating water content in hydrogen chloride gas is 900~1100ppm, the preparation method is that：(1) by the hydrogen chloride gas deep cooling under room temperature
To 0~5 DEG C, hydrogen chloride gas after obtaining deep cooling, water content is lower than 300ppm in the hydrogen chloride gas after the deep cooling；(2)
By the dry hydrogen chloride gas to water content lower than 5ppm, after being dried of hydrogen chloride gas after deep cooling；It (3) will be after drying
Hydrogen chloride gas is compressed to 6~7MPa, obtains compressed liquid hydrogen chloride.The corrosion that the present invention solves aqueous hydrogen chloride gas is asked
Topic, is compressed into bottling industry grade liquid hydrogen chloride for dry hydrogen chloride gas, has and transports, is easy to use, and safety collar again
The features such as guarantor.The present invention thoroughly solves the problems, such as using environmental pollution during hydrogen chloride, have preferable economic benefit and
Social benefit.But the patent is in its specification【0003】It is explicitly pointed out in section background technique：Hydrogen chloride gas in industrial production
It can be obtained using following three kinds of methods：First is that chlorine is reacted with hydrogen；Second is that by carrying out deep analysis to hydrochloric acid；Third is that chlorine
Change sodium and strong sulfuric acid response.The technical issues of this also illustrates that the raw material that the patent uses is synthesising hydrogen, solves is to pass through
Remove the etching problem that the moisture in synthesizing chlorinated hydrogen solves aqueous hydrogen chloride gas.
Chinese patent CN 101648104A discloses a kind of recovery process technology of hydrogen chloride tail gas in chemical production, passes through
Exchange circulating technology of the bubble absorbing tower on absorbing hydrogen chloride order, tower temperature sequentially control 10~30 DEG C of technologies below,
The chlorine hydride absorbents such as desiccant and deionized water, dehydrated alcohol, absolute ethyl alcohol are used cooperatively, and realize returning for hydrogen chloride
It receives.The patent solves the recycling of hydrogen chloride tail gas in chemical production by absorbent absorbing hydrogen chloride, but complex steps, at
This height is still and is carried out by the way of absorbing.
In the prior art, it is reused after 31% or so hydrochloric acid being made in industrial by-product hydrogen chloride gas in a manner of absorption,
It is method the most universal, this method generates a large amount of waste water.In view of the presence of problem above, need to develop a kind of by-product chlorine at present
Change hydrogen and 31% or so hydrochloric acid is made without water absorption, thus the method for reducing waste water generation.
Summary of the invention
The object of the present invention is to provide what a kind of reduction waste water generated to produce liquid hydrogen chloride with by-product hydrogen chloride gas
Method and device thereof.
Method of the present invention with by-product hydrogen chloride gas production liquid hydrogen chloride, is to be with by-product hydrogen chloride gas
Raw material, it is re-liquefied, filling first after condensation and removal high-boiling components.
Wherein：
The by-product hydrogen chloride gas is discharged after condenser condensation and removal high-boiling components from condenser overhead；It is described high boiling
Object is discharged from condenser bottom, in recovery technique.
The condenser is one or more levels；In order to improve efficiency, the preferred multi-tube pass heat exchanger of condenser；The condenser
Temperature be -5~-40 DEG C, in condenser refrigerant be 25~28wt.% of mass percent calcium chloride water, methylene chloride
Or fluoroform.
The liquefaction is to liquefy after deep cooling or first after compression, then cryogenic liquefying.
As known from the above, there are two types of processing modes for the industrial by-product hydrogen chloride gas after high-boiling components are removed in the present invention：
(1) filling after cryogenic liquefying；
(2) filling after compression, cryogenic liquefying.
Above-mentioned processing mode is that parallel technical solution selects a use according to the actual situation.It, can basis when use
The difference of deep cooling medium and pressure is divided into following several situations, and deep cooling medium generally uses fluoroform or liquid nitrogen, preferably three
Fluoromethane.
(1) when deep cooling medium uses fluoroform, there are following several situations：
(1) it when by-product hydrogen chloride gas pressure >=0.6MPa, can be filled after deep cooling liquefies by-product hydrogen chloride gas
Dress；It can also first be compressed, then after deep cooling liquefies by-product hydrogen chloride gas, it is filling.
(2) when by-product hydrogen chloride gas pressure is less than 0.6MPa, after compression, deep cooling liquefy by-product hydrogen chloride gas,
It is filling.
(2) when deep cooling medium uses liquid nitrogen：
No matter by-product hydrogen chloride gas pressure be it is how many, can generally be up in a reasonable range certainly
It is filling directly after deep cooling liquefies by-product hydrogen chloride gas without compression when 4.0MPa (G) deep cooling medium uses liquid nitrogen.
- 45~-110 DEG C of the cryogenic temperature, the deep cooling are level-one deep cooling or multistage deep cooling.The boil down to level-one pressure
Contracting or multi-stage compression, one stage of compression use diaphragm type compressor, and multi-stage compression uses piston compressor.Those skilled in the art's root
It is selected according to actual conditions.
Realize the device with by-product hydrogen chloride gas production liquid chlorine hydrogen methods, including by-product hydrogen chloride gas
Discharge nozzle, by-product hydrogen chloride gas discharge nozzle are sequentially connected with condenser, liquefying plant, filling apparatus.
Wherein：
The condenser is one or more levels.
The condenser is multi-tube pass heat exchanger.
The liquefying plant is the combination of cryogenic condenser either compressor and cryogenic condenser.
The cryogenic condenser is one or more levels.
The compressor is one or more levels, and level-one uses diaphragm type compressor, and multistage uses piston compressor.
Surge tank is set between the liquefying plant and filling apparatus.
The material of condenser used in the present invention is stainless steel, preferably Stainless steel 316 L.
Beneficial effects of the present invention are as follows：
Compared with prior art, the present invention has not only prevented the use of water, has recycled high boiling in by-product hydrogen chloride gas
Object, and reduce the generation of terminal user's waste water, the discharge of terminal user COD is also reduced, environmental pollution is reduced.Together
When, a completely new processing mode is provided for the use of industrial by-product hydrogen chloride gas, is conceived with the prior art entirely different.This
Installation cost used by inventing is low, income is high.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of use device of the present invention；
Fig. 2 is the structural schematic diagram of 1 use device of embodiment；
Fig. 3 is the structural schematic diagram of 2 use device of embodiment；
In figure：1, by-product hydrogen chloride gas discharge nozzle；2, condenser；3, liquefying plant；4, filling apparatus；5, hydrogen chloride essence
Tower processed；6, first-stage condenser；7, secondary condenser；8, level-one cryogenic condenser；9, second level cryogenic condenser；10, surge tank；
11, it pumps；12, hydrogen chloride finished pot；13, Primary diaphragm compressor.
Specific embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
In monochlorodifluoromethane industrial production, fluorination reaction by-product hydrogen chloride gas goes out through hydrogen chloride treating column top row, row
Gas pressure out is 1.6MPa (G), and temperature is -30 DEG C, and gas contains hydrogen chloride, hydrogen fluoride, fluoroform, one chloromethane of difluoro
The components such as alkane.Its composition is calculated in mass percent, and hydrogen chloride accounts for 87.81wt.%, hydrogen fluoride accounts for 1.12wt.%, fluoroform accounts for
3.04wt.%, monochlorodifluoromethane account for 7.95wt.%, and surplus is other components.
The method of the present invention is as follows：
(1) above-mentioned hydrogen chloride gas 15Nm3/ h, through first-stage condenser 150m2, secondary condenser 100m2Condensation, removing are high
Object is boiled, is discharged from secondary condenser top.Level-one, secondary condenser temperature are controlled at -35 DEG C, and refrigerant is all made of dichloromethane
Alkane is multi-tube pass heat exchanger.The high-boiling components such as condensed hydrogen fluoride, monochlorodifluoromethane are recycled, are applied in technique.Second level
The composition of the hydrogen chloride gas of condenser overhead discharge, is calculated in mass percent, hydrogen chloride accounts for 96.64wt.%, fluoroform accounts for
3.31wt.%, surplus are other components.
(2) hydrogen chloride gas being discharged at the top of secondary condenser, enters back into level-one cryogenic condenser 100m2, second level it is deep
Cool condenser 60m2Later, hydrogen chloride gas liquefies, is filling.Cryogenic temperature is -45 DEG C, and deep cooling medium is fluoroform.
The structural schematic diagram of 1 use device of embodiment is as shown in Fig. 2, include the hydrogen chloride treating column 5 being sequentially connected, level-one
Condenser 6, secondary condenser 7, level-one cryogenic condenser 8, second level cryogenic condenser 9, surge tank 10, pump 11, hydrogen chloride finished product
Tank 12.
Embodiment 2
In pentafluoroethane industrial production, by-product hydrogen chloride gas goes out, the gas pressure of discharge through hydrogen chloride treating column top row
For 0.9MPa (G), temperature is -20 DEG C, and gas contains the components such as hydrogen chloride, perfluoroethane, pentafluoroethane.It is formed with quality hundred
Score meter, hydrogen chloride accounts for 94.91wt.%, perfluoroethane accounts for 1.02wt.%, pentafluoroethane accounts for 3.97wt.%, and surplus is other
Component.
The method of the present invention is as follows：
(1) above-mentioned hydrogen chloride gas 10Nm3/ h, through first-stage condenser 60m2, secondary condenser 100m2Condensation removes high boiling
Object is discharged from secondary condenser top.Level-one, secondary condenser temperature are controlled at -30 DEG C, and refrigerant is all made of 26wt.%'s
Calcium chloride water is multi-tube pass heat exchanger.The high-boiling components such as condensed perfluoroethane are recycled, are applied in technique.Second level
The composition of the hydrogen chloride gas of condenser overhead discharge, is calculated in mass percent, hydrogen chloride accounts for 96.91wt.%, pentafluoroethane accounts for
3.06wt.%, surplus are other components.
(2) hydrogen chloride gas being discharged at the top of the secondary condenser, through Primary diaphragm compressor compresses to 1.6MPa (G),
Enter back into level-one cryogenic condenser 80m2, second level cryogenic condenser 40m2Later, hydrogen chloride gas liquefies, is filling.Cryogenic temperature
It is -60 DEG C, deep cooling medium is fluoroform.
The structural schematic diagram of 2 use device of embodiment is as shown in figure 3, include the hydrogen chloride treating column 5 being sequentially connected, level-one
Condenser 6, secondary condenser 7, Primary diaphragm compressor 13, level-one cryogenic condenser 8, second level cryogenic condenser 9, surge tank
10,11, hydrogen chloride finished pot 12 are pumped.
Embodiment 3
In difluoromethane industrial production, by-product hydrogen chloride gas, perfluorinated reaction reflux column discharge.The gas pressure of discharge
For 1.25MPa (G), temperature is 15 DEG C.Gas contains the groups such as hydrogen chloride, difluoromethane, methylene chloride, fluoroform, hydrogen fluoride
Point.Its composition is calculated in mass percent, and hydrogen chloride accounts for 58.08wt.%, difluoromethane accounts for 39.90wt.%, methylene chloride accounts for
0.99wt.%, fluoroform account for 0.54wt.%, hydrogen fluoride accounts for 0.38wt.%, and surplus is other components.
The method of the present invention is as follows：
(1) above-mentioned hydrogen chloride gas 20Nm3/ h, through first-stage condenser 160m2, secondary condenser 100m2Condensation, removing are high
Object is boiled, is discharged from secondary condenser top.Level-one, secondary condenser temperature are controlled at -20 DEG C, and refrigerant is all made of dichloromethane
Alkane is multi-tube pass heat exchanger.The high-boiling components such as condensed difluoromethane, methylene chloride, hydrogen fluoride are recycled, technique is applied
In.The composition for the hydrogen chloride gas being discharged at the top of secondary condenser, is calculated in mass percent, hydrogen chloride accounts for 90.56wt.%, three
Fluoromethane accounts for 9.37wt.%, and surplus is other components.
(2) hydrogen chloride gas being discharged at the top of the secondary condenser, through Primary diaphragm compressor compresses to 2.5MPa (G),
Enter back into level-one cryogenic condenser 100m2, second level cryogenic condenser 60m2Later, hydrogen chloride gas liquefies, is filling.Cryogenic temperature
It is -40 DEG C, deep cooling medium is fluoroform.
Embodiment 4
P-chlorotoluene produces the hydrogen chloride gas of p-chlorotrichlormethyl, p-chloro benzo trifluoride-99 byproduct in process, through hydrogen chloride
The gas pressure of reflux condenser discharge, discharge is normal pressure, and temperature is room temperature, and gas contains hydrogen chloride, hydrogen fluoride, to one chlorine of chlorine
Toluene, to components such as chlorine dichlorotoleune, p-chloro benzo trifluoride-99s.Its composition is calculated in mass percent, hydrogen chloride account for 92.68wt.%,
Hydrogen fluoride accounts for 6.15wt.%, 0.37wt.% is accounted for chlorine monochlorotoluene, accounts for 0.19wt.% to chlorine dichlorotoleune, to chlorine fluoroform
Benzene accounts for 0.49wt.%, and surplus is other components.
The method of the present invention is as follows：
(1) above-mentioned hydrogen chloride gas 6Nm3/ h, through first-stage condenser 100m2, secondary condenser 60m2Condensation removes high boiling
Object is discharged from secondary condenser top.Level-one, secondary condenser temperature are controlled at -35 DEG C, and refrigerant is all made of methylene chloride,
It is multi-tube pass heat exchanger.By condensed hydrogen fluoride, to chlorine monochlorotoluene, contour to chlorine dichlorotoleune, p-chloro benzo trifluoride-99
Object recycling is boiled, is applied in technique.The composition for the hydrogen chloride gas being discharged at the top of secondary condenser, is calculated in mass percent, chlorination
Hydrogen accounts for 99.12wt.%, hydrogen fluoride accounts for 0.8wt.%, and surplus is other components.
(2) hydrogen chloride gas being discharged at the top of secondary condenser is compressed into level-one, stage piston-type compressor
1.6MPa (G) enters back into level-one cryogenic condenser 100m2, second level cryogenic condenser 60m2Later, hydrogen chloride gas liquefaction, filling
Dress.Cryogenic temperature is -45 DEG C, and deep cooling medium is fluoroform.
Embodiment 5
The hydrogen chloride gas of by-product in Tritox production process, is discharged through hydrogen chloride reflux condenser, the gas of discharge
Pressure is 0.03MPa (G), and temperature is 5 DEG C.Gas contains the components such as hydrogen chloride, acetonitrile, chlorine.It is formed with mass percent
Meter, hydrogen chloride accounts for 96.85wt.%, acetonitrile accounts for 1.87wt.%, chlorine accounts for 1.2wt.%, and surplus is other components.
(1) above-mentioned hydrogen chloride gas 5Nm3/ h, through first-stage condenser 40m2, secondary condenser 80m2Condensation removes high boiling
Object is discharged from secondary condenser top.Level-one, secondary condenser temperature are controlled at -25 DEG C, and refrigerant is all made of methylene chloride,
It is multi-tube pass heat exchanger.The high-boiling components such as condensed acetonitrile are recycled, are applied in technique.The chlorine being discharged at the top of secondary condenser
The composition for changing hydrogen, is calculated in mass percent, and hydrogen chloride accounts for 99.41wt.%, chlorine accounts for 0.53wt.%, and surplus is other groups
Point.
(2) hydrogen chloride gas being discharged at the top of secondary condenser, enters back into level-one cryogenic condenser 60m2Later, chlorination
Hydrogen liquefies, is filling.Cryogenic temperature is -80 DEG C, and deep cooling medium is nitrogen.
Other components described in embodiment 1-5 are the lower inevitable conventional constituents of content.
As shown in Figure 1, the device that the present invention uses, including by-product hydrogen chloride gas discharge nozzle 1, by-product hydrogen chloride gas goes out
Expects pipe 1 is sequentially connected with condenser 2, liquefying plant 3, filling apparatus 4.
Wherein：
The condenser 2 is one or more levels multi-tube pass heat exchanger.
The liquefying plant 3 is the combination of cryogenic condenser either compressor and cryogenic condenser.
The cryogenic condenser is one or more levels.
The compressor is one or more levels, and level-one uses diaphragm type compressor, and multistage uses piston compressor.
Surge tank 10 is set between the liquefying plant 3 and filling apparatus 4.
Device used in embodiment 1-5 is the preferred embodiment of above-mentioned apparatus.
Claims (10)
1. a kind of method with by-product hydrogen chloride gas production liquid hydrogen chloride, it is characterised in that：It is with by-product hydrogen chloride gas
Raw material, it is re-liquefied, filling first after condensation and removal high-boiling components.
2. the method according to claim 1 with by-product hydrogen chloride gas production liquid hydrogen chloride, it is characterised in that：It is described
By-product hydrogen chloride gas is discharged after condenser condensation and removal high-boiling components from condenser overhead；The high-boiling components are from condenser bottom
Portion is discharged, in recovery technique.
3. the method according to claim 2 with by-product hydrogen chloride gas production liquid hydrogen chloride, it is characterised in that：It is described
Condenser is one or more levels；The condenser is multi-tube pass heat exchanger；The temperature of the condenser is -5~-40 DEG C, condensation
Refrigerant is calcium chloride water, methylene chloride or the fluoroform of 25~28wt.% of mass percent in device.
4. the method according to claim 1 with by-product hydrogen chloride gas production liquid hydrogen chloride, it is characterised in that：It is described
Liquefaction is to liquefy after deep cooling or first after compression, then cryogenic liquefying.
5. the method according to claim 4 with by-product hydrogen chloride gas production liquid hydrogen chloride, it is characterised in that：It is described
Deep cooling medium is fluoroform.
6. the method according to claim 5 with by-product hydrogen chloride gas production liquid hydrogen chloride, it is characterised in that：
(1) filling after deep cooling liquefies by-product hydrogen chloride gas when the by-product hydrogen chloride gas pressure >=0.6MPa；Or
Person is filling after compression, deep cooling liquefy hydrogen chloride gas；
(2) when the by-product hydrogen chloride gas pressure is less than 0.6MPa, after compression, deep cooling liquefy by-product hydrogen chloride gas,
It is filling.
7. the method according to claim 4 with by-product hydrogen chloride gas production liquid hydrogen chloride, it is characterised in that：It is described
Deep cooling medium is liquid nitrogen.
8. the method according to claim 7 with by-product hydrogen chloride gas production liquid hydrogen chloride, it is characterised in that：Through depth
It is cold by-product hydrogen chloride gas is liquefied after, it is filling.
9. according to any method with by-product hydrogen chloride gas production liquid hydrogen chloride of claim 4~8, feature exists
In：The cryogenic temperature is -45~-110 DEG C, and the deep cooling is one or more levels；The boil down to one or more levels, level-one is adopted
With diaphragm type compressor, multistage uses piston compressor.
10. a kind of realize any dress with by-product hydrogen chloride gas production liquid chlorine hydrogen methods of claim 1~9
It sets, including by-product hydrogen chloride gas discharge nozzle, it is characterised in that：By-product hydrogen chloride gas discharge nozzle and condenser, liquefying plant,
Filling apparatus is sequentially connected；Wherein, the condenser is one or more levels, and the condenser is multi-tube pass heat exchanger；The liquid
Makeup is set to the combination of cryogenic condenser either compressor and cryogenic condenser；The cryogenic condenser is one or more levels；
The compressor is one or more levels, and level-one uses diaphragm type compressor, and multistage uses piston compressor；The liquefying plant with
Surge tank is set between filling apparatus.
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| CN201710345188.7A CN108862197A (en) | 2017-05-16 | 2017-05-16 | With the method and device thereof of by-product hydrogen chloride gas production liquid hydrogen chloride |
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| CN201710345188.7A CN108862197A (en) | 2017-05-16 | 2017-05-16 | With the method and device thereof of by-product hydrogen chloride gas production liquid hydrogen chloride |
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Application publication date: 20181123 |