CN109503362A - Hexafluoropropylene dimmer prepares the device of perfluor isobutyl ether - Google Patents
Hexafluoropropylene dimmer prepares the device of perfluor isobutyl ether Download PDFInfo
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- CN109503362A CN109503362A CN201811458143.1A CN201811458143A CN109503362A CN 109503362 A CN109503362 A CN 109503362A CN 201811458143 A CN201811458143 A CN 201811458143A CN 109503362 A CN109503362 A CN 109503362A
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- perfluor isobutyl
- isobutyl ether
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
Abstract
The invention belongs to fluorine chemical fields, and in particular to a kind of hexafluoropropylene dimmer prepares the device of perfluor isobutyl ether, including hexafluoropropane dimer generation unit, perfluor isobutyl acyl fluorides generation unit and perfluor isobutyl ether generation unit；Hexafluoropropane dimer generation unit includes hexafluoropropene storage tank, catalytic reaction tube, condenser and the activating chamber being linked in sequence；Perfluor isobutyl acyl fluorides generation unit includes the pyrolysis furnace and -2 DEG C of cold-traps being linked in sequence with activating chamber；Perfluor isobutyl ether generation unit includes reaction kettle, stratification tower, drying tower, rectifying column and the product storage being linked in sequence；The liquid outlet of -2 DEG C of cold-traps is connect with reaction kettle.The present invention designs the device that a kind of hexafluoropropylene dimmer prepares perfluor isobutyl ether, and using hydrofluoroether is prepared after being cracked to form perfluor isobutyl acyl fluorides after hexafluoropropene monomer polymerization under the effect of the catalyst, device is simple, it is easy to accomplish.
Description
Technical field
The invention belongs to fluorine chemical fields, and in particular to a kind of hexafluoropropylene dimmer prepares the dress of perfluor isobutyl ether
It sets.
Background technique
The technology of preparing of existing Hydrofluoroether compounds mainly includes following several: (1) fluorine gas or metal fluoride are to ether
The fluorination of class compound.(2) electrochemical fluorination of ether compound.(3) fluorine-containing alcohol is in the presence of the hydroxide of alkali metal, with halogen
Hydrofluoroether is obtained for hydrocarbon reaction.(4) addition reaction of fluorine-containing alcohol and Fluorine containing olefine.(5) alkyl of fluorinated acyl fluoride or fluorinated ketone
Change reaction.There is certain deficiency in the above method, generate hydrogen fluoride in method (1) production process, corrosivity is big, sets to reaction
It is standby to require harshness.Method (2) and (3) are since preparation process is at high cost, and product yield is low, in actual production using compared with
It is few.Report that more is that method (4) prepares hydrofluoroether, the hydrofluoroether of production using the addition reaction of fluorine-containing alcohol and Fluorine containing olefine
Product or it is flammable or have penetrating odor, be unsatisfactory for the use demand of the industries such as electronics；And in fluorine-containing alcohol and fluorinated olefins
The double bond by-product production close with target product boiling point is had during reaction preparation hydrofluoroether, therefore increases final production
The purification procedures of product, and all chlorine or bromine toxicity are big in purification process, require operation stringent.Method is usually adopted in (5)
The method of electricity consumption fluorine chemistry prepares fluorinated acyl fluoride, further prepares hydrofluoroether, but electric fluorine chemistry method is in process of production
Not only power consumption is big, low yield, by-product are more, but also needs a large amount of anhydrous hydrogen fluorides in electrolytic process；And electric fluorine chemistry side
Method would generally generate a large amount of isomer rather than certain specific perfluorinated acid fluorides, due to the boiling of these isomers
Point is same or similar, it is virtually impossible to use distillation technology separating-purifying, the hydrofluoroether product thus produced is also mixture, Wu Fatong
It crosses distillation technology and realizes separation.In order to overcome many defects in the prior art, propose few using cracking catalyst hexafluoropropene
The mode of aggressiveness finally synthesizes hydrofluoroether, because a kind of device to generate the product is just particularly important thus.
Summary of the invention
The purpose of the present invention is to provide the devices that a kind of hexafluoropropylene dimmer prepares perfluor isobutyl ether.
The present invention to achieve the above object, using following technical scheme:
A kind of hexafluoropropylene dimmer prepares the device of perfluor isobutyl ether, including hexafluoropropane dimer generation unit,
Perfluor isobutyl acyl fluorides generation unit and perfluor isobutyl ether generation unit；The hexafluoropropane dimer generation unit includes
Hexafluoropropene storage tank, catalytic reaction tube, condenser and the activating chamber of sequential connection；It is filled in the catalytic reaction tube
AgF/C catalyst；The perfluor isobutyl acyl fluorides generation unit include the pyrolysis furnace being linked in sequence with the activating chamber and-
2 DEG C of cold-traps；The perfluor isobutyl ether generation unit includes the reaction kettle being linked in sequence, stratification tower, drying tower, rectifying
Tower and product storage；The liquid outlet of -2 DEG C of cold-traps is connect with the reaction kettle.The hexafluoropropene
The connection of the bottom of storage tank and catalytic reaction tube；
The gas discharge outlet of -2 DEG C of cold-traps is connect with -70 DEG C of cold-traps to recycle perfluor acetylfluoride.
The condenser external is provided with condensation collet；The condensation collet is provided with for condensed water inlet and outlet
Condensation water inlet and condensation-water drain.
The upper end of the condenser is provided with outlet and connect with the catalytic tower to recycle unreacted six
Fluoropropene.
The activating chamber and pyrolysis furnace connect with heater respectively.
The catalytic reaction tube is provided with heating mantle.
The method for preparing perfluor isobutyl ether using the device that the hexafluoropropylene dimmer prepares perfluor isobutyl ether,
Include the following steps:
1) hexafluoropropylene dimmer enters oxidation furnace and oxygen and carries out cracking reaction under conditions of having catalyst；Rectifying obtains
To perfluor isobutyl acyl fluorides；
2) perfluor isobutyl acyl fluorides is reacted with alkylating reagent is made hydrofluoroether；
Step 1) obtains specific steps are as follows: using oxygen and hexafluoropropylene dimmer as raw material, reacts under the effect of the catalyst
It is prepared；Wherein the molar ratio of oxygen and hexafluoropropylene dimmer is 10:1-1:10；The catalytic time be 0.1s extremely
200s；The pressure of reaction is 0-1MPa；Reaction temperature is 150-600 DEG C；The catalyst is loaded catalyst, active constituent
For the mixture of one or more of AgO, Al2O3, CuO, AgF, NaF, KF, RbF, CsF.
Hexafluoropropylene dimmer enters reactor with liquid form in the device, since fluid molecule is compared to gas molecule
With shorter intermolecular distance, therefore more gaseous state hexafluoropropylene dimmers point are had in the slow gasification of liquid charging stock
Son comes into full contact with oxygen, so as to shorten the pyrolysis time of hexafluoropropylene dimmer, significantly improves raw material entirety lysis efficiency.
And the presence of the hexafluoropropylene dimmer more contacted with oxygen can prevent the perfluor isobutyl acyl fluorides being cracked to form and perfluor acetyl
The further cracking of fluorine, to guarantee that gained perfluor isobutyl acyl fluorides has higher degree.
Preferably as one kind, it further include pre-activate step in step 1)；It specifically includes and is passed through hexafluoropropylene dimmer
1-2h is activated in 180-220 DEG C of the reactor filled with pre-activate carrier；The active constituent of the pre-activate carrier is four (five
Fluorophenyl) borate and alkyl fluoride aluminium salt according to mass ratio 1:1-1:5 mixture；Wherein n=1-6；The load of pre-activate carrier
Body is SiO2, Al2O3 or B2O3；Load capacity is 10%-20%.
The alkyl fluoride aluminium salt is Al ((CR1R2R3) n) 3 monomers or mixture；Wherein R1, R2 and R3 be H or
Person F and at least one be F, n=1-6.
(pentafluorophenyl group) borate and alkyl fluoride aluminium salt mixed catalyst have good activation to C=C four in the reaction
Effect is activated the activation energy that can further decrease C=C cracking to hexafluoropropylene dimmer using the mixed catalyst, mentioned
The accuracy of high C=C fracture.And the pyrolysis product of perfluoroolefine is usually present carbonyl fluoride or all phosphinylidynes in the prior art
Fluorine, thus pre-activate step implementation can guarantee hexafluoropropylene dimmer rule be cracked into perfluor isobutyl acyl fluorides and perfluor second
Acyl effectively avoids the generation of perfluor carbonyl fluoride by-product.
The hexafluoropropylene dimmer is obtained under the catalysis of support type ionic fluorides through gas phase reaction by hexafluoropropene；
Reaction temperature is 150-220 DEG C, time of contact 0.1s-30s；The load capacity of support type ionic fluorides is 10%-20%；It carries
Body is activated carbon, aluminum oxide, silica or magnesia；Ionic fluorides are AgF, NaF, KF, RbF or CsF.
The specific steps of step 2) are as follows: be fluorinated the perfluor isobutyl acyl fluorides, alkylating reagent, alkali metal of step 1) preparation
Object, phase transfer catalyst and solvent are added in pressure-resistant reaction kettle；100-400 revs/min of revolving speed warming while stirring is extremely
20-220 DEG C, heat preservation is reacted for 2-48 hours, reacting kettle inner pressure 1atm-20atm；Matter is added in mixed liquor after to reaction
The lye that score is 20-50% is measured, then by liquid stratification, lower liquid is collected, obtains crude product.Crude product is carried out
Rectification and purification to get arrive target product.
The molar ratio of perfluor isobutyl acyl fluorides and alkylating reagent is 1:5-5:1.
Phase transfer catalyst is selected from one of quaternary ammonium salt, quaternary phosphonium salt, crown ether, cryptand or a variety of mixed in step 2)
Close object；The alkylating reagent is dialkyl sulfate, iodo-alkyl, alkyl tosylate or chloroformic acid ester；
The solvent is diethylene glycol dimethyl ether, tetraethyleneglycol dimethyl ether, dimethylformamide, dimethyl sulfoxide, one in acetonitrile
Kind or mixing.
The lye is the water-soluble of potassium hydroxide, sodium hydroxide, potassium carbonate or the sodium carbonate that mass fraction is 20-50%
Liquid.
Compared with prior art, the beneficial effects of the present invention are:
The present invention devises the device that a kind of hexafluoropropylene dimmer prepares perfluor isobutyl ether, utilizes hexafluoropropene monomer
Hydrofluoroether is prepared after being cracked to form perfluor isobutyl acyl fluorides after polymerization under the effect of the catalyst, device is simple and safe, it is easy to accomplish.
The application further includes the preparation method using the device, mild condition, yield height.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of apparatus of the present invention；
Specific embodiment
In order to make those skilled in the art more fully understand technical solution of the present invention, with reference to the accompanying drawing and most
The present invention is described in further detail for good embodiment.
Fig. 1 shows the device that a kind of hexafluoropropylene dimmer prepares perfluor isobutyl ether, including hexafluoropropane dimer is raw
At unit, perfluor isobutyl acyl fluorides generation unit and perfluor isobutyl ether generation unit；The hexafluoropropane dimer generates
Unit includes hexafluoropropene storage tank 1, catalytic reaction tube 2, condenser 3 and the activating chamber 4 being linked in sequence；The catalysis reaction
Catalyst is filled in pipe；The perfluor isobutyl acyl fluorides generation unit includes the pyrolysis furnace being linked in sequence with the activating chamber
5 and -2 DEG C of cold-traps 6；The perfluor isobutyl ether generation unit includes the reaction kettle 7 being linked in sequence, stratification tower 8, does
Dry tower 9 and product storage 10；The liquid outlet of -2 DEG C of cold-traps is connect with the reaction kettle.Described -2 DEG C
The gas discharge outlet of cold-trap is connect with -70 DEG C of cold-traps 11 to recycle perfluor acetylfluoride.The condenser external is provided with cold
Solidifying collet；The condensation collet is provided with condensation water inlet and condensation-water drain for condensed water inlet and outlet.Described
The upper end of condenser is provided with gas vent and connect with the catalytic tower to recycle unreacted hexafluoropropene.It is described
Activating chamber and pyrolysis furnace connect respectively with heater.
Embodiment 1: the preparation of hexafluoropropylene dimmer raw material: by hexafluoropropene gas by being catalyzed equipped with NaF/Al2O3
The catalytic reaction tube of agent, the load capacity of catalyst are 10%, time of contact 0.1s；The temperature of catalytic reaction tube is 150 DEG C, instead
Mixed gas after answering enters the condenser with cooling jacket by port entrance, and condensate temperature is 10 DEG C, and unreacted six
Fluoropropene is recycled to catalytic reaction tube through gas vent.The purity of liquid hexafluoropropylene dimmer in detection condenser receiver
It is 99.3%.The yield of hexafluoropropylene dimmer is shown in Table 1.
Embodiment 2: the preparation of hexafluoropropylene dimmer raw material: by hexafluoropropene gas by being equipped with AgF/C catalyst
Catalytic reaction tube, the load capacity of catalyst are 15%, and the temperature of catalyst filling column is 180 DEG C, time of contact 10s, reaction
Mixed gas afterwards enters the condenser with cooling jacket by air inlet, and condensate temperature is 10 DEG C；Unreacted hexafluoro third
Alkene is recycled to catalytic reaction tube column through outlet.The purity of liquid hexafluoropropylene dimmer is 99.2% in detection condenser.Set
1 is shown in Table with the yield of rear hexafluoropropylene dimmer.
Embodiment 3: hexafluoropropene gas the preparation of hexafluoropropylene dimmer raw material: is passed through into urging equipped with KF/C catalyst
Change reaction tube, the load capacity of catalyst is 20%, and the temperature of catalyst filling column is 220 DEG C, time of contact 30s；After reaction
Mixed gas by air inlet enter with cooling jacket condenser, condensate temperature be 10 DEG C, unreacted hexafluoropropene
Catalytic reaction tube is recycled to through outlet.The purity of liquid hexafluoropropylene dimmer is 99.3% in detection condenser.After applying
The yield of hexafluoropropylene dimmer is shown in Table 1.
Comparative example 1: the preparation of hexafluoropropylene trimer raw material: by hexafluoropropene gas by being catalyzed equipped with NaF/Al2O3
The catalytic reaction tube of agent, the load capacity of catalyst are 10%, and the temperature of catalyst reaction tube is 260 DEG C, and time of contact is
0.1s；Mixed gas after reaction enters the condenser with cooling jacket by air inlet, and condensate temperature is 10 DEG C, unreacted
Hexafluoropropene through outlet be recycled to catalyst reaction tube.The purity of liquid hexafluoropropylene trimer in detection condenser
It is 99.3%.The yield of hexafluoropropylene trimer is shown in Table 1.
Comparative example 2: the preparation of hexafluoropropylene trimer raw material: by hexafluoropropene gas by being equipped with AgF/C catalyst
Catalytic reaction tube, the load capacity of catalyst are 15%, and the temperature of catalyst reaction tube is 300 DEG C, time of contact 10s,
Mixed gas after reaction enters the condenser with cooling jacket by air inlet, and condensate temperature is 10 DEG C；Unreacted six
Fluoropropene is recycled to catalyst reaction tube through outlet.The purity of liquid hexafluoropropylene trimer is in detection condenser
99.3%.The yield for applying rear hexafluoropropylene trimer is shown in Table 1.
Comparative example 3: hexafluoropropene gas the preparation of hexafluoropropylene trimer raw material: is passed through into urging equipped with KF/C catalyst
Change reaction tube, the load capacity of catalyst is 20%, and the temperature of catalyst reaction tube is 320 DEG C, time of contact 30s；Instead
Mixed gas after answering enters the condenser with cooling jacket by air inlet, and condensate temperature is 10 DEG C, unreacted hexafluoro
Propylene is recycled to catalyst reaction tube through outlet.The purity of liquid hexafluoropropylene trimer is in detection condenser
99.3%.The yield for applying rear hexafluoropropylene trimer is shown in Table 1.
Table 1
Embodiment 4: it hexafluoropropylene dimmer cracking: 1) pre-activate: specifically includes and hexafluoropropylene dimmer is passed through 200 DEG C
The reactor filled with pre-activate carrier in activate 1.5h；The active constituent of the pre-activate carrier is four (pentafluorophenyl group) boron
Hydrochlorate and Al ((CF3) 3) 3 according to mass ratio 1:3 mixture；The carrier of pre-activate carrier is SiO2；Load capacity is 15%.2)
Load capacity is filled in pyrolysis furnace and is 15% Ag2O/Al2O3 catalyst, and pyrolysis furnace is heated to 400 DEG C.By oxygen and activation
Hexafluoropropylene dimmer afterwards is passed through in pyrolysis furnace according to molar ratio 1:1.Reaction pressure is that 5bar. product is perfluor butyryl fluorine
50.09%, perfluor acetylfluoride 26.92%.
Embodiment 5: it hexafluoropropylene dimmer cracking: 1) pre-activate: specifically includes and hexafluoropropylene dimmer is passed through 200 DEG C
The reactor filled with pre-activate carrier in activate 1.5h；The active constituent of the pre-activate carrier is four (pentafluorophenyl group) boron
Hydrochlorate and Al ((CF3) 3) 3 according to mass ratio 1:3 mixture；The carrier of pre-activate carrier is SiO2；Load capacity is 15%.It splits
Load capacity is filled in solution furnace and is 15% KF/Al2O3 catalyst, and pyrolysis furnace is heated to 400 DEG C.After oxygen and activation
Hexafluoropropylene dimmer is passed through in pyrolysis furnace according to molar ratio 1:1, reaction pressure 5bar.Product is perfluor butyryl fluorine
62.46%, perfluor acetylfluoride 33.54%.
Embodiment 6: it hexafluoropropylene dimmer cracking: 1) pre-activate: specifically includes and hexafluoropropylene dimmer is passed through 180 DEG C
The reactor filled with pre-activate carrier in activate 2h；The active constituent of the pre-activate carrier is four (pentafluorophenyl group) boric acid
Salt and Al ((CFH2) 6) 3 according to mass ratio 1:1 mixture；The carrier of pre-activate carrier is Al2O3；Load capacity is 10%.It splits
Load capacity is filled in solution furnace and is 20% CuO/C catalyst, and pyrolysis furnace is heated to 600 DEG C.By six after oxygen and activation
Fluoropropene dimer is passed through in pyrolysis furnace according to molar ratio 10:1, and reaction pressure is normal pressure.Product is perfluor butyryl fluorine
57.90%, perfluor acetylfluoride 31.09%.
Embodiment 7: it hexafluoropropylene dimmer cracking: 1) pre-activate: specifically includes and hexafluoropropylene dimmer is passed through 220 DEG C
The reactor filled with pre-activate carrier in activate 1h；The active constituent of the pre-activate carrier is four (pentafluorophenyl group) boric acid
Salt and Al (CF2H) 3 according to mass ratio 1:5 mixture；The carrier of pre-activate carrier is B2O3；Load capacity is 20%.Pyrolysis furnace
In fill the CsF/C catalyst that load capacity is 10%, and pyrolysis furnace is heated to 150 DEG C.By the hexafluoro third after oxygen and activation
Alkene dimer is passed through in pyrolysis furnace according to molar ratio 1:10, reaction pressure 10bar.Product is perfluor butyryl fluorine 63.76%, entirely
Fluoracyl fluoride 34.24%.
Embodiment 8: hexafluoropropylene dimmer cracking: the Ag2O/Al2O3 that load capacity is 15% is filled in pyrolysis furnace and is catalyzed
Agent, and pyrolysis furnace is heated to 400 DEG C.Oxygen and hexafluoropropylene dimmer are passed through in pyrolysis furnace according to molar ratio 1:1.Reaction
Pressure is that 5bar. product is perfluor butyryl fluorine 35.13%, perfluor acetylfluoride 18.86%.Carbonyl fluoride 12.52%.
Embodiment 9: hexafluoropropylene dimmer cracking: filling the KF/Al2O3 catalyst that load capacity is 15% in pyrolysis furnace,
And pyrolysis furnace is heated to 400 DEG C.Oxygen and hexafluoropropylene dimmer are passed through in pyrolysis furnace according to molar ratio 1:1, reaction pressure
Power is 5bar.Product is perfluor butyryl fluorine 50.74%, perfluor acetylfluoride 27.25%.Carbonyl fluoride 6.32%.
Embodiment 10: hexafluoropropylene dimmer cracking: filling the CuO/C catalyst that load capacity is 20% in pyrolysis furnace, and
Pyrolysis furnace is heated to 600 DEG C.Oxygen and hexafluoropropylene dimmer are passed through in pyrolysis furnace according to molar ratio 10:1, reaction pressure
For normal pressure.Product is perfluor butyryl fluorine 44.24%, perfluor acetylfluoride 23.76%.Carbonyl fluoride 12.35%.
Embodiment 11: hexafluoropropylene dimmer cracking: filling the CsF/C catalyst that load capacity is 10% in pyrolysis furnace, and
Pyrolysis furnace is heated to 150 DEG C.Hexafluoropropylene dimmer after oxygen and activation is passed through in pyrolysis furnace according to molar ratio 1:10,
Reaction pressure is 10bar.Product is perfluor butyryl fluorine 52.69%, perfluor acetylfluoride 28.3%, carbonyl fluoride 5.64%.
Embodiment 12: prepare perfluor isobutyl ether by raw material of perfluor isobutyl acyl fluorides: by perfluor isobutyl acyl fluorides obtained by 28g,
71g iodomethane, 55g diethylene glycol dimethyl ether, 5.8g anhydrous potassium fluoride, 2g methyl tricapryl ammonium chloride, put into can pressure-bearing it is anti-
It answers in kettle, opens electric stirring, speed of agitator is 300 revs/min, sets temperature of reaction kettle as 100 DEG C, the reaction pressure of reaction kettle
Power is 1atm；It is kept for 28 hours, the KOH aqueous solution of 15g mass fraction 30% is added into reaction kettle.Gained mixed liquor is further
Washing, liquid separation are recycled after the dry water removal of upper layer organic solvent and are used, and lower layer's fluorine mutually obtains perfluor after drying, rectifying column rectifying
Isobutyl group methyl ether.It is greater than 99.9% through gas chromatographic detection product purity.Conversion rate of products 93.6%, product selectivity 99%.
Embodiment 13: prepare perfluor isobutyl ether by raw material of perfluor isobutyl acyl fluorides: by perfluor isobutyl acyl fluorides obtained by 108g,
15.6g iodoethane, 30g diethylene glycol dimethyl ether, 5.8g anhydrous potassium fluoride, 1g methyl tricapryl ammonium chloride, putting into can pressure-bearing
In reaction kettle, the reaction pressure of reaction kettle is 10atm；Electric stirring is opened, speed of agitator is 300 revs/min, sets reaction kettle
Temperature is 220 DEG C, and temperature is kept for 8 hours after rising to 220 DEG C, and the KOH that 60g mass fraction 30% is added into reaction kettle is water-soluble
Liquid, and continue to cool down to room temperature after being kept for 1 hour at 220 DEG C.Gained mixed liquor further washes, liquid separation, and upper layer is organic molten
It recycles and uses after the dry water removal of agent, lower layer's fluorine mutually obtains perfluor isobutyl group ether after drying, rectifying column rectifying.Through gas-chromatography
Testing product purity is greater than 99.9%.Conversion rate of products 21.4%.
Embodiment 14: perfluor isobutyl ether is prepared by raw material of perfluor isobutyl acyl fluorides: by perfluor isobutyryl obtained by 21.6g
Fluorine, 12.6g dimethyl suflfate, 25g diethylene glycol dimethyl ether, 5.8g anhydrous potassium fluoride, 1g methyl tricapryl ammonium chloride, put into
Can be in pressure-bearing reaction kettle, the reaction pressure of reaction kettle is 20atm；Electric stirring is opened, speed of agitator is 300 revs/min, setting
Temperature of reaction kettle is 120 DEG C, and temperature is kept for 9 hours after rising to 120 DEG C, and the KOH of 20g mass fraction 30% is added into reaction kettle
Aqueous solution, and continue to cool down to room temperature after being kept for 1 hour at 120 DEG C.Gained mixed liquor further washes, liquid separation, and upper layer has
It recycles and uses after the dry water removal of solvent, lower layer's fluorine mutually obtains perfluor isobutyl group methyl ether after drying, rectifying column rectifying.Through gas phase
Chromatography testing product purity is greater than 99.9%.Conversion rate of products 85.8%.
Embodiment 15: perfluor isobutyl ether is prepared by raw material of perfluor isobutyl acyl fluorides: by perfluor isobutyryl obtained by 21.6g
Fluorine, 12.6g dimethyl suflfate, 25g diethylene glycol dimethyl ether, 5.8g anhydrous potassium fluoride, 1g methyl tricapryl ammonium chloride, put into
Can be in pressure-bearing reaction kettle, the reaction pressure of reaction kettle is 10atm, opens electric stirring, and speed of agitator is 300 revs/min, setting
Temperature of reaction kettle is 20 DEG C, and temperature is kept for 9 hours after rising to 20 DEG C, and the KOH water of 20g mass fraction 30% is added into reaction kettle
Solution, and continue to cool down to room temperature after being kept for 1 hour at 20 DEG C.Gained mixed liquor further washes, liquid separation, and upper layer is organic molten
It recycles and uses after the dry water removal of agent, lower layer's fluorine mutually obtains perfluor isobutyl group methyl ether after drying, rectifying column rectifying.Through gas-chromatography
Testing product purity is greater than 99.9%.Conversion rate of products 81.2%.
The above is only a preferred embodiment of the present invention, for those of ordinary skill in the art, according to the present invention
Thought, there will be changes in the specific implementation manner and application range, and the content of the present specification should not be construed as to the present invention
Limitation.
Claims (6)
1. the device that a kind of hexafluoropropylene dimmer prepares perfluor isobutyl ether, which is characterized in that including hexafluoropropane dimer
Generation unit, perfluor isobutyl acyl fluorides generation unit and perfluor isobutyl ether generation unit；The hexafluoropropane dimer is raw
It include hexafluoropropene storage tank, catalytic reaction tube, condenser and the activating chamber being linked in sequence at unit；The perfluor isobutyryl
Fluorine generation unit includes the pyrolysis furnace and -2 DEG C of cold-traps being linked in sequence with the activating chamber；The perfluor isobutyl ether is raw
It include reaction kettle, stratification tower, drying tower, rectifying column and the product storage being linked in sequence at unit；Described -2 DEG C
The liquid outlet of cold-trap is connect with the reaction kettle.
2. the device that hexafluoropropylene dimmer according to claim 1 prepares perfluor isobutyl ether, which is characterized in that described
The gas discharge outlets of -2 DEG C of cold-traps connect with -70 DEG C of cold-traps to recycle perfluor acetylfluoride.
3. the device that hexafluoropropylene dimmer according to claim 1 prepares perfluor isobutyl ether, which is characterized in that described
Condenser external be provided with condensation collet；The condensation collet is provided with the condensation water inlet for condensed water inlet and outlet
And condensation-water drain.
4. the device that hexafluoropropylene dimmer according to claim 1 prepares perfluor isobutyl ether, which is characterized in that described
Condenser upper end be provided with outlet connect with the catalytic tower to recycle unreacted hexafluoropropene.
5. the device that hexafluoropropylene dimmer according to claim 1 prepares perfluor isobutyl ether, which is characterized in that described
Activating chamber and pyrolysis furnace connect respectively with heater.
6. the device that hexafluoropropylene dimmer according to claim 1 prepares perfluor isobutyl ether, which is characterized in that described
Catalytic reaction tube be provided with heating mantle.
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| CN116020152A (en) * | 2022-12-30 | 2023-04-28 | 滨州黄海科学技术研究院有限公司 | System and method for continuously separating hexafluoropropylene dimer and hexafluoropropylene trimer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116020152A (en) * | 2022-12-30 | 2023-04-28 | 滨州黄海科学技术研究院有限公司 | System and method for continuously separating hexafluoropropylene dimer and hexafluoropropylene trimer |
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