CN106380372B - A kind of purification process and purification devices of octafluoropropane - Google Patents
A kind of purification process and purification devices of octafluoropropane Download PDFInfo
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- CN106380372B CN106380372B CN201610779255.1A CN201610779255A CN106380372B CN 106380372 B CN106380372 B CN 106380372B CN 201610779255 A CN201610779255 A CN 201610779255A CN 106380372 B CN106380372 B CN 106380372B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- 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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/389—Separation; Purification; Stabilisation; Use of additives by adsorption on solids
Abstract
The present invention relates to a kind of purification process of octafluoropropane and purification devices, belong to field of fine chemical.The purification process first use cold-trap to octafluoropropane crude product gas arrange it is light and it is de- handle again, substantially reduce light component and heavy constituent impurity content；It is adsorbed again with adsorbent, makes H2O content reduces, and absorbed portion organic fluorocarbon compounds；Distillation technology is finally used, by controlling rectification parameters, higher boiling and low boiling impurity can be removed, make H2O content is less than 1ppm, and organic fluorocarbon compounds content is less than 1ppm, and total impurities content is less than 10ppm, reduces the cooling capacity consumed in distillation process and heat, and good economy performance can obtain the octafluoropropane that purity is greater than 99.999% after purification.The purification devices specifically include that cold-trap, adsorption tower and rectifying column, are suitable for the purification process and use.
Description
Technical field
The present invention relates to a kind of purification process of octafluoropropane and purification devices, belong to field of fine chemical.
Background technique
High-purity octafluoropropane electronic gas, as the cleaning agent and etching agent of electronic device, be applied to semiconductors manufacture and
Electronics industry.It is also higher and higher to the purity requirement of octafluoropropane as the requirement of semiconductor devices etching precision is higher and higher.One
As for, applied to large scale integrated circuit high-purity octafluoropropane purity be greater than 99.999%.
Main preparation method mainly uses hexafluoropropene or heptafluoro-propane and fluorine gas to react system to octafluoropropane at this stage
It is standby to obtain octafluoropropane, due in preparation process, being related to fluorination and/or pyroreaction, release amount of heat, it may occur that carbon-to-carbon,
Carbon-fluorine, carbon-hydrogen, carbon-chlorine key fracture and reconstruct, generate a large amount of fragment, dimer, polymer or other compound impurities,
The impurity is mainly fluorocarbons, many kinds of, some concentration are only 1 × 10-6Even 1 × 10-9Volume ratio (i.e. ppm or
Ppb) rank；In addition there are unreacted hexafluoropropenes and heptafluoro-propane and O2、N2、CO、CO2And H2The impurity such as O, therefore in order to
High-purity octafluoropropane is made, needs to purify the crude product octafluoropropane being prepared, removes the impurity.
Existing octafluoropropane purification process, is broadly divided into four classes.The first kind is the method for rectifying, but due to octafluoropropane
There are many middle dopant species, often there is boiling point and perfluoro alkane approaches or the impurity of azeotropic, it is difficult to be carried out with the method for rectifying pure
Change.Second class is the method for absorption, and common adsorbent is molecular sieve, active carbon and carbon molecular sieve etc., but some impurity are in institute
The adsorption capacity very little in adsorbent is stated, is difficult to remove in this way.Third class is catforming, by boiling point and perfluor alkane
The close impurity of hydrocarbon boiling point is decomposed or is converted to boiling point and the biggish impurity of perfluoro alkane boiling point difference, but this by catalyst
Kind method is often only effective to certain several specific impurity.4th class is membrane separation process, and the method for UF membrane can only divide at this stage
From with the biggish substance of octafluoropropane molecular size difference, such as nitrogen, helium, be more suitable for from the tail containing a large amount of inert gases
Perfluoro alkane is recycled in gas.
The purification process of the octafluoropropane has limitation, and in the prior art, single rectifying, absorption, catalysis turn
Change method and membrane separation process, which are all difficult to obtain all technical, all to meet the requirements, and purity is greater than 99.999% octafluoropropane.
Summary of the invention
In view of the defects existing in the prior art, one of the objects of the present invention is to provide a kind of purifying sides of octafluoropropane
Method, the purification process can remove fluorocarbons in octafluoropropane, O2、N2、CO、CO2And H2The impurity such as O reduce purification process
In spent cooling capacity and heat, equipment investment is few, and easy to operate, after purified, indices meet the requirements, octafluoropropane
Purity can be used for semicon industry and other relevant industries 99.999% or more.
The second object of the present invention is the provision of a kind of purification devices of octafluoropropane.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of purification process of octafluoropropane, steps are as follows for the purification process:
(1) octafluoropropane crude product conductance is entered in cold-trap of the temperature less than -90 DEG C, with 1 DEG C/min~2 DEG C/min rate
Heating, carries out arranging light processing at -90 DEG C~-40 DEG C, makes low-boiling light component impurity vaporization discharge, be greater than when temperature rises to -
40 DEG C, when being less than or equal to -20 DEG C, by treated, octafluoropropane crude product conductance enters to adsorb tower bottom, and temperature, which rises to, is greater than -20
DEG C, stop being passed through to absorption tower bottom, the higher heavy constituent impurity left in cold-trap is discharged, carries out de- reset at dirt
Reason；
The purity of the octafluoropropane crude product gas is 90%~99.99%；It is preferred that the octafluoropropane crude product gas is using existing
There are hexafluoropropene or heptafluoro-propane and the fluorine gas reaction in technology to be prepared.
(2) treated after octafluoropropane crude product gas enters adsorption tower, is 0MPa~0.5MPa, absorption temperature in adsorptive pressure
Degree is to contact at -10 DEG C~40 DEG C with the adsorbent in adsorption tower, and time of contact 0.1s~5s carries out adsorption treatment, inhaled
Attached treated gas；
The adsorbent is one or more of active carbon, molecular sieve and carbon molecular sieve, and preferably a kind of adsorbent is independent
It uses；The adsorbent partial size is 0.5mm~5mm；The adsorbent in 100 DEG C~300 DEG C heating and with flow velocity is using preceding
Inert gas or the nitrogen purging of 1L/min~100L/min is activated.
(3) bottom temperature of rectifying column is down to -90 DEG C~-60 DEG C, the gas after adsorption treatment, which is passed through in tower reactor, to liquefy,
Stop being passed through after liquefaction 50kg~500kg, heat tower reactor carries out rectifying, and control bottom temperature is -28 DEG C~32 DEG C, and pressure is
0.05MPa~0.94MPa, the tower top temperature of rectifying column are -30 DEG C~30 DEG C, and pressure is 0.04MPa~0.90MPa, makes to adsorb
Treated, and gas after infinite reflux 2h~16h, is arranged with the flow of 0.1kg/h~10kg/h from tower top between tower reactor and tower top
Out, the constituent and content of detection discharge gas, when each component meets the octafluoropropane index of required purity, described in collection
Discharge gas obtains high-purity octafluoropropane；When the impurity content in the component for detecting the discharge gas is more than or equal to required pure
When the octafluoropropane index of degree, stop collecting the discharge gas, and impurity content in tower reactor is unsatisfactory for high-purity octafluoropropane
It is required that octafluoropropane from tower reactor bottom be discharged；
Wherein, preferably as the impurity in discharge gas, i.e. O2、N2、CO、CO2、H2The content of O and organic carbon fluorine is less than table 1
In impurity content when, meet requirement of high-purity octafluoropropane to impurity content, collect the discharge gas and obtain high-purity octafluoro
Propane；When the impurity content in the component for detecting the discharge gas is more than or equal to the impurity content in table 1, stop collecting
The discharge gas, and the octafluoropropane that impurity content in tower reactor is unsatisfactory for high-purity octafluoropropane requirement is arranged from tower reactor bottom
Out；
Table 1
| Dopant species | O2 | N2 | CO | CO2 | H2O | Organic carbon fluorine |
| Content/ppm | 1 | 2 | 0.5 | 0.5 | 1.0 | 5.0 |
Wherein, organic carbon fluorine refers to the impurity containing carbon (C) atom and fluorine (F) atom, such as: carbon tetrafluoride, perfluoroethane,
Hexafluoropropene, heptafluoro-propane, dicholorodifluoromethane etc.；
The rectifying column is made of tower reactor, rectifying column and overhead condenser, and the rectifying column is stuffing rectification column or board-like
Rectifying column, preferably stuffing rectification column；
When the rectifying column is stuffing rectification column, filler is Pall ring, θ ring or Raschig ring；The material of the filler is
Polytetrafluoroethylene (PTFE), stainless steel, nickel or monel metal, preferably stainless steel；The diameter of the filler is 1mm~100mm, preferably
For 5mm~50mm；
When the rectifying column is plate distillation column, the number of plates is 20~80, preferably 30~50；
The material of the rectifying column is stainless steel, nickel or monel metal, preferably stainless steel；
The height of the rectifying column is 0.5m~15m, preferably 3m~8m；
The diameter of the rectifying column is 50mm~500mm, preferably 100mm~300mm；
It is preferred that the reflux ratio of the infinite reflux is 5~500, more preferably 20~30.
A kind of purification devices of octafluoropropane, the purification devices are suitable for a kind of purifying of octafluoropropane of the present invention
Method uses；The purification devices specifically include that cold-trap, adsorption tower and rectifying column.
Wherein, cold-trap top is equipped with cold-trap gas outlet, and cold-trap feed inlet is equipped in the middle part of cold-trap, and cold-trap bottom is de- equipped with cold-trap
Weight mouth, cold-trap lower part are equipped with temperature control equipment, pressure gauge P-1 and thermometer T-1.
It adsorbs tower bottom and is equipped with adsorption tower air inlet, adsorbent is placed in adsorption tower, is equipped with adsorption tower at the top of adsorption tower
Gas outlet, adsorption tower top are equipped with pressure gauge P-2, are equipped with thermometer T-2 in the middle part of adsorption tower.
Rectifying column is mainly made of tower reactor, rectifying column and overhead condenser；Tower reactor top is equipped with tower bottom of rectifying tower air inlet,
Temperature control equipment, pressure gauge P-3 and thermometer T-3 are equipped in the middle part of tower reactor, tower reactor bottom is equipped with tower bottom of rectifying tower outlet, tower
It pushes up and is equipped with pressure gauge P-4 and thermometer T-4 in the middle part of condenser.
Cold-trap takes off weight mouth and is connected with the pipeline for being equipped with valve V-3, and line end is outlet, and cold-trap gas outlet passes through pipe
Road is connect with adsorption tower air inlet, and on this pipeline, the rear of cold-trap gas outlet is successively arranged cold-trap and arranges light mouth and nitrogen purging
Outlet, flowmeter F-1 and valve V-1, cold-trap arranges light mouth and nitrogen purging exit is connected with the pipe for being equipped with valve V-2
Road, line end are outlet；Adsorption tower gas outlet is connect by pipeline with tower bottom of rectifying tower air inlet, on this pipeline, absorption
The rear of tower gas outlet is successively arranged adsorption tower sample tap and the import of nitrogen purging, flowmeter F-2 and valve V-4, adsorption tower take
Sample mouth and nitrogen purging entrance are connected with the pipeline for being equipped with valve V-5, and line end is outlet；At the top of overhead condenser
Equipped with pipeline, the pipeline is divided into two branches, and a branch road is equipped with valve V-7, and end is rectifying column outlet, another branch
Road is equipped with valve V-8, and end is tower top sample tap, and tower reactor bottom tower bottom of rectifying tower outlet is connected with one and is equipped with valve V-
6 pipeline, line end are outlet.
A kind of working method of the purification devices of octafluoropropane of the present invention is as follows, when not working, at all valves
In closed state:
(1) octafluoropropane crude product gas is imported in cold-trap of the temperature less than -90 DEG C by cold-trap feed inlet, with 1 DEG C/min
The rate of~2 DEG C/min heats up, and carries out arranging light processing at -90 DEG C~-40 DEG C, arrange in light treatment process, opens valve V-2, makes
The vaporization of low-boiling light component impurity is discharged from cold-trap gas outlet, is arranged by cold-trap and to be connected at light mouth and nitrogen purging outlet 3
Pipeline equipped with valve V-2 is discharged to the outside；It is greater than -40 DEG C when temperature rises to, when being less than or equal to -20 DEG C, opens valve V-1,
Valve V-2 is closed, making that treated, octafluoropropane crude product gas is discharged from cold-trap gas outlet, and it is light that cold-trap row is successively passed through by pipeline
Mouth and the outlet of nitrogen purging, flowmeter F-1 and valve V-1, are passed through absorption tower bottom from adsorption tower air inlet, when temperature rises to greatly
In -20 DEG C, valve V-1 is closed, stops being passed through to absorption tower bottom, opens valve V-3, the higher weight that will be left in cold-trap
Composition impurity is discharged to the outside from the pipeline equipped with valve V-3 that the de- weight mouth of cold-trap connects；
(2) adsorbent in adsorption tower is heated using preceding at 100 DEG C~300 DEG C, and is opened valve V-2 and valve V-5 and used
The inert gas or nitrogen purging that flow velocity is 1L/min~100L/min are activated, and valve V-2, processing are closed after the completion of activation
It is 0MPa~0.5MPa in adsorptive pressure, adsorption temp is -10 DEG C~40 DEG C after octafluoropropane crude product gas afterwards enters adsorption tower
It is lower to be contacted with the adsorbent in adsorption tower, time of contact 0.1s~5s, progress adsorption treatment, the gas after obtaining adsorption treatment,
The pipeline equipped with valve V-5 that import discharge connection is purged by adsorption tower sample tap and nitrogen, can post-process absorption
Gas composition ingredient and content detected, after detection close valve V-5；
(3) bottom temperature of rectifying column is down to -90 DEG C~-60 DEG C, opens valve V-4, the gas after adsorption treatment from
It is discharged by adsorption tower gas outlet, adsorption tower sample tap and the import of nitrogen purging, flowmeter F-2 and valve is successively passed through by pipeline
Door V-4, is passed through in tower reactor from tower bottom of rectifying tower air inlet and liquefies, and valve V-4 stopping is closed after the 50kg~500kg that liquefies and is passed through；
Heat tower reactor carries out rectifying, and control bottom temperature is -28 DEG C~32 DEG C, and pressure is 0.05MPa~0.94MPa, the tower of rectifying column
Pushing up temperature is -30 DEG C~30 DEG C, and pressure is 0.04MPa~0.90MPa, and the gas after making adsorption treatment is between tower reactor and tower top
After infinite reflux 2h~16h, with the flow of 0.1kg/h~10kg/h from pipeline discharge at the top of overhead condenser, valve V-8 is opened,
Gas after adsorption treatment is discharged from tower top sample tap, the constituent and content of detection discharge gas, when in discharge gas
Impurity, i.e. O2、N2、CO、CO2、H2When the content of O and organic carbon fluorine is less than the impurity content in table 1, meet high-purity octafluoropropane
Valve V-7 is opened in requirement to impurity content, is exported collection discharge gas from rectifying column and is obtained high-purity octafluoropropane；Work as detection
When being more than or equal to the impurity content in table 1 to the impurity content in the component of the discharge gas, valve V-7 and valve V- is closed
8, stop collecting discharge gas, opens valve V-6, impurity content in tower reactor is unsatisfactory for the octafluoro third of high-purity octafluoropropane requirement
Alkane is discharged from the tower bottom of rectifying tower outlet of tower reactor bottom.
Beneficial effect
1. the purification process is thick to octafluoropropane using cold-trap the present invention provides a kind of purification process of octafluoropropane
Product gas arrange it is light and it is de- handle again, then the method combined with distillation technology and adsorption technology reduces in distillation process and disappears
The cooling capacity and heat of consumption, good economy performance；
2. the present invention provides a kind of octafluoropropane purification process, fluorine carbon compound can be made after purification through the purification process
Object, O2、N2、CO、CO2And H2The impurity concentrations such as O be down to it is below the mark, obtain purity be greater than 99.999% octafluoropropane；
3. the purification process is thick to octafluoropropane using cold-trap the present invention provides a kind of purification process of octafluoropropane
Product gas arrange it is light and it is de- handle again, substantially reduce light component and heavy constituent impurity content, such as H2The impurity such as O, make adsorbent
Extend the time required to being saturated to impurity absorption, reduces adsorbent and desorb number.It reduces and arranges light weight and re-scheduling amount in distillation process, mention
High product yield；
4. the present invention provides a kind of octafluoropropane purification process, the method for rectifying is utilized in the prior art, it is difficult to make eight
H in fluoro-propane2O is down to 1ppm hereinafter, the purification process is by using adsorbent, makes the H into rectifying column2O content drop
It is low, make H2O content enters rectifying column, the H that when rectifying is enriched in tower reactor after being lower than 5ppm2O is reduced, while obtains overhead collection
Octafluoropropane H2O content is less than 1ppm；Adsorbent can also adsorb other impurities simultaneously, such as the organic fluorocarbon in part, reduce
The cooling capacity and heat consumed in distillation process, improves product yield；The adsorbent particle size is 0.5mm~5mm；Partial size
Size have an impact to the effect of absorption, when partial size is excessive, specific surface area is small, insufficient contact；Partial size is too small, will lead to pressure
It is excessive, and it is easy blocking adsorption tower and pipeline, the preferably described adsorbent is activated using preceding heating and with inert gas purge,
So that the impurity desorption of its absorption；
5. the purification process can be removed by control rectification parameters the present invention provides a kind of octafluoropropane purification process
Higher boiling and low boiling impurity are removed, fluorocarbons content is made to be less than 1ppm, total impurities content is less than 10ppm.
6. the purification devices are suitable for purifying of the present invention the present invention provides a kind of octafluoropropane purification devices
Method obtains the octafluoropropane that purity is greater than 99.999%.
Detailed description of the invention
Fig. 1 is purification devices used in the purification process of octafluoropropane a kind of in embodiment.
In figure: 1-cold-trap, 2. cold-trap gas outlets, 3-cold-traps arrange light mouth and the outlet of nitrogen purging, and 4-cold-traps take off weight mouth,
5-adsorption towers, 6-adsorption tower air inlets, 7-adsorbents, 8-adsorption tower gas outlets, 9-adsorption tower sample taps and nitrogen purging
Import, 10-rectifying columns, 11-tower bottom of rectifying tower air inlets, 12-tower reactors, 13-rectifying columns, 14-fillers, 15-tower tops are cold
Condenser, the outlet of 16-rectifying columns, 17-tower top sample taps, 18 --- cold-trap feed inlet, 19-tower bottom of rectifying tower outlets, 20-
Valve V-1,21-valve V-2,22-valve V-3,23-valve V-4,24-valve V-5,25-valve V-6,26-valves
V-7,27-valve V-8,28-flowmeter F-1,29-flowmeter F-2,30-thermometer T-1,31-thermometer T-2,32-
Thermometer T-3,33-thermometer T-4,34-pressure gauge P-1,35-pressure gauge P-2,36-pressure gauge P-3,37-pressure gauges
P-4。
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
In following embodiment:
The gas composition ingredient and content be discharged to tower top sample tap 17 is detected with gas chromatograph, chromatography: Shimadzu
GC-14C；Carrier gas: nitrogen；Detector: hydrogen flame ionization detector (FID)；Sample volume: 0.2mL.
The organic carbon fluorine refers to the impurity containing carbon (C) atom and fluorine (F) atom.
As shown in Figure 1, a kind of purification devices of octafluoropropane, the purification devices are suitable for a kind of octafluoro of the present invention
The purification process of propane uses；The purification devices specifically include that cold-trap 1, adsorption tower 5 and rectifying column 10.
Wherein, 1 top of cold-trap is equipped with cold-trap gas outlet 2, is equipped with cold-trap feed inlet 18 in the middle part of cold-trap 1,1 bottom of cold-trap is equipped with
Cold-trap takes off weight mouth 4, and 1 lower part of cold-trap is equipped with temperature control equipment, pressure gauge P-1 34 and thermometer T-1 30.
5 bottom of adsorption tower is equipped with adsorption tower air inlet 6, is placed with adsorbent 7 in the middle part of adsorption tower 5, is equipped at the top of adsorption tower 5
Adsorption tower gas outlet 8,5 top of adsorption tower are equipped with pressure gauge P-2 35, are equipped with thermometer T-2 31 in the middle part of adsorption tower 5.
Rectifying column 10 is mainly made of tower reactor 12, rectifying column 13 and overhead condenser 15；Wherein, 12 top of tower reactor is equipped with essence
Tower tower reactor air inlet 11 is evaporated, is equipped with temperature control equipment, pressure gauge P-336 and thermometer T-3 32, tower reactor 12 in the middle part of tower reactor 12
Bottom is equipped with tower bottom of rectifying tower outlet 19, is equipped with pressure gauge P-4 37 and thermometer T-4 33 in the middle part of overhead condenser 15.
Cold-trap takes off weight mouth 4 and is connected with the pipeline for being equipped with valve V-3 22, and line end is outlet, cold-trap gas outlet 2
Connect by pipeline with adsorption tower air inlet 6, on this pipeline, the rear of cold-trap gas outlet 2 be successively arranged cold-trap arrange light mouth and
Nitrogen purging outlet 3, flowmeter F-1 28 and valve V-1 20, cold-trap are arranged and are connected with one at light mouth and nitrogen purging outlet 3
Pipeline equipped with valve V-2 21, line end are outlet；Adsorption tower gas outlet 8 passes through pipeline and tower bottom of rectifying tower air inlet 11
It connects, on this pipeline, the rear of adsorption tower gas outlet 8 is successively arranged adsorption tower sample tap and nitrogen purging import 9, flowmeter
The pipe for being equipped with valve V-5 24 is connected at F-2 29 and valve V-4 23, adsorption tower sample tap and nitrogen purging import 9
Road, line end are outlet；Pipeline is equipped at the top of overhead condenser 15, the pipeline is divided into two branches, and a branch road is set
There is valve V-7 26, end is rectifying column outlet 16, and another branch road is equipped with valve V-8 27, and end is tower top sample tap
17,12 bottom tower bottom of rectifying tower outlet 19 of tower reactor is connected with the pipeline for being equipped with valve V-6 25, and line end is outlet.
Embodiment 1
Rectifying column 10 is stuffing rectification column, and filler 14 is the stainless steel θ ring of diameter 1mm, and the material of rectifying column 10 is nickel, high
15m is spent, the diameter of rectifying column 13 is 50mm.
A kind of purification process of octafluoropropane, steps are as follows for the purification process:
(1) octafluoropropane crude product conductance is entered in -100 DEG C of temperature of cold-trap 1, is heated up with the rate of 1 DEG C/min, -90
DEG C~-40 DEG C carry out arranging light processing, make the vaporization discharge of low-boiling light component impurity, be greater than -40 DEG C when temperature rises to, be less than etc.
When -20 DEG C, will treated octafluoropropane crude product conductance enters 5 bottom of adsorption tower, temperature rises to when being greater than -20 DEG C, stop to
5 bottom of adsorption tower is passed through, and the higher heavy constituent impurity left in cold-trap 1 is discharged, and carries out de- weight sewage treatment；
The octafluoropropane crude product gas purity is 90%.
(2) treated after octafluoropropane crude product gas enters adsorption tower 5, is 0MPa in adsorptive pressure, adsorption temp is -10
It is contacted at DEG C with the adsorbent 7 in adsorption tower 5, time of contact 0.1s, carries out adsorption treatment, the gas after obtaining adsorption treatment；
The adsorbent 7 is the activated carbon fiber that partial size is 0.5mm；The adsorbent 7 is used in combination using preceding in 100 DEG C of heating
The nitrogen purging that flow velocity is 100L/min is activated.
(3) 12 temperature of tower reactor of rectifying column 10 is down to -90 DEG C, the gas after adsorption treatment is passed through in tower reactor 12 and liquefies,
Stop being passed through after liquefaction 50kg, heat tower reactor 12 carries out rectifying, and control 12 temperature of tower reactor is 32 DEG C, pressure 0.94MPa, rectifying
The tower top temperature of tower 10 is 30 DEG C, pressure 0.90MPa, gas infinite reflux between tower reactor 12 and tower top after making adsorption treatment
After 16h, be discharged with the flow of 1kg/h from tower top, the reflux ratio of the infinite reflux is 30, the constituent of detection discharge gas and
Content, the impurity in discharge gas, i.e. O2、N2、CO、CO2、H2The content of O and organic carbon fluorine is less than the impurity content in table 1
When, meet requirement of high-purity octafluoropropane to impurity content, collects the discharge gas and obtain high-purity octafluoropropane；When detecting
When impurity content in the component of the discharge gas is more than or equal to the impurity content in table 1, stop collecting the discharge gas,
And the octafluoropropane that impurity content in tower reactor 12 is unsatisfactory for high-purity octafluoropropane requirement is discharged from 12 bottom of tower reactor；Collection obtains
Octafluoropropane 30kg, yield 60% are detected its purity and have reached 99.999%, and every impurity constituent and content are shown in Table
2。
Table 2
| Dopant species | O2 | N2 | CO | CO2 | H2O | Organic carbon fluorine |
| Content/ppm | 0.3 | 0.5 | 0.1 | 0.1 | 0.3 | 3.8 |
Embodiment 2
Rectifying column 10 is stuffing rectification column, and filler 14 is the nickel Pall ring of diameter 5mm, and the material of rectifying column 10 is stainless
Steel, height 8m, the diameter of rectifying column 13 are 500mm.
A kind of purification process of octafluoropropane, steps are as follows for the purification process:
(1) octafluoropropane crude product conductance is entered in -91 DEG C of temperature of cold-trap 1, is heated up with the rate of 2 DEG C/min, at -90 DEG C
~-40 DEG C carry out arranging light processing, make low-boiling light component impurity vaporization discharge, are greater than -40 DEG C when temperature rises to, be less than etc.
When -20 DEG C, will treated octafluoropropane crude product conductance enters 5 bottom of adsorption tower, temperature rises to when being greater than -20 DEG C, stop to
5 bottom of adsorption tower is passed through, and the higher heavy constituent impurity left in cold-trap 1 is discharged, and carries out de- weight sewage treatment；
The octafluoropropane crude product gas purity is 99.9%.
(2) treated after octafluoropropane crude product gas enters adsorption tower 5, is 0.2MPa in adsorptive pressure, adsorption temp is
It is contacted at 20 DEG C with the adsorbent 7 in adsorption tower 5, time of contact 2s, carries out adsorption treatment, the gas after obtaining adsorption treatment；
The adsorbent 7 is the 3A molecular sieve that partial size is 2mm；The adsorbent 7 is heated in 300 DEG C using preceding and is used flow velocity
It is activated for the helium purge of 1L/min.
(3) 12 temperature of tower reactor of rectifying column 10 is down to -80 DEG C, the gas after adsorption treatment is passed through in tower reactor 12 and liquefies,
Stop being passed through after liquefaction 500kg, heat tower reactor 12 carries out rectifying, and control 12 temperature of tower reactor is -28 DEG C, pressure 0.05MPa, essence
The tower top temperature for evaporating tower 10 is -30 DEG C, pressure 0.04MPa, and the gas after making adsorption treatment is complete between tower reactor 12 and tower top
It flows back after 8h, is discharged with the flow of 0.1kg/h from tower top, the reflux ratio of the infinite reflux is 500, the composition of detection discharge gas
Ingredient and content, the impurity in discharge gas, i.e. O2、N2、CO、CO2、H2The content of O and organic carbon fluorine is less than miscellaneous in table 1
When matter content, meet requirement of high-purity octafluoropropane to impurity content, collects the discharge gas and obtain high-purity octafluoropropane；When
When detecting that the impurity content in the component of the discharge gas is more than or equal to the impurity content in table 1, stop collecting the row
Gas out, and the octafluoropropane that impurity content in tower reactor 12 is unsatisfactory for high-purity octafluoropropane requirement is discharged from 12 bottom of tower reactor；
Collection obtains octafluoropropane 480kg, and yield 96% is detected its purity and has reached 99.999%, every impurity constituent
And content is shown in Table 3.
Table 3
| Dopant species | O2 | N2 | CO | CO2 | H2O | Organic carbon fluorine |
| Content/ppm | 0.5 | 0.8 | 0.2 | 0.2 | 0.5 | 0.3 |
Embodiment 3
Rectifying column 10 is stuffing rectification column, and filler 14 is the polytetrafluoroethylene (PTFE) Pall ring of diameter 100mm, the material of rectifying column 10
Matter is monel metal, and height 5m, the diameter of rectifying column 13 is 300mm.
A kind of purification process of octafluoropropane, steps are as follows for the purification process:
(1) octafluoropropane crude product conductance is entered in -100 DEG C of temperature of cold-trap 1, is heated up with the rate of 1.5 DEG C/min, -
90 DEG C~-40 DEG C carry out arranging light processing, make low-boiling light component impurity vaporization discharge, are greater than -40 DEG C when temperature rises to, are less than
When equal to -20 DEG C, by treated, octafluoropropane crude product conductance enters 5 bottom of adsorption tower, when temperature is risen to greater than -20 DEG C, stops
It is passed through to 5 bottom of adsorption tower, the higher heavy constituent impurity left in cold-trap 1 is discharged, carry out de- weight sewage treatment；
The octafluoropropane crude product gas purity is 99.99%.
(2) treated after octafluoropropane crude product gas enters adsorption tower 5, is 0.5MPa in adsorptive pressure, adsorption temp is
It is contacted at 40 DEG C with the adsorbent 7 in adsorption tower 5, time of contact 5s, carries out adsorption treatment, the gas after obtaining adsorption treatment；
The adsorbent 7 is the carbon molecular sieve that partial size is 5mm；The adsorbent 7 is heated in 250 DEG C using preceding and is used flow velocity
It is activated for the nitrogen purging of 10L/min.
(3) 12 temperature of tower reactor of rectifying column 10 is down to -60 DEG C, the gas after adsorption treatment is passed through in tower reactor 12 and liquefies,
Stop being passed through after liquefaction 300kg, heat tower reactor 12 carries out rectifying, and control 12 temperature of tower reactor is -8 DEG C, pressure 0.22MPa, essence
The tower top temperature for evaporating tower 10 is -10 DEG C, pressure 0.20MPa, and the gas after making adsorption treatment is complete between tower reactor 12 and tower top
Flow back after 2h, be discharged with the flow of 10kg/h from tower top, the reflux ratio of the infinite reflux is 5, the composition of detection discharge gas at
Point and content, when discharge gas in impurity, i.e. O2、N2、CO、CO2、H2The content of O and organic carbon fluorine is less than the impurity in table 1
When content, meet requirement of high-purity octafluoropropane to impurity content, collects the discharge gas and obtain high-purity octafluoropropane；Work as inspection
When measuring the impurity content in the component of the discharge gas and being more than or equal to the impurity content in table 1, stop collecting the discharge
Gas, and the octafluoropropane that impurity content in tower reactor 12 is unsatisfactory for high-purity octafluoropropane requirement is discharged from 12 bottom of tower reactor；It receives
Collection obtains octafluoropropane 280kg, yield 93%, is detected its purity and has reached 99.999%, every impurity constituent and
Content is shown in Table 4.
Table 4
| Dopant species | O2 | N2 | CO | CO2 | H2O | Organic carbon fluorine |
| Content/ppm | 0.4 | 0.6 | 0.1 | 0.2 | 0.8 | 0.1 |
Embodiment 4
Rectifying column 10 is stuffing rectification column, and filler 14 is the polytetrafluoroethylene (PTFE) Pall ring of diameter 50mm, the material of rectifying column 10
Matter is stainless steel, and height 3m, the diameter of rectifying column 13 is 200mm.
A kind of purification process of octafluoropropane, steps are as follows for the purification process:
(1) octafluoropropane crude product conductance is entered in -100 DEG C of temperature of cold-trap 1, is heated up with the rate of 1.5 DEG C/min, -
90 DEG C~-40 DEG C carry out arranging light processing, make low-boiling light component impurity vaporization discharge, are greater than -40 DEG C when temperature rises to, are less than
When equal to -20 DEG C, by treated, octafluoropropane crude product conductance enters 5 bottom of adsorption tower, when temperature is risen to greater than -20 DEG C, stops
It is passed through to 5 bottom of adsorption tower, the higher heavy constituent impurity left in cold-trap 1 is discharged, carry out de- weight sewage treatment；
The octafluoropropane crude product gas purity is 99.99%.
(2) treated after octafluoropropane crude product gas enters adsorption tower 5, is 0.2MPa in adsorptive pressure, adsorption temp is
It is contacted at 20 DEG C with the adsorbent 7 in adsorption tower 5, time of contact 2s, carries out adsorption treatment, the gas after obtaining adsorption treatment；
The adsorbent 7 is the carbon molecular sieve that partial size is 2mm；The adsorbent 7 is heated in 200 DEG C using preceding and is used flow velocity
It is activated for the nitrogen purging of 10L/min.
(3) 12 temperature of tower reactor of rectifying column 10 is down to -80 DEG C, the gas after adsorption treatment is passed through in tower reactor 12 and liquefies,
Stop being passed through after liquefaction 300kg, heat tower reactor 12 carries out rectifying, and control 12 temperature of tower reactor is -8 DEG C, pressure 0.22MPa, essence
The tower top temperature for evaporating tower 10 is -10 DEG C, pressure 0.20MPa, and the gas after making adsorption treatment is complete between tower reactor 12 and tower top
Flow back after 8h, be discharged with the flow of 1kg/h from tower top, the reflux ratio of the infinite reflux is 20, the composition of detection discharge gas at
Point and content, when discharge gas in impurity, i.e. O2、N2、CO、CO2、H2The content of O and organic carbon fluorine is less than the impurity in table 1
When content, meet requirement of high-purity octafluoropropane to impurity content, collects the discharge gas and obtain high-purity octafluoropropane；Work as inspection
When measuring the impurity content in the component of the discharge gas and being more than or equal to the impurity content in table 1, stop collecting the discharge
Gas, and the octafluoropropane that impurity content in tower reactor 12 is unsatisfactory for high-purity octafluoropropane requirement is discharged from 12 bottom of tower reactor；It receives
Collection obtains octafluoropropane 285kg, yield 95%, is detected its purity and has reached 99.999%, every impurity constituent and
Content is shown in Table 5.
Table 5
| Dopant species | O2 | N2 | CO | CO2 | H2O | Organic carbon fluorine |
| Content/ppm | 0.4 | 0.7 | 0.1 | 0.3 | 0.7 | 0.2 |
Embodiment 5
Rectifying column 10 is stuffing rectification column, and filler 14 is the monel metal Raschig ring of diameter 10mm, the material of rectifying column 10
Matter is stainless steel, and height 0.5m, the diameter of rectifying column 13 is 100mm.
A kind of purification process of octafluoropropane, steps are as follows for the purification process:
(1) octafluoropropane crude product conductance is entered in -100 DEG C of temperature of cold-trap 1, is heated up with the rate of 1.5 DEG C/min, -
90 DEG C~-40 DEG C carry out arranging light processing, make low-boiling light component impurity vaporization discharge, are greater than -40 DEG C when temperature rises to, are less than
When equal to -20 DEG C, by treated, octafluoropropane crude product conductance enters 5 bottom of adsorption tower, when temperature is risen to greater than -20 DEG C, stops
It is passed through to 5 bottom of adsorption tower, the higher heavy constituent impurity left in cold-trap 1 is discharged, carry out de- weight sewage treatment；
The octafluoropropane crude product gas purity is 99.9%.
(2) treated after octafluoropropane crude product gas enters adsorption tower 5, is 0.2MPa in adsorptive pressure, adsorption temp is
It is contacted at 20 DEG C with the adsorbent 7 in adsorption tower 5, time of contact 2s, carries out adsorption treatment, the gas after obtaining adsorption treatment；
The adsorbent 7 is the carbon molecular sieve that partial size is 2mm；The adsorbent 7 is heated in 200 DEG C using preceding and is used flow velocity
It is activated for the nitrogen purging of 10L/min.
(3) 12 temperature of tower reactor of rectifying column 10 is down to -80 DEG C, the gas after adsorption treatment is passed through in tower reactor 12 and liquefies,
Stop being passed through after liquefaction 300kg, heat tower reactor 12 carries out rectifying, and control 12 temperature of tower reactor is -8 DEG C, pressure 0.22MPa, essence
The tower top temperature for evaporating tower 10 is -10 DEG C, pressure 0.20MPa, and the gas after making adsorption treatment is complete between tower reactor 12 and tower top
Flow back after 8h, be discharged with the flow of 1kg/h from tower top, the reflux ratio of the infinite reflux is 25, the composition of detection discharge gas at
Point and content, when discharge gas in impurity, i.e. O2、N2、CO、CO2、H2The content of O and organic carbon fluorine is less than the impurity in table 1
When content, meet requirement of high-purity octafluoropropane to impurity content, collects the discharge gas and obtain high-purity octafluoropropane；Work as inspection
When measuring the impurity content in the component of the discharge gas and being more than or equal to the impurity content in table 1, stop collecting the discharge
Gas, and the octafluoropropane that impurity content in tower reactor 12 is unsatisfactory for high-purity octafluoropropane requirement is discharged from 12 bottom of tower reactor；It receives
Collection obtains octafluoropropane 265kg, yield 88%, is detected its purity and has reached 99.999%, every impurity constituent and
Content is shown in Table 6.
Table 6
| Dopant species | O2 | N2 | CO | CO2 | H2O | Organic carbon fluorine |
| Content/ppm | 0.3 | 0.7 | 0.2 | 0.4 | 0.9 | 1.2 |
Embodiment 6
Rectifying column 10 is plate distillation column, and the number of plates 80, the material of rectifying column 10 is stainless steel, height 5m, rectifying column
13 diameter is 200mm.
A kind of purification process of octafluoropropane, steps are as follows for the purification process:
(1) octafluoropropane crude product conductance is entered in -100 DEG C of temperature of cold-trap 1, is heated up with 1.5 DEG C of rate, at -90 DEG C
~-40 DEG C carry out arranging light processing, make low-boiling light component impurity vaporization discharge, are greater than -40 DEG C when temperature rises to, be less than etc.
When -20 DEG C, will treated octafluoropropane crude product conductance enters 5 bottom of adsorption tower, temperature rises to when being greater than -20 DEG C, stop to
5 bottom of adsorption tower is passed through, and the higher heavy constituent impurity left in cold-trap 1 is discharged, and carries out de- weight sewage treatment；
The octafluoropropane crude product gas purity is 99.9%.
(2) treated after octafluoropropane crude product gas enters adsorption tower 5, is 0.2MPa in adsorptive pressure, adsorption temp is
It is contacted at 20 DEG C with the adsorbent 7 in adsorption tower 5, time of contact 2s, carries out adsorption treatment, the gas after obtaining adsorption treatment；
The adsorbent 7 is the carbon molecular sieve that partial size is 2mm；The adsorbent 7 is heated in 200 DEG C using preceding and is used flow velocity
It is activated for the nitrogen purging of 10L/min.
(3) 12 temperature of tower reactor of rectifying column 10 is down to -80 DEG C, the gas after adsorption treatment is passed through in tower reactor 12 and liquefies,
Stop being passed through after liquefaction 300kg, heat tower reactor 12 carries out rectifying, and control 12 temperature of tower reactor is -8 DEG C, pressure 0.22MPa, essence
The tower top temperature for evaporating tower 10 is -10 DEG C, pressure 0.20MPa, and the gas after making adsorption treatment is complete between tower reactor 12 and tower top
Flow back after 8h, be discharged with the flow of 1kg/h from tower top, the reflux ratio of the infinite reflux is 25, the composition of detection discharge gas at
Point and content, when discharge gas in impurity, i.e. O2、N2、CO、CO2、H2The content of O and organic carbon fluorine is less than the impurity in table 1
When content, meet requirement of high-purity octafluoropropane to impurity content, collects the discharge gas and obtain high-purity octafluoropropane；Work as inspection
When measuring the impurity content in the component of the discharge gas and being more than or equal to the impurity content in table 1, stop collecting the discharge
Gas, and the octafluoropropane that impurity content in tower reactor 12 is unsatisfactory for high-purity octafluoropropane requirement is discharged from 12 bottom of tower reactor；It receives
Collection obtains octafluoropropane 286kg, yield 95%, is detected its purity and has reached 99.999%, every impurity constituent and
Content is shown in Table 7.
Table 7
| Dopant species | O2 | N2 | CO | CO2 | H2O | Organic carbon fluorine |
| Content/ppm | 0.2 | 0.5 | 0.1 | 0.2 | 0.4 | 0.8 |
Embodiment 7
Rectifying column 10 is plate distillation column, the number of plates 20, and the material of rectifying column 10 is nickel, height 5m, rectifying column 13
Diameter is 200mm.
A kind of purification process of octafluoropropane, steps are as follows for the purification process:
(1) octafluoropropane crude product conductance is entered in -100 DEG C of temperature of cold-trap 1, is heated up with the rate of 1.5 DEG C/min, -
90 DEG C~-40 DEG C carry out arranging light processing, make low-boiling light component impurity vaporization discharge, are greater than -40 DEG C when temperature rises to, are less than
When equal to -20 DEG C, by treated, octafluoropropane crude product conductance enters 5 bottom of adsorption tower, when temperature is risen to greater than -20 DEG C, stops
It is passed through to 5 bottom of adsorption tower, the higher heavy constituent impurity left in cold-trap 1 is discharged, carry out de- weight sewage treatment；
The octafluoropropane crude product gas purity is 99.9%.
(2) treated after octafluoropropane crude product gas enters adsorption tower 5, is 0.2MPa in adsorptive pressure, adsorption temp is
It is contacted at 20 DEG C with the adsorbent 7 in adsorption tower 5, time of contact 2s, carries out adsorption treatment, the gas after obtaining adsorption treatment；
The adsorbent 7 is the carbon molecular sieve that partial size is 2mm；The adsorbent 7 is heated in 200 DEG C using preceding and is used flow velocity
It is activated for the nitrogen purging of 10L/min.
(3) 12 temperature of tower reactor of rectifying column 10 is down to -80 DEG C, the gas after adsorption treatment is passed through in tower reactor 12 and liquefies,
Stop being passed through after liquefaction 300kg, heat tower reactor 12 carries out rectifying, and control 12 temperature of tower reactor is -8 DEG C, pressure 0.22MPa, essence
The tower top temperature for evaporating tower 10 is -10 DEG C, pressure 0.20MPa, and the gas after making adsorption treatment is complete between tower reactor 12 and tower top
It flows back after 8h, is discharged with the flow of 0.1kg/h from tower top, the reflux ratio of the infinite reflux is 100, the composition of detection discharge gas
Ingredient and content, the impurity in discharge gas, i.e. O2、N2、CO、CO2、H2The content of O and organic carbon fluorine is less than miscellaneous in table 1
When matter content, meet requirement of high-purity octafluoropropane to impurity content, collects the discharge gas and obtain high-purity octafluoropropane；When
When detecting that the impurity content in the component of the discharge gas is more than or equal to the impurity content in table 1, stop collecting the row
Gas out, and the octafluoropropane that impurity content in tower reactor 12 is unsatisfactory for high-purity octafluoropropane requirement is discharged from 12 bottom of tower reactor；
Collection obtains octafluoropropane 277kg, and yield 92% is detected its purity and has reached 99.999%, every impurity constituent
And content is shown in Table 8.
Table 8
| Dopant species | O2 | N2 | CO | CO2 | H2O | Organic carbon fluorine |
| Content/ppm | 0.3 | 0.6 | 0.1 | 0.3 | 0.6 | 2.4 |
Embodiment 8
Rectifying column 10 is plate distillation column, and the number of plates 30, the material of rectifying column 10 is monel metal, height 5m, essence
The diameter of fractional distillation column 13 is 200mm.
A kind of purification process of octafluoropropane, steps are as follows for the purification process:
(1) octafluoropropane crude product conductance is entered in -100 DEG C of temperature of cold-trap 1, is heated up with the rate of 1.5 DEG C/min, -
90 DEG C~-40 DEG C carry out arranging light processing, make low-boiling light component impurity vaporization discharge, are greater than -40 DEG C when temperature rises to, are less than
When equal to -20 DEG C, by treated, octafluoropropane crude product conductance enters 5 bottom of adsorption tower, when temperature is risen to greater than -20 DEG C, stops
It is passed through to 5 bottom of adsorption tower, the higher heavy constituent impurity left in cold-trap 1 is discharged, carry out de- weight sewage treatment；
The octafluoropropane crude product gas purity is 99.9%.
(2) treated after octafluoropropane crude product gas enters adsorption tower 5, is 0.2MPa in adsorptive pressure, adsorption temp is
It is contacted at 20 DEG C with the adsorbent 7 in adsorption tower 5, time of contact 2s, carries out adsorption treatment, the gas after obtaining adsorption treatment；
The adsorbent 7 is the carbon molecular sieve that partial size is 2mm；The adsorbent 7 is heated in 200 DEG C using preceding and is used flow velocity
It is activated for the nitrogen purging of 10L/min.
(3) 12 temperature of tower reactor of rectifying column 10 is down to -80 DEG C, the gas after adsorption treatment is passed through in tower reactor 12 and liquefies,
Stop being passed through after liquefaction 300kg, heat tower reactor 12 carries out rectifying, and control 12 temperature of tower reactor is -8 DEG C, pressure 0.22MPa, essence
The tower top temperature for evaporating tower 10 is -10 DEG C, pressure 0.20MPa, and the gas after making adsorption treatment is complete between tower reactor 12 and tower top
Flow back after 8h, be discharged with the flow of 1kg/h from tower top, the reflux ratio of the infinite reflux is 25, the composition of detection discharge gas at
Point and content, when discharge gas in impurity, i.e. O2、N2、CO、CO2、H2The content of O and organic carbon fluorine is less than the impurity in table 1
When content, meet requirement of high-purity octafluoropropane to impurity content, collects the discharge gas and obtain high-purity octafluoropropane；Work as inspection
When measuring the impurity content in the component of the discharge gas and being more than or equal to the impurity content in table 1, stop collecting the discharge
Gas, and the octafluoropropane that impurity content in tower reactor 12 is unsatisfactory for high-purity octafluoropropane requirement is discharged from 12 bottom of tower reactor；It receives
Collection obtains octafluoropropane 266kg, yield 87%, is detected its purity and has reached 99.999%, every impurity constituent and
Content is shown in Table 9.
Table 9
| Dopant species | O2 | N2 | CO | CO2 | H2O | Organic carbon fluorine |
| Content/ppm | 0.4 | 0.8 | 0.2 | 0.3 | 0.8 | 2.8 |
Embodiment 9
Rectifying column 10 is plate distillation column, and the number of plates 50, the material of rectifying column 10 is stainless steel, height 5m, rectifying column
13 diameter is 200mm.
A kind of purification process of octafluoropropane, steps are as follows for the purification process:
(1) octafluoropropane crude product conductance is entered in -100 DEG C of temperature of cold-trap 1, is heated up with the rate of 1.5 DEG C/min, -
90 DEG C~-40 DEG C carry out arranging light processing, make low-boiling light component impurity vaporization discharge, are greater than -40 DEG C when temperature rises to, are less than
When equal to -20 DEG C, by treated, octafluoropropane crude product conductance enters 5 bottom of adsorption tower, when temperature is risen to greater than -20 DEG C, stops
It is passed through to 5 bottom of adsorption tower, the higher heavy constituent impurity left in cold-trap 1 is discharged, carry out de- weight sewage treatment；
The octafluoropropane crude product gas purity is 99.9%.
(2) treated after octafluoropropane crude product gas enters adsorption tower 5, is 0.2MPa in adsorptive pressure, adsorption temp is
It is contacted at 20 DEG C with the adsorbent 7 in adsorption tower 5, time of contact 2s, carries out adsorption treatment, the gas after obtaining adsorption treatment；
The adsorbent 7 is the carbon molecular sieve that partial size is 2mm；The adsorbent 7 is heated in 200 DEG C using preceding and is used flow velocity
It is activated for the nitrogen purging of 10L/min.
(3) 12 temperature of tower reactor of rectifying column 10 is down to -80 DEG C, the gas after adsorption treatment is passed through in tower reactor 12 and liquefies,
Stop being passed through after liquefaction 300kg, heat tower reactor 12 carries out rectifying, and control 12 temperature of tower reactor is -8 DEG C, pressure 0.22MPa, essence
The tower top temperature for evaporating tower 10 is -10 DEG C, pressure 0.20MPa, and the gas after making adsorption treatment is complete between tower reactor 12 and tower top
Flow back after 8h, be discharged with the flow of 1kg/h from tower top, the reflux ratio of the infinite reflux is 25, the composition of detection discharge gas at
Point and content, when discharge gas in impurity, i.e. O2、N2、CO、CO2、H2The content of O and organic carbon fluorine is less than the impurity in table 1
When content, meet requirement of high-purity octafluoropropane to impurity content, collects the discharge gas and obtain high-purity octafluoropropane；Work as inspection
When measuring the impurity content in the component of the discharge gas and being more than or equal to the impurity content in table 1, stop collecting the discharge
Gas, and the octafluoropropane that impurity content in tower reactor 12 is unsatisfactory for high-purity octafluoropropane requirement is discharged from 12 bottom of tower reactor；It receives
Collection obtains octafluoropropane 283kg, yield 94%, is detected its purity and has reached 99.999%, every impurity constituent and
Content is shown in Table 10.
Table 10
| Dopant species | O2 | N2 | CO | CO2 | H2O | Organic carbon fluorine |
| Content/ppm | 0.1 | 0.2 | 0.1 | 0.1 | 0.3 | 0.8 |
Embodiment 10
Rectifying column 10 is plate distillation column, and the number of plates 40, the material of rectifying column 10 is stainless steel, height 5m, rectifying column
13 diameter is 200mm.
A kind of purification process of octafluoropropane, steps are as follows for the purification process:
(1) octafluoropropane crude product conductance is entered in -100 DEG C of temperature of cold-trap 1, is heated up with the rate of 1.5 DEG C/min, -
90 DEG C~-40 DEG C carry out arranging light processing, make low-boiling light component impurity vaporization discharge, are greater than -40 DEG C when temperature rises to, are less than
When equal to -20 DEG C, by treated, octafluoropropane crude product conductance enters 5 bottom of adsorption tower, when temperature is risen to greater than -20 DEG C, stops
It is passed through to 5 bottom of adsorption tower, the higher heavy constituent impurity left in cold-trap 1 is discharged, carry out de- weight sewage treatment；
The octafluoropropane crude product gas purity is 99.9%.
(2) treated after octafluoropropane crude product gas enters adsorption tower 5, is 0.2MPa in adsorptive pressure, adsorption temp is
It is contacted at 20 DEG C with the adsorbent 7 in adsorption tower 5, time of contact 2s, carries out adsorption treatment, the gas after obtaining adsorption treatment；
The adsorbent 7 is the carbon molecular sieve that partial size is 2mm；The adsorbent 7 is heated in 200 DEG C using preceding and is used flow velocity
It is activated for the nitrogen purging of 10L/min.
(3) 12 temperature of tower reactor of rectifying column 10 is down to -80 DEG C, the gas after adsorption treatment is passed through in tower reactor 12 and liquefies,
Stop being passed through after liquefaction 300kg, heat tower reactor 12 carries out rectifying, and control 12 temperature of tower reactor is -8 DEG C, pressure 0.22MPa, essence
The tower top temperature for evaporating tower 10 is -10 DEG C, pressure 0.20MPa, and the gas after making adsorption treatment is complete between tower reactor 12 and tower top
Flow back after 8h, be discharged with the flow of 1kg/h from tower top, the reflux ratio of the infinite reflux is 25, the composition of detection discharge gas at
Point and content, when discharge gas in impurity, i.e. O2、N2、CO、CO2、H2The content of O and organic carbon fluorine is less than the impurity in table 1
When content, meet requirement of high-purity octafluoropropane to impurity content, collects the discharge gas and obtain high-purity octafluoropropane；Work as inspection
When measuring the impurity content in the component of the discharge gas and being more than or equal to the impurity content in table 1, stop collecting the discharge
Gas, and the octafluoropropane that impurity content in tower reactor 12 is unsatisfactory for high-purity octafluoropropane requirement is discharged from 12 bottom of tower reactor；It receives
Collect obtained octafluoropropane 278kg, yield 93% is detected its purity and has reached 99.999%, every impurity constituent
And content is shown in Table 11.
Table 11
| Dopant species | O2 | N2 | CO | CO2 | H2O | Organic carbon fluorine |
| Content/ppm | 0.2 | 0.4 | 0.1 | 0.2 | 0.4 | 1.3 |
Claims (9)
1. a kind of purification process of octafluoropropane, it is characterised in that: steps are as follows for the purification process:
(1) octafluoropropane crude product conductance is entered in cold-trap (1) of the temperature less than -90 DEG C, with 1 DEG C/min~2 DEG C/min rate
Heating, carries out arranging light processing at -90 DEG C~-40 DEG C, is greater than -40 DEG C when temperature rises to, when being less than or equal to -20 DEG C, after processing
Octafluoropropane crude product conductance enter adsorption tower (5) bottom, temperature, which rises to, is greater than -20 DEG C, stop being passed through to adsorption tower (5) bottom,
The higher heavy constituent impurity left in cold-trap (1) is discharged；
The purity of the octafluoropropane crude product gas is 90%~99.99%；
(2) treated after octafluoropropane crude product gas enters adsorption tower (5), is 0MPa~0.5MPa, absorption temperature in adsorptive pressure
Degree is to contact with the adsorbent (7) in adsorption tower (5), time of contact 0.1s~5s obtains adsorption treatment at -10 DEG C~40 DEG C
Gas afterwards；
The adsorbent (7) is one or more of active carbon, molecular sieve and carbon molecular sieve, and partial size is 0.5mm~5mm, described
Adsorbent (7) using it is preceding in 100 DEG C~300 DEG C heating and with flow velocity be 1L/min~100L/min inert gas or nitrogen blow
Sweep into capable activation；
(3) tower reactor (12) temperature of rectifying column (10) is down to -90 DEG C~-60 DEG C, the gas after adsorption treatment is passed through tower reactor
(12) in liquefaction, liquefy 50kg~500kg after stops being passed through, heat tower reactor (12) carry out rectifying, control tower reactor (12) temperature for-
28 DEG C~32 DEG C, pressure is 0.05MPa~0.94MPa, and the tower top temperature of rectifying column (10) is -30 DEG C~30 DEG C, and pressure is
0.04MPa~0.90MPa, the gas after making adsorption treatment between tower reactor (12) and tower top after infinite reflux 2h~16h, with
The flow of 0.1kg/h~10kg/h is discharged from tower top, the constituent and content of detection discharge gas, needed for each component satisfaction
When index, collects the discharge gas and obtain high-purity octafluoropropane；When the impurity in the component for detecting the discharge gas contains
When amount is more than or equal to required index, stop collecting the discharge gas, and impurity content in tower reactor (12) is unsatisfactory for high-purity eight
The octafluoropropane that fluoro-propane requires is discharged from tower reactor (12) bottom；
The reflux ratio of the infinite reflux is 5~500；
Rectifying column (10) is made of tower reactor (12), rectifying column (13) and overhead condenser (15), is stuffing rectification column or board-like essence
Tower is evaporated,
When the rectifying column (10) are stuffing rectification column, filler (14) is Pall ring, θ ring or Raschig ring；The material of filler (14)
Matter is polytetrafluoroethylene (PTFE), stainless steel, nickel or monel metal；The diameter of filler (14) is 1mm~100mm；
When the rectifying column (10) are plate distillation column, the number of plates is 20~80；
The material of the rectifying column (10) is stainless steel, nickel or monel metal；
The height of the rectifying column (10) is 0.5m~15m；
The diameter of the rectifying column (13) is 50mm~500mm.
2. a kind of purification process of octafluoropropane according to claim 1, it is characterised in that: the octafluoropropane crude product gas
It is prepared using hexafluoropropene or the reaction of heptafluoro-propane and fluorine gas；Impurity in discharge gas, i.e. O2、N2、CO、CO2、H2O
When being less than the impurity content in table 1 with the content of organic carbon fluorine, meet requirement of high-purity octafluoropropane to impurity content, collects institute
It states discharge gas and obtains high-purity octafluoropropane；When the impurity content in the component for detecting the discharge gas is more than or equal to table 1
In impurity content when, stop collecting the discharge gas, and impurity content in tower reactor (12) is unsatisfactory for high-purity octafluoropropane
It is required that octafluoropropane from tower reactor (12) bottom be discharged；
Table 1
Wherein, organic carbon fluorine refers to the impurity containing carbon atom and fluorine atom.
3. a kind of purification process of octafluoropropane according to claim 1, it is characterised in that: the adsorbent (7) is to live
Property charcoal, molecular sieve or carbon molecular sieve.
4. a kind of purification process of octafluoropropane according to claim 1, it is characterised in that: rectifying column (10) is filler essence
Evaporate tower；The material of filler (14) is stainless steel；The diameter of filler (14) is 5mm~50mm.
5. a kind of purification process of octafluoropropane according to claim 1, it is characterised in that: the rectifying column (10) is plate
Formula rectifying column, the number of plates are 30~50.
6. a kind of purification process of octafluoropropane according to claim 1, it is characterised in that: the material of the rectifying column (10)
Matter is stainless steel, is highly 3m~8m；The diameter of the rectifying column (13) is 100mm~300mm.
7. a kind of purification process of octafluoropropane according to claim 1, it is characterised in that: the reflux ratio of the infinite reflux
It is 20~30.
8. a kind of purification process of octafluoropropane according to claim 1, it is characterised in that: the octafluoropropane crude product gas
It is prepared using hexafluoropropene or the reaction of heptafluoro-propane and fluorine gas；Impurity in discharge gas, i.e. O2、N2、CO、CO2、H2O
When being less than the impurity content in table 1 with the content of organic carbon fluorine, meet requirement of high-purity octafluoropropane to impurity content, collects institute
It states discharge gas and obtains high-purity octafluoropropane；When the impurity content in the component for detecting the discharge gas is more than or equal to table 1
In impurity content when, stop collecting the discharge gas, and impurity content in tower reactor (12) is unsatisfactory for high-purity octafluoropropane
It is required that octafluoropropane from tower reactor (12) bottom be discharged；
Table 1
Organic carbon fluorine refers to the impurity containing carbon atom and fluorine atom；
The adsorbent (7) is active carbon, molecular sieve or carbon molecular sieve；
When the rectifying column (10) is stuffing rectification column, the material of filler (14) is stainless steel；The diameter of filler (14) be 5mm~
50mm；
When the rectifying column (10) is plate distillation column, the number of plates is 30~50；
The material of the rectifying column (10) is stainless steel, is highly 3m~8m；The diameter of the rectifying column (13) be 100mm~
300mm；
The reflux ratio of infinite reflux is 5~500.
9. a kind of purification devices of octafluoropropane, it is characterised in that: the purification devices are suitable for such as any one of claim 1~8
A kind of purification process of octafluoropropane uses；The purification devices specifically include that cold-trap (1), adsorption tower (5) and rectifying
Tower (10)；
Cold-trap (1) top is equipped with cold-trap gas outlet (2), and middle part is equipped with cold-trap feed inlet (18), and bottom is equipped with the de- weight mouth of cold-trap
(4), lower part is equipped with temperature control equipment, pressure gauge P-1 (34) and thermometer T-1 (30)；
Adsorption tower (5) bottom is equipped with adsorption tower air inlet (6), is placed with adsorbent (7) in adsorption tower (5), and top is equipped with absorption
Tower gas outlet (8), top are equipped with pressure gauge P-2 (35), and middle part is equipped with thermometer T-2 (31)；
Rectifying column (10) is mainly made of tower reactor (12), rectifying column (13) and overhead condenser (15)；Tower reactor (12) top is equipped with
Tower bottom of rectifying tower air inlet (11), middle part are equipped with temperature control equipment, pressure gauge P-3 (36) and thermometer T-3 (32), and bottom is set
Have tower bottom of rectifying tower outlet (19), pressure gauge P-4 (37) and thermometer T-4 (33) are equipped in the middle part of overhead condenser (15)；
De- weight mouth (4) of cold-trap is connected with the pipeline for being equipped with valve V-3 (22), and line end is outlet, cold-trap gas outlet (2)
It is connect by pipeline with adsorption tower air inlet (6), on this pipeline, it is light that the rear of cold-trap gas outlet (2) is successively arranged cold-trap row
Mouth and nitrogen purging outlet (3), flowmeter F-1 (28) and valve V-1 (20), cold-trap arranges light mouth and nitrogen purges at outlet (3)
It is connected with the pipeline for being equipped with valve V-2 (21), line end is outlet；Adsorption tower gas outlet (8) passes through pipeline and rectifying
Tower tower reactor air inlet (11) connects, and on this pipeline, the rear of adsorption tower gas outlet (8) is successively arranged adsorption tower sample tap and nitrogen
Air-blowing sweeps into mouth (9), flowmeter F-2 (29) and valve V-4 (23), connects at adsorption tower sample tap and nitrogen purging import (9)
There is the pipeline for being equipped with valve V-5 (24), line end is outlet；Pipeline, the pipe are equipped at the top of overhead condenser (15)
Road is divided into two branches, and a branch road is equipped with valve V-7 (26), and end is that rectifying column exports (16), and another branch road is set
Have valve V-8 (27), end is tower top sample tap (17), and tower reactor (12) bottom tower bottom of rectifying tower outlet (19) is connected with one
Pipeline equipped with (25) valve V-6, line end are outlet.
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| CN111018662B (en) * | 2019-12-26 | 2021-07-23 | 福建德尔科技有限公司 | Production method for recovering and purifying electronic-grade hexafluoroethane from industrial waste gas generated in carbon tetrafluoride production |
| CN113354508B (en) * | 2021-08-11 | 2021-10-29 | 苏州金宏气体股份有限公司 | Energy-saving purification device and energy-saving purification process for electronic grade gas |
| CN113877313B (en) * | 2021-10-25 | 2022-06-17 | 上海杰视医疗科技有限公司 | Purification device and purification method for medical perfluoropropane |
| CN114133314B (en) * | 2021-11-02 | 2023-10-27 | 山东东岳化工有限公司 | Purification device and purification process of electronic grade trifluoromethane |
| CN115849401A (en) * | 2022-07-26 | 2023-03-28 | 苏州源展材料科技有限公司 | Preparation method and device of ammonia gas for preparing active metal complex in laboratory |
| CN115925506B (en) * | 2022-11-30 | 2023-06-23 | 福建省巨颖高能新材料有限公司 | Preparation method of octafluoropropane |
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| CN1455764A (en) * | 2001-01-15 | 2003-11-12 | 昭和电工株式会社 | Process for purifying octafluoropropane, process for preparing same and use thereof |
| CN103497086A (en) * | 2013-09-22 | 2014-01-08 | 佛山市华特气体有限公司 | Preparation method of perfluoropropane |
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| CN103497086A (en) * | 2013-09-22 | 2014-01-08 | 佛山市华特气体有限公司 | Preparation method of perfluoropropane |
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