CN107056581A - The separation method of the high-boiling components of the Difluoroethane production technology of 1 chlorine 1,1 - Google Patents
The separation method of the high-boiling components of the Difluoroethane production technology of 1 chlorine 1,1 Download PDFInfo
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- CN107056581A CN107056581A CN201710363889.3A CN201710363889A CN107056581A CN 107056581 A CN107056581 A CN 107056581A CN 201710363889 A CN201710363889 A CN 201710363889A CN 107056581 A CN107056581 A CN 107056581A
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- 238000009835 boiling Methods 0.000 title claims abstract description 56
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 41
- 238000005516 engineering process Methods 0.000 title claims abstract description 38
- 238000000926 separation method Methods 0.000 title claims abstract description 22
- NPNPZTNLOVBDOC-UHFFFAOYSA-N 1,1-difluoroethane Chemical compound CC(F)F NPNPZTNLOVBDOC-UHFFFAOYSA-N 0.000 title abstract description 10
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title abstract description 8
- 229910052801 chlorine Inorganic materials 0.000 title abstract description 8
- 239000000460 chlorine Substances 0.000 title abstract description 8
- BOSAWIQFTJIYIS-UHFFFAOYSA-N 1,1,1-trichloro-2,2,2-trifluoroethane Chemical compound FC(F)(F)C(Cl)(Cl)Cl BOSAWIQFTJIYIS-UHFFFAOYSA-N 0.000 claims abstract description 32
- OIQOUHIUUREZOM-UHFFFAOYSA-N 1,1-dichloro-1,2-difluoroethane Chemical class FCC(F)(Cl)Cl OIQOUHIUUREZOM-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000007872 degassing Methods 0.000 claims abstract description 23
- 239000000470 constituent Substances 0.000 claims abstract description 10
- BHNZEZWIUMJCGF-UHFFFAOYSA-N 1-chloro-1,1-difluoroethane Chemical class CC(F)(F)Cl BHNZEZWIUMJCGF-UHFFFAOYSA-N 0.000 claims description 19
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims description 6
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 6
- PQIOSYKVBBWRRI-UHFFFAOYSA-N methylphosphonyl difluoride Chemical group CP(F)(F)=O PQIOSYKVBBWRRI-UHFFFAOYSA-N 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052731 fluorine Inorganic materials 0.000 abstract description 8
- 239000011737 fluorine Substances 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 14
- 238000004458 analytical method Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000004817 gas chromatography Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 125000001340 2-chloroethyl group Chemical class [H]C([H])(Cl)C([H])([H])* 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- SLGOCMATMKJJCE-UHFFFAOYSA-N 1,1,1,2-tetrachloro-2,2-difluoroethane Chemical class FC(F)(Cl)C(Cl)(Cl)Cl SLGOCMATMKJJCE-UHFFFAOYSA-N 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- SDUQYLNIPVEERB-QPPQHZFASA-N gemcitabine Chemical compound O=C1N=C(N)C=CN1[C@H]1C(F)(F)[C@H](O)[C@@H](CO)O1 SDUQYLNIPVEERB-QPPQHZFASA-N 0.000 description 2
- 229960005277 gemcitabine Drugs 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- LZCMQBRCQWOSHZ-UHFFFAOYSA-N 2-bromo-2,2-difluoroacetic acid Chemical compound OC(=O)C(F)(F)Br LZCMQBRCQWOSHZ-UHFFFAOYSA-N 0.000 description 1
- HTHNTJCVPNKCPZ-UHFFFAOYSA-N 2-chloro-1,1-difluoroethene Chemical class FC(F)=CCl HTHNTJCVPNKCPZ-UHFFFAOYSA-N 0.000 description 1
- HBAQYPYDRFILMT-UHFFFAOYSA-N 8-[3-(1-cyclopropylpyrazol-4-yl)-1H-pyrazolo[4,3-d]pyrimidin-5-yl]-3-methyl-3,8-diazabicyclo[3.2.1]octan-2-one Chemical class C1(CC1)N1N=CC(=C1)C1=NNC2=C1N=C(N=C2)N1C2C(N(CC1CC2)C)=O HBAQYPYDRFILMT-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- LYJKGSALBRSKNL-UHFFFAOYSA-N bromodifluoroacetyl chloride Chemical class FC(F)(Br)C(Cl)=O LYJKGSALBRSKNL-UHFFFAOYSA-N 0.000 description 1
- 239000007806 chemical reaction intermediate Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000004494 ethyl ester group Chemical group 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- UHCBBWUQDAVSMS-UHFFFAOYSA-N fluoroethane Chemical compound CCF UHCBBWUQDAVSMS-UHFFFAOYSA-N 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011275 oncology therapy Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of separation method, and in particular to a kind of separation method of the high-boiling components of the Difluoroethane production technology of 1 chlorine 1,1.The high-boiling components of the Difluoroethane production technology of 1 chlorine 1,1 are pre-processed in degassing tower, the Difluoroethane of 1 chlorine of light component 1,1 that recovered overhead goes out in high-boiling components；The heavy constituent of degassing tower tower reactor enters rectifying column 1#, and rectifying column 1# overhead condensers distillate finished product difluoro dichloroethanes；The heavy constituent of rectifying column 1# tower reactors enters rectifying column 2#, and rectifying column 2# overhead condensers distillate the trifluorotrichloroethane of finished product two.The composition of the high-boiling components mainly includes the Difluoroethane of 1 chlorine 1,1, difluoro dichloroethanes, two trifluorotrichloroethanes and its their isomer.The present invention isolates difluoro dichloroethanes and two trifluorotrichloroethanes from the high-boiling components of the Difluoroethane production technology of 1 chlorine 1,1, the problem of solving the fluorine wasting of resources, reduces cost, lifts economic benefit, is that positive contribution is made in environmental protection.
Description
Technical field
The present invention relates to a kind of separation method, and in particular to a kind of high-boiling components of 1- chlorine-1,1-difluoroethanes production technology
Separation method.
Background technology
1- chlorine-1,1-difluoroethanes (R142b) are the high temperature refrigerant that a kind of generality is used, polymer (plastics) foaming
The intermediate of agent, thermostatic control switch and aero propulsion agent, while also being used as producing Kynoar.Recently as the country
PVDF industries are developed rapidly, and the production capacity of each business unit 1- chlorine-1,1-difluoroethanes (R142b) expands day by day.
Occur dry method optical chlorinating reaction with chlorine in the A of the CN 101781164 1,1- Difluoroethanes (R152a) reported to produce
In the technique of 1- chlorine-1,1-difluoroethanes (R142b), the high-boiling components for about producing 4-7wt% { wherein mainly contain the 3- of entrainment
5wt% 1- chlorine-1,1-difluoroethanes (R142b), 30-40wt% difluoro dichloroethanes, the 10-20wt% chloroethene of difluoro three
Alkane and some other isomer or the similar heavy constituent impurity of structure }.The current chloro- 1,1- Difluoroethanes of 1- both domestic and external
(R142b) manufacturer disposes the high-boiling components using the method hoarded or burned mostly, cause serious environmental pollution and
The wasting of resources.
Difluoro dichloroethanes and two trifluorotrichloroethanes are all preferable fluorination work reaction intermediates.The A of CN 103965010 are reported
The side that the coproduction of liquid phase optical chlorinating reaction prepares two trifluorotrichloroethanes and difluoro tetrachloroethanes occurs for a kind of difluoro dichloroethanes in road
Method；CN 102992945 A, CN 105152852 the A and A of CN 104761446 report respectively use two trifluorotrichloroethanes for
Raw material prepares the chloro- 2,2- difluoroethylenes of fluorine fine chemical material 1-, the bromo- 1-2,2- difluoroethylenes of 1- of high added value
(R111211) and the bromo- 2,2- difluoroacetic acid chlorides of 2- and the bromo- 2,2- difluoro acetates of 2- method.Therefore the height boiling is rationally utilized
Thing, the problem of fluorine wasting of resources and environmental pollution can be solved perfectly.
The current country has begun to start to develop the profit of the high-boiling components of chloro- 1,1- Difluoroethanes (R142b) production technologies of 1-
With path, the problem of to attempt to solve the fluorine wasting of resources.Such as A of patent CN 102746150 report difluoromono-chloroethane productions
The high-boiling components of technique prepare the intermediate difluoro bromoacetic acid of cancer therapy drug gemcitabine (Gemcitabine) by series reaction
Ethyl ester；The high-boiling components of the A of patent CN 102766017 report chloro- 1,1- Difluoroethanes (R142b) production technologies of 1- are in illumination condition
Lower progress optical chlorinating reaction prepares tetrachlorodifluoroethane.It is complicated yet with high-boiling components composition and production technology path, produced
Uncontrollable factor is more in journey, and production cost is higher.By comparison, difluoro dichloroethanes and difluoro three are isolated from high-boiling components
The technology of chloroethanes can not only promote the exploitation in its new opplication field, the problem of solving the fluorine wasting of resources, and can reduce
Production cost, promotes environment-friendly development.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of 1- chlorine-1,1-difluoroethanes production technology
High-boiling components separation method, isolate difluoro dichloro from the high-boiling components of 1- chlorine-1,1-difluoroethanes (R142b) production technology
Ethane and two trifluorotrichloroethanes, are that positive contribution is made in the protection of environment the problem of to solve the fluorine wasting of resources.
The separation method of the high-boiling components of 1- chlorine-1,1-difluoroethanes production technology of the present invention, comprises the following steps：
(1) high-boiling components of 1- chlorine-1,1-difluoroethanes production technology are pre-processed in degassing tower, and recovered overhead goes out height boiling
The chloro- 1,1- Difluoroethanes of light component 1- in thing；
(2) heavy constituent of degassing tower tower reactor enters rectifying column 1#, and rectifying column 1# overhead condensers distillate finished product difluoro dichloro
Ethane；
(3) heavy constituent of rectifying column 1# tower reactors enters rectifying column 2#, and rectifying column 2# overhead condensers distillate finished product difluoro three
Chloroethanes.
Wherein：
The component light compared to difluoro dichloroethanes is reclaimed in overhead condenser top gas phase in rectifying column 1#.
Component of the rectifying column 2# tower reactors discharge compared to two trifluorotrichloroethanes weight.
The high-boiling components of 1- chlorine-1,1-difluoroethanes (R142b) production technology of the present invention are a kind of mixtures, be by
The chloro- 1,1- Difluoroethanes of the accessory substance higher than R142b boiling point and 1- produced in production process are mixed.The chloro- 1,1- bis- of 1-
The production technology of fluoroethane is to refer to 1,1- Difluoroethanes gas to occur the optical chlorinating reaction preparation chloro- 1,1- Difluoroethanes of 1- with chlorine
Process, the technique is this area common process.High-boiling components main component has the chloro- 1,1- Difluoroethanes (R142b) of 1-, difluoro two
Chloroethanes, two trifluorotrichloroethanes and its their isomer.
The high-boiling components composition of 1- chlorine-1,1-difluoroethane production technologies is complex, mainly contains the 3-5wt%'s of entrainment
1- chlorine-1,1-difluoroethanes, 30-40wt% difluoro dichloroethanes, 10-20wt% two trifluorotrichloroethanes and its theirs is same
Enantiomers.Described isomer is for component light compared to difluoro dichloroethanes in rectifying column 1#, compared to the chloroethene of difluoro three
The component of alkane weight.
The present invention is produced according to the difference of each component physical property using three rectifying columns to 1- chlorine-1,1-difluoroethanes
The high-boiling components of technique are handled, and are reclaimed out and are divided in 1- chlorine-1,1-difluoroethanes, rectifying column 1# and rectifying column 2# in degassing tower
Difluoro dichloroethanes and the high-purity product of two trifluorotrichloroethanes are not isolated.
The present invention using the difference of three rectifying columns according to each component boiling point in high-boiling components, isolate difluoro dichloroethanes and
Two trifluorotrichloroethanes.
The present invention operates degassing tower, rectifying column 1# and rectifying column 2# by the way of intermittently or serially, chloro- to isolate 1-
Difluoro dichloroethanes and two trifluorotrichloroethanes in 1,1- Difluoroethanes (R142b) production technology high-boiling components.
Wherein：
Degassing tower：55-80 DEG C of bottom temperature, tower reactor pressure 0.10-0.40MPa, 10-40 DEG C of tower top temperature, tower top pressure
0.05-0.35MPa.The height of chloro- 1,1- Difluoroethanes (R142b) production technologies of 1- is reclaimed by the way of condenser overhead is vented
Boil the light component R142b in thing.
85-120 DEG C of rectifying column 1# bottom temperature, tower reactor pressure 0.09-0.25MPa, 60-85 DEG C of tower top temperature, tower top
Pressure 0.04-0.20MPa.Rectifying column 1# overhead condensers distillate finished product difluoro dichloroethanes, and reflux ratio is 5-20；Rectifying simultaneously
Light component in tower 1# compared to difluoro dichloroethanes can also be reclaimed in overhead condenser top gas phase.
110-135 DEG C of rectifying column 2# bottom temperature, tower reactor pressure 0.10-0.25MPa, 85-110 DEG C of tower top temperature, tower
Pressure on top surface 0.05-0.20MPa.Overhead condenser distillates the trifluorotrichloroethane of finished product two, and rectifying column 2# reflux ratios are 5-20；Tower reactor is arranged
Go out the component compared to two trifluorotrichloroethanes weight.
The mode of operation of degassing tower, rectifying column 1# and rectifying column 2# is to be operated batch-wise or continuously.
The filler of degassing tower, rectifying column 1# and rectifying column 2# is stainless steel Pall ring, cascade ring or screen waviness packings.
As a kind of perferred technical scheme, the high-boiling components of 1- chlorine-1,1-difluoroethanes production technology of the present invention
Separation method, comprise the following steps：
Step 1：The high-boiling components (logistics 2) of chloro- 1,1- Difluoroethanes (R142b) production technologies of 1- are by high-boiling components storage tank through thing
Material conveying pump 1# is pre-processed into degassing tower, the light component 1- chlorine-1,1-difluoroethanes that recovered overhead goes out in high-boiling components
(R142b, logistics 3)；
Step 2：The heavy constituent (logistics 4) of degassing tower tower reactor enters rectifying column 1#, rectifying column 1# by material-handling pump 2#
Overhead condenser distillates finished product difluoro dichloroethanes (logistics 6), while component light compared to difluoro dichloroethanes in rectifying column 1#
Can be in overhead condenser recovered overhead (logistics 5)；
Step 3：The heavy constituent (logistics 7) of rectifying column 1# tower reactors enters rectifying column 2#, rectifying column by material-handling pump 3#
2# overhead condensers distillate the trifluorotrichloroethane of finished product two (logistics 8), and the discharge of rectifying column 2# tower reactors is compared to two trifluorotrichloroethanes weight
Component (logistics 9).
The material-handling pump that separating technology is used is canned motor pump, measuring pump or pneumatic diaphragm pump.
Rectifying column 1# recovered overheads compared to the light component of difluoro dichloroethanes can centralized collection, for secondary separation, enter
Onestep extraction has the fluorine-containing heavy constituent of value.
In summary, the present invention has advantages below：
The present invention isolates difluoro dichloroethanes and two trifluorotrichloroethanes according to the difference of each component boiling point in high-boiling components,
The problem of solving the fluorine wasting of resources in 1- chlorine-1,1-difluoroethanes (R142b) production technology, reduces chloro- 1, the 1- difluoros of 1-
The production cost of ethane (R142b), promotes the further exploitation in fluoride new opplication field, improves the economic effect of enterprise
Benefit, the protection to environmental resource is made that positive contribution.
Brief description of the drawings
Fig. 1 is the technique stream of the separation method of the high-boiling components of the chloro- 1,1- Difluoroethanes production technologies of 1- of the present invention
Cheng Tu；
In figure：I-high-boiling components storage tank, II-material-handling pump 1#, III-degassing tower, IV-material-handling pump 2#, V-rectifying column
1#, VI-material-handling pump 3#, VII-rectifying column 2#.
Embodiment
With reference to embodiment, the present invention will be further described.
Embodiment carries out analysis detection using Japanese Shimadzu Corporation gas-chromatography.
The equipment that embodiment is used：
High-boiling components storage tank is horizontal or vertical storage tank；Degassing tower, rectifying column 1# are identical with rectifying column 2# tower body sizes, tower height
For 25-30 meters, tower diameter is DN200-DN350, and filler is stainless steel Pall ring, cascade ring or screen waviness packings.
Fig. 1 is the technique stream of the separation method of the high-boiling components of the chloro- 1,1- Difluoroethanes production technologies of 1- of the present invention
Cheng Tu；
1-9 corresponds to logistics 1-9 respectively in figure, specific as follows：
1st, high-boiling components, mainly contain 1- chlorine-1,1-difluoroethanes (R142b), difluoro dichloroethanes, two trifluorotrichloroethanes and
Its their isomer；
2nd, the chloro- 1,1- Difluoroethanes (R142b) of 1-, difluoro dichloroethanes, two trifluorotrichloroethanes and its they same point it is different
Structure body；
3rd, the chloro- 1,1- Difluoroethanes (R142b) of 1-；
4th, difluoro dichloroethanes, two trifluorotrichloroethanes and its their isomer；
5th, the component light compared to difluoro dichloroethanes；
6th, difluoro dichloroethanes；
7th, two trifluorotrichloroethanes and some other components heavy compared to two trifluorotrichloroethanes；
8th, two trifluorotrichloroethane；
9th, compared to the component of two trifluorotrichloroethanes weight.
Embodiment 1
The high-boiling components of chloro- 1,1- Difluoroethanes (R142b) production technologies of 1- are entered by high-boiling components storage tank through material-handling pump 1#
Enter 2 tons of materials of degassing tower, control the degassing tower operating parameter fluctuation range to be：55-60 DEG C of bottom temperature, tower reactor pressure 0.10-
0.20MPa, 10-18 DEG C of tower top temperature, tower top pressure 0.05-0.15MPa.
Analysis detection is carried out to degassing column overhead and tower reactor sample using gas-chromatography.According to sampling analysis result, when de-
Gas tower component is kept after balance, and the interval that tower top starts reclaims the light component 1- chlorine-1,1-difluoroethanes (R142b) in high-boiling components；
When 1- chlorine-1,1-difluoroethanes (R142b) is not present in degassing tower tower reactor, fed through material-handling pump 2# toward rectifying column 1#.
The rectifying column 1# operating parameter fluctuation ranges are controlled to be：85-95 DEG C of bottom temperature, tower reactor pressure 0.09-0.15MPa,
60-66 DEG C of tower top temperature, tower top pressure 0.04-0.10MPa.
Analysis detection is carried out to rectifying column 1# tower tops and tower reactor sample using gas-chromatography.According to sampling analysis result, when
Rectifying column 1# components are kept after balance, and rectifying column 1# overhead condensers distillate finished product difluoro dichloroethanes；When rectifying column 1# tower reactors
During in the absence of difluoro dichloroethanes, fed through material-handling pump 3# toward rectifying column 2#.
The rectifying column 2# operating parameter fluctuation ranges are controlled to be：110-120 DEG C of bottom temperature, tower reactor pressure 0.10-
0.15MPa, 85-95 DEG C of tower top temperature, tower top pressure 0.05-0.10MPa.
Analysis detection is carried out to rectifying column 2# tower tops and tower reactor sample using gas-chromatography.According to sampling analysis result, when
Rectifying column 2# components are kept after balance, and rectifying column 2# overhead condensers distillate the trifluorotrichloroethane of finished product two；When rectifying column 2# tower reactors
During in the absence of two trifluorotrichloroethanes, bottom product is discharged.
The purity of returned logistics 3 is：96.37wt%1- chlorine-1,1-difluoroethanes (R142b), the chloroethene of 3.63wt% difluoros two
Alkane；The purity of logistics 6 is：99.72wt% difluoro dichloroethanes；The purity of logistics 8 is：The trifluorotrichloroethanes of 99.58wt% bis-.
Embodiment 2
Whole technique is controlled using continuous mode of operation, controls the degassing tower operating parameter fluctuation range to be：Bottom temperature
60-70 DEG C, tower reactor pressure 0.20-0.30MPa, 18-27 DEG C of tower top temperature, tower top pressure 0.15-0.25MPa；Rectifying column 1# is grasped
Making parameter fluctuation scope is：95-108 DEG C of bottom temperature, tower reactor pressure 0.15-0.20MPa, 65-78 DEG C of tower top temperature, tower top pressure
Power 0.10-0.15MPa；Rectifying column 2# operating parameter fluctuation range is：120-128 DEG C of bottom temperature, tower reactor pressure 0.15-
0.20MPa, 95-103 DEG C of tower top temperature, tower top pressure 0.10-0.15MPa.
The purity of returned logistics 3 is：The chloro- 1,1- Difluoroethanes (R142b) of 95.78wt%1-, the chloroethene of 4.22wt% difluoros two
Alkane；The purity of logistics 6 is：99.24wt% difluoro dichloroethanes；The purity of logistics 8 is：The trifluorotrichloroethanes of 99.69wt% bis-.
Embodiment 3
Whole technique is controlled using continuous mode of operation, controls the degassing tower operating parameter fluctuation range to be：Bottom temperature
70-80 DEG C, tower reactor pressure 0.30-0.40MPa, 25-40 DEG C of tower top temperature, tower top pressure 0.25-0.35MPa；Rectifying column 1# is grasped
Making parameter fluctuation scope is：110-120 DEG C of bottom temperature, tower reactor pressure 0.20-0.25MPa, 78-85 DEG C of tower top temperature, tower top
Pressure 0.15-0.20MPa；Rectifying column 2# operating parameter fluctuation range is：128-135 DEG C of bottom temperature, tower reactor pressure 0.20-
0.25MPa, 103-110 DEG C of tower top temperature, tower top pressure 0.15-0.20MPa.
The purity of returned logistics 3 is：94.39wt%1- chlorine-1,1-difluoroethanes (R142b), the chloroethene of 5.61wt% difluoros two
Alkane；The purity of logistics 6 is：99.13wt% difluoro dichloroethanes；The purity of logistics 8 is：The trifluorotrichloroethanes of 99.27wt% bis-.
Claims (10)
1. a kind of separation method of the high-boiling components of 1- chlorine-1,1-difluoroethanes production technology, it is characterised in that：Including following step
Suddenly：
(1) high-boiling components of 1- chlorine-1,1-difluoroethanes production technology are pre-processed in degassing tower, and recovered overhead goes out in high-boiling components
The chloro- 1,1- Difluoroethanes of light component 1-；
(2) heavy constituent of degassing tower tower reactor enters rectifying column 1#, and rectifying column 1# overhead condensers distillate finished product difluoro dichloroethanes；
(3) heavy constituent of rectifying column 1# tower reactors enters rectifying column 2#, and rectifying column 2# overhead condensers distillate the chloroethene of finished product difluoro three
Alkane.
2. the separation method of the high-boiling components of 1- chlorine-1,1-difluoroethanes production technology according to claim 1, its feature exists
In：The component light compared to difluoro dichloroethanes is reclaimed in overhead condenser top gas phase in rectifying column 1#.
3. the separation method of the high-boiling components of 1- chlorine-1,1-difluoroethanes production technology according to claim 1, its feature exists
In：Component of the rectifying column 2# tower reactors discharge compared to two trifluorotrichloroethanes weight.
4. the separation method of the high-boiling components of 1- chlorine-1,1-difluoroethanes production technology according to claim 1, its feature exists
In：55-80 DEG C of the bottom temperature of degassing tower, tower reactor pressure 0.10-0.40MPa, 10-40 DEG C of tower top temperature, tower top pressure 0.05-
0.35MPa。
5. the separation method of the high-boiling components of 1- chlorine-1,1-difluoroethanes production technology according to claim 1, its feature exists
In：85-120 DEG C of rectifying column 1# bottom temperature, tower reactor pressure 0.09-0.25MPa, 60-85 DEG C of tower top temperature, tower top pressure
0.04-0.20MPa。
6. the separation method of the high-boiling components of 1- chlorine-1,1-difluoroethanes production technology according to claim 1 or 5, it is special
Levy and be：Rectifying column 1# reflux ratio is 5-20.
7. the separation method of the high-boiling components of 1- chlorine-1,1-difluoroethanes production technology according to claim 1, its feature exists
In：110-135 DEG C of rectifying column 2# bottom temperature, tower reactor pressure 0.10-0.25MPa, 85-110 DEG C of tower top temperature, tower top pressure
0.05-0.20MPa。
8. the separation method of the high-boiling components of the 1- chlorine-1,1-difluoroethane production technologies according to claim 1 or 7, it is special
Levy and be：Rectifying column 2# reflux ratio is 5-20.
9. the separation method of the high-boiling components of 1- chlorine-1,1-difluoroethanes production technology according to claim 1, its feature exists
In：The mode of operation of degassing tower, rectifying column 1# and rectifying column 2# is to be operated batch-wise or continuously.
10. the separation method of the high-boiling components of 1- chlorine-1,1-difluoroethanes production technology according to claim 1, its feature
It is：The high-boiling components main component have the chloro- 1,1- Difluoroethanes of the 1- of entrainment, difluoro dichloroethanes, two trifluorotrichloroethanes and its
Their isomer.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781164A (en) * | 2010-02-10 | 2010-07-21 | 山东东岳化工有限公司 | Preparation method of difluoromono-chloroethane |
| CN102766017A (en) * | 2012-07-31 | 2012-11-07 | 山东华安新材料有限公司 | Preparation method of tetrachloro-1,2-difluoroethane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101781164A (en) * | 2010-02-10 | 2010-07-21 | 山东东岳化工有限公司 | Preparation method of difluoromono-chloroethane |
| CN102766017A (en) * | 2012-07-31 | 2012-11-07 | 山东华安新材料有限公司 | Preparation method of tetrachloro-1,2-difluoroethane |
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| CN113372214A (en) * | 2021-06-03 | 2021-09-10 | 常熟三爱富振氟新材料有限公司 | Continuous rectification process of F112 |
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