CN106076101B - A kind of tail gas defluorinate absorption plant and its implementation - Google Patents
A kind of tail gas defluorinate absorption plant and its implementation Download PDFInfo
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- CN106076101B CN106076101B CN201610670301.4A CN201610670301A CN106076101B CN 106076101 B CN106076101 B CN 106076101B CN 201610670301 A CN201610670301 A CN 201610670301A CN 106076101 B CN106076101 B CN 106076101B
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- tail gas
- absorption tower
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- absorption
- chloride
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- 238000010521 absorption reaction Methods 0.000 title claims abstract description 218
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 158
- 239000007788 liquid Substances 0.000 claims abstract description 90
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 72
- 238000000034 method Methods 0.000 claims abstract description 27
- 239000006227 byproduct Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000000694 effects Effects 0.000 claims abstract description 11
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 239000012267 brine Substances 0.000 claims abstract description 6
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000012530 fluid Substances 0.000 claims description 39
- 238000006243 chemical reaction Methods 0.000 claims description 29
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 15
- 239000000945 filler Substances 0.000 claims description 15
- 239000007921 spray Substances 0.000 claims description 14
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052801 chlorine Inorganic materials 0.000 claims description 9
- 125000004122 cyclic group Chemical group 0.000 claims description 8
- 238000004090 dissolution Methods 0.000 claims description 7
- 238000009826 distribution Methods 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- NXFLUFCZKPBUCP-UHFFFAOYSA-N ClC=1C(=C(C=CC1)OC)Cl.[F] Chemical compound ClC=1C(=C(C=CC1)OC)Cl.[F] NXFLUFCZKPBUCP-UHFFFAOYSA-N 0.000 claims description 6
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 150000002118 epoxides Chemical class 0.000 claims description 4
- 239000013589 supplement Substances 0.000 claims description 4
- XEMRAKSQROQPBR-UHFFFAOYSA-N (trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=CC=C1 XEMRAKSQROQPBR-UHFFFAOYSA-N 0.000 claims description 3
- MFHPYLFZSCSNST-UHFFFAOYSA-N 1-chloro-2-(trichloromethyl)benzene Chemical compound ClC1=CC=CC=C1C(Cl)(Cl)Cl MFHPYLFZSCSNST-UHFFFAOYSA-N 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- PQIOSYKVBBWRRI-UHFFFAOYSA-N methylphosphonyl difluoride Chemical group CP(F)(F)=O PQIOSYKVBBWRRI-UHFFFAOYSA-N 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims 1
- 238000006115 defluorination reaction Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 113
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 41
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 41
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 14
- 239000000463 material Substances 0.000 description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 7
- 229910052731 fluorine Inorganic materials 0.000 description 6
- FRGGQBXYUVXSDW-UHFFFAOYSA-N C1(=CC=CC=C1)C(Cl)Cl.[F] Chemical compound C1(=CC=CC=C1)C(Cl)Cl.[F] FRGGQBXYUVXSDW-UHFFFAOYSA-N 0.000 description 5
- 239000011737 fluorine Substances 0.000 description 5
- 238000005660 chlorination reaction Methods 0.000 description 4
- 230000001351 cycling effect Effects 0.000 description 4
- 238000003682 fluorination reaction Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- OVUKQQRPTLPXTD-UHFFFAOYSA-N 1-(chloromethyl)-2,3-difluorobenzene Chemical compound FC1=CC=CC(CCl)=C1F OVUKQQRPTLPXTD-UHFFFAOYSA-N 0.000 description 2
- DGRVQOKCSKDWIH-UHFFFAOYSA-N 1-chloro-2-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=CC=C1Cl DGRVQOKCSKDWIH-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- GETTZEONDQJALK-UHFFFAOYSA-N (trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=CC=C1 GETTZEONDQJALK-UHFFFAOYSA-N 0.000 description 1
- GOYDNIKZWGIXJT-UHFFFAOYSA-N 1,2-difluorobenzene Chemical compound FC1=CC=CC=C1F GOYDNIKZWGIXJT-UHFFFAOYSA-N 0.000 description 1
- CAHQGWAXKLQREW-UHFFFAOYSA-N Benzal chloride Chemical compound ClC(Cl)C1=CC=CC=C1 CAHQGWAXKLQREW-UHFFFAOYSA-N 0.000 description 1
- 101100165177 Caenorhabditis elegans bath-15 gene Proteins 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- UMVPOPGPVLNLSL-UHFFFAOYSA-L [Ca+2].[F].[Cl-].[Cl-] Chemical compound [Ca+2].[F].[Cl-].[Cl-] UMVPOPGPVLNLSL-UHFFFAOYSA-L 0.000 description 1
- HXELGNKCCDGMMN-UHFFFAOYSA-N [F].[Cl] Chemical group [F].[Cl] HXELGNKCCDGMMN-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001805 chlorine compounds Chemical group 0.000 description 1
- -1 chloromethane epoxide Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- GQHWSLKNULCZGI-UHFFFAOYSA-N trifluoromethoxybenzene Chemical compound FC(F)(F)OC1=CC=CC=C1 GQHWSLKNULCZGI-UHFFFAOYSA-N 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- 150000005226 trifluoromethylbenzenes Chemical class 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/68—Halogens or halogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/20—Halogens or halogen compounds
- B01D2257/206—Organic halogen compounds
- B01D2257/2066—Fluorine
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Treating Waste Gases (AREA)
- Gas Separation By Absorption (AREA)
Abstract
The invention discloses a kind of tail gas defluorinate absorption plants, including reactor, cryogenic condenser, salt water enters pipe, first circulation liquid inlet/outlet pipe, brine outlet pipe, offgas outlet pipe, first grade absorption tower connection, first circulation liquid inlet/outlet pipe, first circulation pump, tail gas tandem tube, two-level absorption tower, it is connected between first grade absorption tower and two-level absorption tower by second circulation liquid inlet/outlet pipe, second circulation liquid inlet/outlet pipe is pumped equipped with second circulation, it is connect by exhaust emission tube with tail gas absorption by Hydrochloric Acid device at the top of two-level absorption tower, tail gas absorption by Hydrochloric Acid bottom of device is equipped with by-product hydrochloric acid discharge nozzle, two-level absorption tower is connect by chloride feed pipe with measuring tank, chloride delivery pump is provided on chloride feed pipe.The invention also discloses a kind of implementation methods of tail gas defluorinate absorption plant.The present invention has the characteristics that simple structure, low cost, multistage defluorinate, defluorination effect is good, protect environment and facilitates popularization.
Description
Technical field
The present invention relates to defluorinate absorption techniques, specifically a kind of tail gas defluorinate absorption plant and its implementation.
Background technique
Many important Organic fluoride chemicals such as fluorochloroparaffins, trifluomethoxybenzene the class, (letter of the products such as trifluoromethylbenzene class
Claim fluoride) it is obtained frequently with chlorine-fluorine exchange method, i.e., under certain temperature, pressure, chlorohydrocarbon or fragrant chlorocarbon (abbreviation chlorination
Object) and HF reaction, fluorine atom replaces chlorine atom, generation fluoride, while generating hydrogen chloride (HCL), passes through tail gas of releasing and keeps
It is mobile to fluoride direction is generated to be conducive to reaction for pressure.Because HF boiling point is lower (at 19 DEG C or so), in the tail gas released, with HCL
Based on gas, simultaneously containing a large amount of unreacted HF gases.Usual reaction end gas recycles HF's using multistage refrigerated condensation, deep cooling
Method, however still contain more HF in tail gas.The common method for further recycling HF has: 1, low-temperature liquefaction method, 2, sulfuric acid absorption
Method, 3, by-product hydrochloric acid defluorinate method.Low-temperature liquefaction method is compared with suitable for the scale of large-tonnage fluorochloroparaffins, continuous production, tail
Atmospheric pressure flow is more stable, and tail gas compression at high pressure and is freezed, and separates under low temperature liquid, and effect is good.But it is raw using batch process
It produces, flow and the pressure tail gas unstable in each stage of reaction, feed sump unload or the turn tail gas of the generations such as material should not be adopted
With liquefaction separation method.Sulfuric acid absorption method has certain dissolubility using HF in sulfuric acid, and the HF in tail gas is removed.But sulfuric acid is inhaled
Receipts method is big because there are sulfuric acid dosages, seriously corroded, and blocking and leakage easily occurs, and a small amount of sulfuric acid enters tail gas absorbing system, influences
The problems such as by-product hydrochloric acid quality.By-product hydrochloric acid defluorinate method is directly to absorb tail gas through water to generate by-product hydrochloric acid, in by-product hydrochloric acid
Fluorinion concentration is up to thousands of ppm, or even ppm up to ten thousand.Common calcium chloride fluorine removal processing.Hydrochloric acid fluoride-removing equipment requires tight, cost
Higher, the control of fluorinion concentration in hydrochloric acid is improper to be still higher than controlled concentration 150ppm value.
Many fluorides are produced, the exhaust flow and pressure of generation are in each reaction because production scale is few using batch process
Stage is unstable, feed sump unload or turn material etc. generations tail gas, should not use low-temperature liquefaction method, substituted sulfuric acid absorption process,
By-product hydrochloric acid defluorinate method.
Summary of the invention
It is an object of the invention to overcome above the shortcomings of the prior art, provide a kind of structure is simple, cost just
Preferably, chloride make absorbing liquid carry out plural serial stage defluorinate, defluorination effect is good, protects environment and the tail gas defluorinate of popularization is facilitated to absorb
Device.
The present invention also provides a kind of implementation methods of tail gas defluorinate absorption plant.
In order to achieve the above object, the invention adopts the following technical scheme: a kind of tail gas defluorinate absorption plant, including reaction
Device, reactor are connect by tail gas recycle pipe with cryogenic condenser, cryogenic condenser bottom equipped with salt water enter pipe and tail gas into
Entering pipe, cryogenic condenser top is equipped with brine outlet pipe and offgas outlet pipe, and offgas outlet pipe is connect with first grade absorption tower side,
First order absorption tower bottom is first circulation liquid bath, and circulation fluid outlet arranged at first circulation liquid bath bottom, circulation fluid outlet and the
One circulating pump connects, and first circulation pump discharge is connect with first order absorption top of tower, carries out cyclic absorption, first order absorption top of tower tail
Gas tandem tube is connect with two-level absorption tower side, and two-level absorption tower bottom is second circulation liquid bath, and second circulation liquid bath bottom has
Second circulation liquid outlet, second circulation liquid outlet and second circulation pump connect, second circulation pump discharge and two-level absorption tower
Top connection carries out cyclic absorption, has chloride feed pipe to connect with measuring tank at the top of second circulation liquid bath, chloride feed pipe
On be provided with chloride delivery pump；After the circulation fluid of first circulation liquid bath goes to reactor, by the circulation of second circulation liquid bath
Liquid goes to first circulation liquid bath, and second circulation liquid bath supplements fresh chloride by measuring tank；Pass through tail gas at the top of two-level absorption tower
Discharge pipe is connect with tail gas absorption by Hydrochloric Acid device, and tail gas absorption by Hydrochloric Acid bottom of device is equipped with by-product hydrochloric acid discharge nozzle.
Paddle is equipped in the reactor, paddle is connect with stirring motor.
It is equipped with filler in the first grade absorption tower and two-level absorption tower, is equipped with liquid distribution trough above filler, under filler
Side is equipped with gas-liquid separator, and gas-liquid separator is connected with corresponding circulation liquid bath.
The first grade absorption tower and two-level absorption tower are made of stainless steel.
The top of the first grade absorption tower and two-level absorption tower is equipped with spray head.
The absorption by Hydrochloric Acid device, as absorbing medium, is provided with graphite using water.
The exhaust emission tube is equipped with pressure gauge and flowmeter.
The implementation method of above-mentioned tail gas defluorinate absorption plant, comprising the following steps:
(1), the circulation fluid of first grade absorption tower pumps through first circulation chloride being pumped into reactor, two-level absorption tower circulation fluid
It is pumped through second circulation and chloride is pumped into first grade absorption tower, chloride is pumped by effect of the measuring tank through perchlorhydria delivery pump
Two-level absorption tower；
(2), first circulation liquid is added in reactor and anhydrous HF, anhydrous HF is reacted with chloride, generate HCL tail gas,
Contain more HF in HCL tail gas at this time；
(3), HCL and HF mixed tail gas enters cryogenic condenser, and most of HF is condensed back in cryogenic condenser to anti-
Device is answered, the uncooled HF of small part is exported in cryogenic condenser with HCL tail gas and is discharged, and cryogenic condenser outlet tail gas pressure is
0.05~0.3Mpa, flow are 15~50 cubes ms/h, and the volumetric concentration of HF is 2~5%；
(4), HF and HCL mixed tail gas enters first grade absorption tower, and the chloride in circulation fluid is after spraying, HF and chloride
The reaction of circulation fluid counter current contacting generates a fluorine dichloro methoxybenzene and HCL gas, and HCL gas is mixed into tail gas；Its temperature be 30~
80 DEG C, sprinkle density is in 30~100m3/m2h；
(5), the gas that first grade absorption tower is ejected enters two-level absorption tower bottom, and from two-level absorption tower top spray stream
Under chloride circulation fluid continue gas-liquid counter current haptoreaction；Its temperature is 30~80 DEG C, sprinkle density 30~
100m3/m2h；
(6), the gas being ejected from two-level absorption tower enters absorption by Hydrochloric Acid device, into its HF of the tail gas of absorption by Hydrochloric Acid device
Substantially by whole defluorinates or dissolution, tail gas pressure, flow are held essentially constant；
(7), the by-product hydrochloric acid that absorption by Hydrochloric Acid device obtains, at this point, fluorinion concentration≤150ppm in hydrochloric acid.
The chloride is trichlorine metoxybenzene；Chain reaction occurs for trichlorine metoxybenzene and HF, first replaces a chlorine original
Son releases HCL simultaneously, generates a fluorine dichloro methoxybenzene, then replaces a chlorine atom and generate one chloromethane epoxide benzene of difluoro, into one
Step reaction generates trifluomethoxybenzene；Its reaction equation are as follows:
Ar-COCL3+HF→Ar-COCL2F+HCL
Ar-COCL2F+HF→Ar-COCLF2+HCL
Ar-COCLF2+HF→Ar-COF3+HCL。
The chloride is trichlorine metoxybenzene, o-chlorotrichlorotoluene or benzotrichloride.
The present invention compared with the existing technology, have following advantages and effects
1, the present invention includes reactor, and reactor is connect by tail gas recycle pipe with cryogenic condenser, cryogenic condenser bottom
Portion enters pipe equipped with salt water and tail gas enters pipe, and cryogenic condenser top is equipped with brine outlet pipe and offgas outlet pipe, tail gas go out
Mouth pipe is connect with first grade absorption tower side, and first order absorption tower bottom is first circulation liquid bath, and circulation is arranged at first circulation liquid bath bottom
Liquid outlet, circulation fluid outlet and first circulation pump connect, and first circulation pump discharge is connect with first order absorption top of tower, is carried out
Cyclic absorption, first order absorption top of tower tail gas tandem tube are connect with two-level absorption tower side, and two-level absorption tower bottom is followed for second
Second circulation liquid outlet is arranged at ring liquid bath, second circulation liquid bath bottom, and second circulation liquid outlet and second circulation pump connect, the
It is connect at the top of two circulating-pump outlets and two-level absorption tower, carries out cyclic absorption, have chloride feed pipe at the top of second circulation liquid bath
It is connect with measuring tank, chloride delivery pump is provided on chloride feed pipe；When the circulation fluid of first circulation liquid bath goes to reaction
After device, first circulation liquid bath is gone to by the circulation fluid of second circulation liquid bath, second circulation liquid bath supplements fresh chlorination by measuring tank
Object；It is connect by exhaust emission tube with tail gas absorption by Hydrochloric Acid device at the top of two-level absorption tower, tail gas absorption by Hydrochloric Acid bottom of device is set
There is by-product hydrochloric acid discharge nozzle, there is good structure simple, low cost, multistage defluorinate, defluorination effect, protection environment and facilitates popularization
The features such as.
2, it is equipped with paddle in the reactor in the present invention, paddle connect with stirring motor, stirs evenly, reaction speed
Fastly, using effect is good.
3, it is equipped with filler in the first grade absorption tower and two-level absorption tower in the present invention, is equipped with liquid distribution above filler
Device, filler lower section are equipped with gas-liquid separator, and gas-liquid separator is connected with corresponding circulation liquid bath；Guarantee its reaction effect.
4, the top of the first grade absorption tower in the present invention and two-level absorption tower is equipped with spray head；Designed for can be equal
Even reaction, enlarged-area.
5, the exhaust emission tube in the present invention is equipped with pressure gauge and flowmeter；To improve flow measurement accuracy, carry out
Pressure compensation.
6, for the present invention to improve assimilation effect and comprehensive utilization of resources, reactor, which feeds intake, applies chlorination in first grade absorption tower
Object absorbing liquid, when the chloride in first grade absorption tower is pumped to reactor, the chloride cyclic absorption liquid pump in two-level absorption tower is extremely
First grade absorption tower continues cycling through absorption, and new chloride is added in two-level absorption tower.
7, the present invention is main absorption equipment with absorption tower, adaptable to exhaust flow and the fluctuation of tail gas pressure, is applicable in
In accomplished continuously or intermittently reacting, storage tank emptying turns various other tail gas such as material.
8, HF is chlorinated object absorption or dissolution in tail gas of the present invention, makees fluorination reaction raw material, absorbs raw material kind not increasing
In the case where class, the dosage of HF raw material can be reduced.
9, the chloride after cyclic absorption of the present invention is as production materials, on the quality of product, yield without influence.
10, the present invention uses chloride as circulating absorption solution, and stainless steel material can be selected, and equipment is simple, with low investment, operation
Stablize.
11, fluorinion concentration contained by hydrochloric acid of the present invention after water absorbs, lower than the standard of by-product hydrochloric acid sale regulation.It can
Fluorine ion pollution is reduced, comprehensive utilization range is expanded.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of tail gas defluorinate absorption plant.
Figure label is as follows with title:
| 1 | Reactor | 2 | Tail gas recycle pipe |
| 3 | Cryogenic condenser | 4 | Salt water enters pipe |
| 5 | Tail gas enters pipe | 6 | Brine outlet pipe |
| 7 | Offgas outlet pipe | 8 | First grade absorption tower |
| 9 | First circulation liquid bath | 10 | Circulation fluid outlet |
| 11 | First circulation pump | 12 | Tail gas tandem tube |
| 13 | Two-level absorption tower | 14 | Second circulation liquid bath |
| 15 | Second circulation liquid outlet | 16 | Second circulation pump |
| 17 | Chloride feed pipe | 18 | Measuring tank |
| 19 | Chloride delivery pump | 20 | Exhaust emission tube |
| 21 | Tail gas absorption by Hydrochloric Acid device | 22 | By-product hydrochloric acid discharge nozzle |
| 23 | Spray head | 24 | Paddle |
Specific embodiment
In order to facilitate the understanding of those skilled in the art, the present invention is made further specifically with reference to the accompanying drawings and embodiments
It is bright.
Embodiment 1:
As shown in Figure 1, a kind of tail gas defluorinate absorption plant, including reactor, reactor pass through tail gas recycle pipe and deep cooling
Condenser connection, cryogenic condenser bottom enters pipe equipped with salt water and tail gas enters pipe, and cryogenic condenser top goes out equipped with salt water
Mouth pipe and offgas outlet pipe, offgas outlet pipe are connect with first grade absorption tower side, and first order absorption tower bottom is first circulation liquid bath,
Circulation fluid outlet arranged at first circulation liquid bath bottom, and circulation fluid outlet and first circulation pump connect, first circulation pump discharge with
The connection of first order absorption top of tower, carries out cyclic absorption, and first order absorption top of tower tail gas tandem tube is connect with two-level absorption tower side,
Two-level absorption tower bottom is second circulation liquid bath, and second circulation liquid outlet is arranged at second circulation liquid bath bottom, and second circulation liquid goes out
Mouth pipe and second circulation pump connect, and connect at the top of second circulation pump discharge and two-level absorption tower, progress cyclic absorption, second circulation
There is chloride feed pipe to connect with measuring tank at the top of liquid bath, chloride delivery pump is provided on chloride feed pipe；It follows when first
After the circulation fluid of ring liquid bath goes to reactor, first circulation liquid bath, second circulation liquid are gone to by the circulation fluid of second circulation liquid bath
Slot supplements fresh chloride by measuring tank；It is connect by exhaust emission tube with tail gas absorption by Hydrochloric Acid device at the top of two-level absorption tower,
Tail gas absorption by Hydrochloric Acid bottom of device is equipped with by-product hydrochloric acid discharge nozzle.
Paddle is equipped in reactor in the present embodiment, paddle is connect with stirring motor；First grade absorption tower and second level
Be equipped with filler in absorption tower, liquid distribution trough be equipped with above filler, be equipped with gas-liquid separator below filler, gas-liquid separator and
Corresponding circulation liquid bath connection；First grade absorption tower and two-level absorption tower are made of stainless steel；First grade absorption tower and two-level absorption tower
Top be equipped with spray head；Absorption by Hydrochloric Acid device, as absorbing medium, is provided with graphite using water；Exhaust emission tube is equipped with pressure
Power table and flowmeter.
The implementation method of above-mentioned tail gas defluorinate absorption plant, comprising the following steps:
(1), the circulation fluid of first grade absorption tower pumps through first circulation chloride being pumped into reactor, two-level absorption tower circulation fluid
It is pumped through second circulation and chloride is pumped into first grade absorption tower, chloride is pumped by effect of the measuring tank through perchlorhydria delivery pump
Two-level absorption tower；
(2), first circulation liquid is added in reactor and anhydrous HF, anhydrous HF is reacted with chloride, generate HCL tail gas,
Contain more HF in HCL tail gas at this time；
(3), HCL and HF mixed tail gas enters cryogenic condenser, and most of HF is condensed back in cryogenic condenser to anti-
Device is answered, the uncooled HF of small part is exported in cryogenic condenser with HCL tail gas and is discharged, and cryogenic condenser outlet tail gas pressure is
0.05~0.3Mpa, flow are 15~50 cubes ms/h, and the volumetric concentration of HF is 2~5%；
(4), HF and HCL mixed tail gas enters first grade absorption tower, and the chloride in circulation fluid is after spraying, HF and chloride
The reaction of circulation fluid counter current contacting generates a fluorine dichloro methoxybenzene and HCL gas, and HCL gas is mixed into tail gas；Its temperature be 30~
80 DEG C, sprinkle density is in 30~100m3/m2h；
(5), the gas that first grade absorption tower is ejected enters two-level absorption tower bottom, and from two-level absorption tower top spray stream
Under chloride circulation fluid continue gas-liquid counter current haptoreaction；Its temperature is 30~80 DEG C, sprinkle density 30~
100m3/m2h；
(6), the gas being ejected from two-level absorption tower enters absorption by Hydrochloric Acid device, into its HF of the tail gas of absorption by Hydrochloric Acid device
Substantially by whole defluorinates or dissolution, tail gas pressure, flow are held essentially constant；
(7), the by-product hydrochloric acid that absorption by Hydrochloric Acid device obtains, at this point, fluorinion concentration≤150ppm in hydrochloric acid.
Chloride in the present embodiment is trichlorine metoxybenzene；Chain reaction occurs for trichlorine metoxybenzene and HF, first replaces
One chlorine atom releases HCL simultaneously, generates a fluorine dichloro methoxybenzene, then replaces a chlorine atom and generate one chloromethane epoxide of difluoro
Benzene, further reaction generates trifluomethoxybenzene；Its reaction equation are as follows:
Ar-COCL3+HF→Ar-COCL2F+HCL
Ar-COCL2F+HF→Ar-COCLF2+HCL
Ar-COCLF2+HF→Ar-COF3+HCL。
Embodiment 2:
Using anhydrous hydrofluoric acid and trichlorine metoxybenzene reaction production trifluomethoxybenzene.Using HF and trichlorine metoxybenzene
Reaction generates trifluomethoxybenzene and releases HCL gas simultaneously.The resulting HCL gas containing HF, multi-stage condensing recycle HF
Afterwards, the tail gas pressure through pressure relief device discharge is 0.15MPa, flow 22.3m3The volumetric concentration of/h, HF are about 3.7%,
The ratio of middle HCL and HF is about 30:1, and rate of discharge 113Kg/h, HF rate of discharge is 5.1Kg/h, and tail gas enters absorption work
Section, preceding second level use the defluorinate of chloride absorption tower, and the tail gas of discharge carries out multistage HCL and absorbs to obtain by-product hydrochloric acid.First order absorption
Tower and two-level absorption tower are equipped with liquid distribution trough and tetrafluoro material filler, liquid circulation slot and other attachmentes；Absorption tower and its attached
Part uses stainless steel；Chloride is sent to first grade absorption tower top spray with circulating pump and is flowed down, circulating fluid flow rate 10m3/ h is cold
Tail gas after solidifying enters from first order absorption tower bottom, and HF and the reaction of chloride circulation fluid counter current contacting generate a fluorine dichloro in tower
Methylbenzene and HCL gas, HCL gas are mixed into tail gas.The gas that first grade absorption tower is ejected enters two-level absorption tower bottom, with from
The chloride circulation fluid that two-level absorption tower top spray flows down continues gas-liquid counter current haptoreaction, ejects from two-level absorption tower
The gas come enters absorption by Hydrochloric Acid device, into the tail gas of absorption by Hydrochloric Acid device its HF substantially by whole defluorinates or dissolution, tail gas
Pressure, flow are held essentially constant, but the discharge volume concentration of HF is down to 0.075%.Absorb the fluorine in rear stage absorption tower
Dichloromethyl benzene concentration is 7.7%, and difluoro chloromethyl benzene concentration is 0.5%, and the non-oxygen determination of trifluoromethoxy benzene concentration goes out.Second level
A fluorine dichloromethyl benzene concentration in absorption tower is 3.2%, other not measure.Circulation fluid chloride temperature is 60 DEG C.Into salt
Concentration of hydrochloric acid is 32.1% after sour absorption plant, and wherein the concentration of fluorine ion is 78ppm.After absorbing reaction, first grade absorption tower
Chloride pumpable is used as fluorination reaction and feeds intake to reactor, then the chloride of two-level absorption tower is pumped to first grade absorption tower, second level
Fresh chloride is added in absorption tower, continues cycling through absorption.
Embodiment 3:
It is reacted using HF and o-chlorotrichlorotoluene, generates chlorobenzotrifluoride and release HCL gas simultaneously.Thus it generates and contains
The HCL gas of HF, after multi-stage condensing recycles HF, the tail gas pressure through pressure relief device discharge is 0.21MPa, flow 36.8m3/
The volumetric concentration of h, HF are about that the ratio of 3.2%, wherein HCL and HF is about 30:1, rate of discharge 263Kg/h, HF discharge speed
Rate is 8.6Kg/h, and tail gas enters absorption section, and preceding second level uses the defluorinate of chloride absorption tower, and the tail gas of discharge carries out multistage HCL
Absorption obtains by-product hydrochloric acid.First grade absorption tower and two-level absorption tower are equipped with liquid distribution trough and tetrafluoro material filler, liquid circulation
Slot and other attachmentes；Absorption tower and its attachment use stainless steel；Chloride is sent to first grade absorption tower top spray with circulating pump
It flows down, circulating fluid flow rate 15m3/ h, condensed tail gas enter from first order absorption tower bottom, HF and chloride circulation in tower
The reaction of liquid counter current contacting generates a fluorine xylylene dichlorides and HCL gas, and HCL gas is mixed into tail gas.First grade absorption tower top of tower goes out
The gas come enters two-level absorption tower bottom, continues gas with the chloride circulation fluid flowed down from two-level absorption tower top spray
The reaction of liquid counter current contacting, the gas being ejected from two-level absorption tower enters absorption by Hydrochloric Acid device, into the tail gas of absorption by Hydrochloric Acid device
Substantially by whole defluorinates or dissolution, tail gas pressure, flow are held essentially constant its HF, but the discharge volume concentration of HF is down to
0.076%.Absorbing one fluorine dichloromethyl benzene concentration of 2- chlorine in rear stage absorption tower is that 9.1%, 2- chlorine difluoro chloromethyl benzene is dense
Degree is that 0.76%, 2- chlorobenzotrifluoride concentration is not measured.One fluorine dichloromethyl benzene concentration of 2- chlorine is 2.9% in two-level absorption tower,
It is other not measure.Circulation fluid chloride temperature is 62 DEG C.After into absorption by Hydrochloric Acid device concentration of hydrochloric acid be 32.1%, wherein fluorine from
The concentration of son is 76ppm.After absorbing reaction, the chloride pumpable of first grade absorption tower to reactor is used as fluorination reaction and feeds intake, then
The chloride of two-level absorption tower is pumped to first grade absorption tower, fresh chloride is added in two-level absorption tower, continues cycling through and absorbs
Embodiment 4:
It uses anhydrous HF and benzenyl trichloride for raw material, is stirred to react generation trifluoromethyl at the temperature and pressure of setting
Benzene, while a large amount of HCl gas is generated, anhydrous HF is excessive in production process.The gas of generation, through multistage chilled brine deep cooling
Recycle HF after, by pressure relief device be discharged the HCl tail gas containing HF, tail gas pressure be 0.19MPa, flow be 26.5 cubic metres/
Hour, the volumetric concentration of HF is about that the ratio of 4%, wherein HCL and HF is about 30:1, rate of discharge 169Kg/h, HF discharge speed
Rate is 7Kg/h, and tail gas enters absorption section, and preceding second level uses the defluorinate of chloride absorption tower, and the tail gas of discharge carries out multistage HCL and inhales
Receipts obtain by-product hydrochloric acid.First grade absorption tower and two-level absorption tower are equipped with liquid distribution trough and tetrafluoro material filler, liquid circulation slot
And other attachmentes；Absorption tower and its attachment use stainless steel；Chloride is sent to first grade absorption tower top spray stream with circulating pump
Under, circulating fluid flow rate is 10 cubes ms/h, and condensed tail gas enters from first order absorption tower bottom, HF and chlorination in tower
The reaction of object circulation fluid counter current contacting generates a fluorine xylylene dichlorides and HCL gas, and HCL gas is mixed into tail gas.First order absorption tower top
Gas out enters two-level absorption tower bottom, continues with the chloride circulation fluid flowed down from two-level absorption tower top spray
Gas-liquid counter current haptoreaction, the gas being ejected from two-level absorption tower enter absorption by Hydrochloric Acid device, into the tail of absorption by Hydrochloric Acid device
Its HF of gas is substantially by whole defluorinates or dissolution, and tail gas pressure, flow are held essentially constant, but the discharge volume concentration of HF is down to
0.092%.The fluorine dichloromethyl benzene concentration for absorbing rear stage absorption tower is 8.5%, and difluoro chloromethyl benzene concentration is
0.7%, benzotrifluoride concentration is not measured.One fluorine dichloromethyl benzene concentration of two-level absorption tower is 3.6%, other not measure.It follows
Ring liquid chlorine compound temperature is 65 DEG C.Concentration of hydrochloric acid is 31.8% after into absorption by Hydrochloric Acid device, and wherein the concentration of fluorine ion is
97ppm.After absorbing reaction, the chloride pumpable in first grade absorption tower is used as fluorination reaction and feeds intake to reactor, then second level is inhaled
The chloride received in tower is pumped into first grade absorption tower, and fresh chloride is added in two-level absorption tower, continues cycling through absorption.
Above-mentioned specific embodiment is the preferred embodiment of the present invention, can not be limited the invention, and others are appointed
The change or other equivalent substitute modes what is made without departing from technical solution of the present invention, are included in protection of the invention
Within the scope of.
Claims (9)
1. a kind of implementation method of tail gas defluorinate absorption plant, tail gas defluorinate absorption plant includes reactor, and reactor passes through tail
Gas recovery tube is connect with cryogenic condenser, and cryogenic condenser bottom enters pipe equipped with salt water and tail gas enters pipe, cryogenic condenser
Top is equipped with brine outlet pipe and offgas outlet pipe, and offgas outlet pipe is connect with first grade absorption tower side, first order absorption tower bottom
For first circulation liquid bath, circulation fluid outlet is arranged at first circulation liquid bath bottom, and circulation fluid outlet and first circulation pump connect, the
One circulating-pump outlet is connect with first order absorption top of tower, carries out cyclic absorption, first order absorption top of tower tail gas tandem tube and second level
The connection of absorption tower side, two-level absorption tower bottom are second circulation liquid bath, and the outlet of second circulation liquid is arranged at second circulation liquid bath bottom
Pipe, second circulation liquid outlet and second circulation pump connect, and connect, are followed at the top of second circulation pump discharge and two-level absorption tower
Ring absorbs, and has chloride feed pipe to connect with measuring tank at the top of second circulation liquid bath, is provided with chloride on chloride feed pipe
Delivery pump；After the circulation fluid of first circulation liquid bath goes to reactor, first circulation is gone to by the circulation fluid of second circulation liquid bath
Liquid bath, second circulation liquid bath supplement fresh chloride by measuring tank；Pass through exhaust emission tube and tail gas salt at the top of two-level absorption tower
Sour absorption plant connection, tail gas absorption by Hydrochloric Acid bottom of device are equipped with by-product hydrochloric acid discharge nozzle；It is characterised in that it includes following step
It is rapid:
(1), the circulation fluid of first grade absorption tower pumps through first circulation chloride being pumped into reactor, and two-level absorption tower circulation fluid is through the
Chloride is pumped into first grade absorption tower by two circulating pumps, and chloride is pumped into second level by effect of the measuring tank through perchlorhydria delivery pump
Absorption tower；
(2), first circulation liquid is added in reactor and anhydrous HF, anhydrous HF is reacted with chloride, generate HCL tail gas, at this time
Contain more HF in HCL tail gas；
(3), HCL and HF mixed tail gas enters cryogenic condenser, and most of HF is condensed back to reactor in cryogenic condenser,
The uncooled HF of small part is exported in cryogenic condenser with HCL tail gas and is discharged, and it is 0.05 that cryogenic condenser, which exports tail gas pressure,
~0.3Mpa, flow are 15~50 cubes ms/h, and the volumetric concentration of HF is 2~5%；
(4), HF and HCL mixed tail gas enters first grade absorption tower, and the chloride in circulation fluid is after spraying, HF and chloride circulation
The reaction of liquid counter current contacting generates a fluorine dichloro methoxybenzene and HCL gas, and HCL gas is mixed into tail gas；Its temperature is 30~80 DEG C,
Sprinkle density is in 30~100m3/m2h；
(5), the gas that first grade absorption tower is ejected enters two-level absorption tower bottom, and flows down from two-level absorption tower top spray
Chloride circulation fluid continues gas-liquid counter current haptoreaction；Its temperature is 30~80 DEG C, and sprinkle density is in 30~100m3/m2h；
(6), the gas being ejected from two-level absorption tower enters absorption by Hydrochloric Acid device, and into the tail gas of absorption by Hydrochloric Acid device, its HF is basic
By whole defluorinates or dissolution, tail gas pressure, flow are held essentially constant；
(7), the by-product hydrochloric acid that absorption by Hydrochloric Acid device obtains, at this point, fluorinion concentration≤150ppm in hydrochloric acid.
2. the implementation method of tail gas defluorinate absorption plant according to claim 1, it is characterised in that: set in the reactor
There is paddle, paddle is connect with stirring motor.
3. the implementation method of tail gas defluorinate absorption plant according to claim 1, it is characterised in that: the first grade absorption tower
Be equipped with filler in two-level absorption tower, liquid distribution trough is equipped with above filler, gas-liquid separator, gas-liquid point are equipped with below filler
It is connected from device with corresponding circulation liquid bath.
4. the implementation method of tail gas defluorinate absorption plant according to claim 1, it is characterised in that: the first grade absorption tower
It is made with two-level absorption tower of stainless steel.
5. the implementation method of tail gas defluorinate absorption plant according to claim 1, it is characterised in that: the first grade absorption tower
Spray head is equipped with the top of two-level absorption tower.
6. the implementation method of tail gas defluorinate absorption plant according to claim 1, it is characterised in that: the absorption by Hydrochloric Acid dress
It sets using water as absorbing medium, is provided with graphite.
7. the implementation method of tail gas defluorinate absorption plant according to claim 1, it is characterised in that: the exhaust emission tube
It is equipped with pressure gauge and flowmeter.
8. the implementation method of tail gas defluorinate absorption plant according to claim 1, it is characterised in that: the chloride is three
Chloromethane epoxide benzene；Chain reaction occurs for trichlorine metoxybenzene and HF, first replaces a chlorine atom and releases HCL simultaneously, generates a fluorine
Dichloro methoxybenzene, then replace a chlorine atom and generate one chloromethane epoxide benzene of difluoro, further reaction generates trifluomethoxybenzene；
Its reaction equation are as follows:
Ar-COCL3+HF→Ar-COCL2F+HCL
Ar-COCL2F+HF→Ar-COCLF2+HCL
Ar-COCLF2+HF→Ar-COF3+HCL。
9. the implementation method of tail gas defluorinate absorption plant according to claim 1, it is characterised in that: the chloride is three
Chloromethane epoxide benzene, o-chlorotrichlorotoluene or benzotrichloride.
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| CN106672905A (en) * | 2016-12-27 | 2017-05-17 | 江苏三美化工有限公司 | Method and device for recycling by-product hydrochloric acid in methane fluorine compound production |
| CN108815996A (en) * | 2018-07-02 | 2018-11-16 | 江苏三美化工有限公司 | A kind of hydrofluorocarbon exhaust treatment system and its application method |
| CN111116523B (en) * | 2019-12-30 | 2021-09-07 | 浙江新和成股份有限公司 | System and process for producing alpha-chloro-alpha-acetyl-gamma-butyrolactone |
| CN112546803A (en) * | 2020-12-22 | 2021-03-26 | 中船重工（邯郸）派瑞特种气体有限公司 | Treatment system and method for cathode tail gas of nitrogen trifluoride electrolytic cell |
| CN115138184A (en) * | 2022-07-25 | 2022-10-04 | 福建康峰新材料有限公司 | Purification method of chlorination reaction tail gas and application thereof |
| CN117547928B (en) * | 2023-11-15 | 2024-06-18 | 上海开鸿环保科技有限公司 | Organic fluoro compound AHF method synthesis tail gas deep cooling coupling adsorption denitration purification system |
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Effective date of registration: 20231017 Address after: 354000 Xingling Platform, Phase III, Jintang Industrial Park, Shaowu City, Nanping City, Fujian Province Patentee after: Fujian Kangfeng New Materials Co.,Ltd. Address before: 322104 Bachelor's Residence Industry, Weishan Town, Dongyang City, Jinhua City, Zhejiang Province Patentee before: ZHEJIANG KANGFENG CHEMICALS Co.,Ltd. |