CN107349871A - A kind of long-chain perfluoropolyether surfactants and preparation method thereof - Google Patents
A kind of long-chain perfluoropolyether surfactants and preparation method thereof Download PDFInfo
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- CN107349871A CN107349871A CN201710505403.5A CN201710505403A CN107349871A CN 107349871 A CN107349871 A CN 107349871A CN 201710505403 A CN201710505403 A CN 201710505403A CN 107349871 A CN107349871 A CN 107349871A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
- C09K23/007—Organic compounds containing halogen
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D1/00—Fire-extinguishing compositions; Use of chemical substances in extinguishing fires
- A62D1/0071—Foams
- A62D1/0085—Foams containing perfluoroalkyl-terminated surfactant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
- C08G65/332—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof
- C08G65/3322—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof acyclic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/333—Polymers modified by chemical after-treatment with organic compounds containing nitrogen
- C08G65/33303—Polymers modified by chemical after-treatment with organic compounds containing nitrogen containing amino group
- C08G65/33306—Polymers modified by chemical after-treatment with organic compounds containing nitrogen containing amino group acyclic
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Abstract
The present invention relates to a kind of long-chain perfluoropolyether surfactants and preparation method thereof to be：PFPE acyl fluorides ether, solvent are first added in a kettle, adds two aminates, heating response kettle while stirring, and reaction is cooled to room temperature after terminating；Reduced pressure treatment and column chromatography purification are carried out afterwards, finally chloracetate solution, water are added in compound A, heating stirring, and reaction obtains long-chain perfluoropolyether surfactants after terminating.Long-chain perfluoropolyether surfactants preparation method of the present invention is simple, and stable processing technique is easily operated；Reaction condition is gentle, it is not necessary to which catalyst, energy consumption is small, and equipment requirement is simple；High conversion rate, the discharge of production process non-toxic by-products is pollution-free, has good environment protecting.
Description
Technical field
The present invention relates to surfactant, especially a kind of long-chain perfluoropolyether surfactants and preparation method thereof.
Background technology
Fluorine surfactant is that active highest is a kind of in known surfactant, and it has " three high ", " two hate " i.e.
High surface, high thermal stability, high chemical stability, fluorocarbon chain section are both hydrophobic and oleophobic, and its application field is extensive, such as work
The flotation of ore in industry, sugaring, is all widely used in pharmacy, and microbiological plants.
One of application of fluorocarbon surfactant is used as aqueous film-forming foam extinguishing agent, with hc-surfactant and fluorine carbon
Surfactant is base-material, and can form the fire foam of water membrane on some hydrocarbon liquids surfaces.Common dioxy
Change carbon extinguishing chemical DeGrain, especially in the case where the fire condition of the large area such as oil storage tank occurs, traditional fire extinguishing technique has one
Fixed limitation, it is necessary to which a kind of spreadability is good, and anti-burning significant effect, now, fluorine-containing surfactant just shows uniqueness
Extinguishing property.When being characterized in fire extinguishing, the foam of formation can be spread over well forms water membrane on pasta, this layer of water
Film can completely cut off air, reduce oil surface temperature, so as to play quick extinguishing effect, be lived due to adding fluorochemical surface in extinguishing chemical
Property agent, greatly reduces the surface tension of water, sprawls rapidly, and foam is also sprawled rapidly, equivalent to two layers barrier film, available for putting out
The various non-solution including oils are flammable, the fire that flammable liquid occurs.Additionally, due to the addition of fluorine-containing surfactant,
The shearing force that foam flows in liquid surface is reduced, improves mobile performance, so as to reach the effect of quick extinguishing.
The performance of fluorocarbon surfactant is related to the length of its carbochain, its mobile performance of the fluorocarbon surfactant of long-chain
More preferably, fire extinguishing when can preferably quick extravagance open, so as to improve its extinguishing property.But the fluorocarbon surface of long-chain is lived in industry
Property agent synthesis cost it is higher, it is necessary to using catalyst, late-stage products separation is difficult, and product purity is bad, so as to influence puts out a fire
Performance.
The content of the invention
Problem to be solved by this invention is to overcome the shortcomings of the prior art, there is provided a kind of long-chain PFPE surface
Activating agent and preparation method thereof.The long-chain perfluoropolyether surfactants simple production process, it is not necessary to use catalyst, product
Purity is high, and high income is economic and environment-friendly.
The main component of long-chain perfluoropolyether surfactants of the present invention is PFPE glycine betaine, its molecule knot
Structure formula is CF3(OCF2)nCONH(CH2)mN(R)(R’)CH2COONa, wherein n=60；M=2,3,4；R=CH3Or C2H5；R '=
CH3Or C2H5, because its structure is different from the perfluoropolyether surfactants of small molecule series, and sulfonic group is not contained, so its
Extinguishing effect is more preferable, and does not produce toxic smog sulfur dioxide.
The present invention is using PFPE acyl fluorides ether, two aminates as raw material, it is not necessary to and catalyst can directly carry out ammonolysis reaction,
Synthetic product obtains target product by column chromatography for separation, then quaterisation occurs with chloracetate, you can synthesis perfluor gathers
Ether surface active agent.Wherein column chromatography processing improves the purity of active ingredient in perfluoropolyether surfactants, and separates skill
Art is safe and reliable, and the other useless components avoided in reaction environment produce pernicious gas in fire extinguishing, have good environmental protection
Effect.
In preparation method of the present invention, reduced pressure treatment step is very crucial, if without depressurization steps, will be unable to close
Into target product.Product heats after ammonolysis reaction to 100 DEG C, 2-4h are taken out using vacuum pump pressure by the present invention, are changed anti-
The interior environment answered, so as to ensure that the orderly growth of carbochain, side reaction is considerably less, and quaterisation could be carried out successfully.
Concrete scheme is as follows：
A kind of long-chain perfluoropolyether surfactants, are prepared according to following steps：
Ammonolysis reaction：PFPE acyl fluorides ether, solvent are added in reactor, adds two aminates while stirring, is heated
Reactor, reaction are cooled to room temperature after terminating；
Reduced pressure treatment：Product after ammonolysis reaction is subjected to reduced pressure treatment, takes out 2- with vacuum pump pressure under the conditions of 100 DEG C
4h；
Column chromatography purifies：Product after upper step reduced pressure treatment is subjected to separating-purifying, chromatographic column is 100-200 mesh silica gel, is used
Two pairs of benzotrifluorides make solvent between 1,3, obtain compound A；
Quaterisation：Chloracetate solution, water are added in compound A, heating stirring, reaction is grown after terminating
Chain perfluoropolyether surfactants；The molecular weight of described long-chain PFPE acyl fluorides ether is 3000-4000.
Further, in described ammonolysis reaction step, raw material adding proportion is：PFPE acyl fluorides ether, solvent, diamines
The mol ratio of compound is 1:0.5:1.1-1.3.
Further, in described ammonolysis reaction step, two described aminates are NH2(CH2)mN (R ') R, wherein, m=
2,3,4；R=CH3Or C2H5；R '=CH3Or C2H5；
Optional, two described aminates are N, and N- bis- substitutes propane diamine.
Further, in described ammonolysis reaction step, described solvent is in isopropanol, dichloromethane, chloroform
Any one.
Further, in described ammonolysis reaction step, reaction temperature is 90-130 DEG C, and the reaction time is 6-8 hours.
Further, in described quaterisation step, chloracetate solution is the chlorine that mass concentration is 20%-30%
The aqueous solution of acetate.
Further, in described quaterisation step, the addition of chloracetate solution is, solute chloracetate
Quality is 1.3-1.6 times of PFPE acyl fluorides ether；
Optional, in described quaterisation step, the addition of water is the PFPE acyl added in reaction system
Fluorine ether, solvent, 3.5 times of two aminates and chloracetate solution gross weight.
Further, in described quaterisation step, reaction condition is that 1.5-2.5 hours are reacted under reflux state.
A kind of purposes of described long-chain perfluoropolyether surfactants, it is molten as heat transfer fluid, foam foaming agent, gas
The host of glue propellant, flame retardant or aqueous film-forming foam extinguishing agent.
A kind of preparation method of described long-chain perfluoropolyether surfactants, comprises the following steps：
Ammonolysis reaction：PFPE acyl fluorides ether, solvent are added in reactor, adds two aminates while stirring, is heated
Reactor, reaction are cooled to room temperature after terminating；
Reduced pressure treatment：Product after ammonolysis reaction is subjected to reduced pressure treatment, takes out 2- with vacuum pump pressure under the conditions of 100 DEG C
4h；
Column chromatography purifies：Product after upper step reduced pressure treatment is subjected to separating-purifying, chromatographic column is 100-200 mesh silica gel, is used
Two pairs of benzotrifluorides make solvent between 1,3, obtain compound A；
Quaterisation：Chloracetate solution, water are added in compound A, heating stirring, reaction is grown after terminating
Chain perfluoropolyether surfactants.
Beneficial effect：Long-chain perfluoropolyether surfactants preparation method of the present invention is simple, stable processing technique
It is easily operated；Reaction condition is gentle, it is not necessary to which catalyst, energy consumption is small, and equipment requirement is simple；Handled by decompression and column chromatography
Long-chain products are obtained, and product yield is high, isolation technics is safe and reliable, and target product purity is high, has good environmental protection effect
Fruit；Long-chain perfluoropolyether surfactants excellent performance of the present invention, the aqueous film-forming foam extinguishing agent prepared as host
The control fire time it is short, fire-fighting efficiency is high, and especially durable lather hardness is high, and interfacial film is firmer, and the time of anti-burning is longer, every
Index reaches national sector standard.
Embodiment
Technical solution of the present invention is further elaborated with reference to embodiment.Unreceipted particular technique or bar in embodiment
Part person, carried out according to the technology described by document in the art or condition or according to product description.Agents useful for same or instrument
The unreceipted production firm person of device, being can be by the conventional products of acquisition purchased in market.
Product inspection method is as follows：
1. anti-freeze, melt performance test
Required instrument, equipment have：Refrigerating chamber：Temperature requirement as defined in this standard 1.2a can be reached；Port grinding bottle (or plastics
Bottle)：500ml, water white transparency
Method：A) temperature of refrigerating chamber is adjusted to tract below 10 DEG C of sample freezing point；B) 300ml samples are injected into port grinding bottle
(or plastic bottle), being put into refrigerating chamber cooling freezes it, and keeping temperature 24h；C) repeat said process three times, complete four jellies
Knot and melt cycle；D) observation sample whether there is layering and heterogeneous phenomenon
2. the measure of foam number pH value, performed by GB 15308-94 5.4
3. the measure of foam solution sediment
Required device includes：Centrifuge：2 000r/min of controllable rotating speed ± 100r/min；Taper scale centrifuge tube：
50mL, conical lower portion minimum division value 0.1mL sub-sieves；180 μm of aperture；Plastic squeeze bottle.
Method：The taper scale centrifuge tube equipped with 50mL foam solutions is symmetrically put into centrifuge respectively, covers lid,
10min is centrifuged under conditions of 2 000r/min ± 100r/min；Centrifuge tube is taken out, records the percentage by volume of sediment；With
Plastic squeeze bottle in the sample wash in test tube to 180 μm of sub-sieves, will be observed under current of the sediment in plastic squeeze bottle rinse
It is no to disperse to pass through sieve.
Pay attention to：To ensure that the precipitate distribution in shuttle is uniform during sampling, first with two taper scale centrifuge tubes
50mL is taken to have bubble as the sample before degradation respectively；Then take 120mL to be placed in vial again to seal mouth,
Degradation is done, 24h ± 2h is kept at 60 DEG C ± 2 DEG C, sample returns to room temperature after degradation, stirs evenly, with two tapers
Scale centrifuge tube takes 50mL samples respectively, must not there is bubble.
4. the measure of foam solution mobility, performed by GB 15308-94 5.3
5. the measure of foam solution diffusion coefficient
Required instrument, equipment and reagent include：Surface tension instrument：Precision is 0.1mN/m；Measurement range be 0mN/m~
180mN/m；Hexamethylene：Content is not less than 99%；Foam solution：Using 100mL volumetric flasks and pipette, advised by product description
Fixed concentration prepares foam solution with distilled water of the surface tension not less than 70mN/m.
Method：
1) measure of surface tension
A) foam solution temperature is adjusted to 20 DEG C ± 1 DEG C, is determined its surface tension, is accurate to 0.1mN/m；
B) experiment is repeated once, takes the average value tested twice as measurement result.
2) measure of interfacial tension
A) after having determined surface tension, platinum loop is made to be down to below foam solution liquid level, on foam solution plus one layer of 5mm~
20 DEG C ± 1 DEG C thick 7mm of hexamethylene.After waiting 6min ± 1min, interfacial tension is determined, is accurate to 0.1mN/m；
B) experiment is repeated once, takes the average value tested twice as measurement result.
3) calculating of diffusion coefficient
The diffusion coefficient of foam solution is calculated as follows：
S=Tc-Ts-Ti
In formula：S --- diffusion coefficient, mN/m；
The surface tension of Tc --- hexamethylene, mN/m；
The surface tension of Ts --- foam solution, mN/m；
Ti --- the interfacial tension between foam solution and hexamethylene, mN/m.
6. the measure of coefficient of foaming and 25% drainage time, performed according to GB 15308-94
7. the measure of extinguishing property, performed according to GB 15308-94, wherein AFFF, AFFF/AR are to non-water-soluble liquid
The particular content of the fire-extinguishing test of fuel is as follows：
1) instrument, equipment, material
Steel tray for combustion：2 400mm of internal diameter ± k25mm, depth 200mm ± 15mm, wall thickness 2.5mm；
Baffle plate：Long 1 000mm ± 50mm, high 1 000mm ± 50mm, apply experiment suitable for slow；
The anti-burning tank of steel：Internal diameter 300mm ± 5mm, depth 250mm ± 5mm, wall thickness 2.5mm；
Anemobiagraph：0~10m/s；
Stopwatch：Precision 0.1s；
Fuel：Rubber industry solvent naphtha, meet the requirement of the certified products of SH 0004-90.
2) fire-extinguishing test step is applied
By 7.5.1.2 in GB 15308-94.
Anti- burning tank size in the experiment of 25% fire resistanttime should meet this standard 7.5.1a).
3) fire-extinguishing test step is applied by force
Standard foam rifle position, which is put, should be such that foam center jet directly falls in away from the combustion at 1 000mm of distal disc wall ± 100mm
Expect on surface；The application foam time is 180s ± 2s.Record attack time.Such as stop flame after applying foam not extinguish, can
Whether extinguish etc. flame to be seen, if fray-out of flame, record attack time.Terminate applying foam to anti-burning on-test
When, it is allowed to it is not more than 500mm flash burn flame in disk with the presence of horizontal size summation.Applying foam allows the short time to pause, and stops
Immediately total application foam time should be charged between.
Embodiment 1
2.0 moles of PFPE acyl fluorides ether, its molecular weight are 3000-4000,1 mole of solvent isopropanol, are added to 20L bands
It is added dropwise 2.6 moles of N in the reactor for having return stirring and heating and heat-insulating device, under stirring in batches, N dimethyl the third two
Amine, and slowly heating, 60 DEG C of system temperature, react 6 hours, are cooled to room temperature, and process produces a small amount of hydrogen fluoride gas by condensing
The alkali lye pond suitable for reading that imported into is managed to absorb；Then in the above-mentioned product 2-4h of 100 DEG C of reduced pressure treatments, solvent and two aminates are removed.
Column chromatography processing：Chromatographic column, 100-200 mesh silica gel, silica gel is with bulk product than 3:1-5:1, with two pairs three between 1,3
Toluene fluoride makees solvent, is separated, and point plate leaves required component, obtains compound A, its yield is about 85%-90%, and purity can
To reach more than 98%.
The sodium chloroacetate aqueous solution that previously prepared 2.6 molar concentration is 20% is added in compound A, backflow 1.5
Hour, obtain dark yellow liquid.It is cooled to room temperature, it is determined as sample 1, it is stand-by.
Embodiment 2
Such as embodiment 1, difference is that ammonolysis reaction solvent is dichloromethane, and temperature is 90 DEG C, during quaterisation
Backflow 2 hours, it is determined as sample 2, it is stand-by.
Embodiment 3
Such as embodiment 1, difference is in the N in ammonolysis reaction, 2.4 moles of N dimethyl propane diamine dosage, reaction temperature
115 DEG C, to react 7 hours, sodium chloroacetate dosage is 2.6 moles during quaterisation, is made into 30% aqueous solution, is flowed back 2 hours,
It is set to sample 3, it is stand-by.
Embodiment 4
Such as embodiment 1, difference is in the N in ammonolysis reaction, 2.5 moles of N dimethyl propane diamine dosage, reaction temperature 90
DEG C, to react 7 hours, sodium chloroacetate dosage is 2.8 moles during quaterisation, is made into 20% aqueous solution, is flowed back 2.5 hours,
It is set to sample 4, it is stand-by.
Embodiment 5
Such as embodiment 1, difference is in ammonolysis reaction, and solvent is chloroform, N, N dimethyl propane diamine dosage
2.5 moles, 50 DEG C of reaction temperature, react 7 hours, 2.6 moles of sodium chloroacetate dosage during quaterisation, be made into 20% it is water-soluble
Liquid, flow back 2 hours, it is determined as sample 5, it is stand-by.
Embodiment 6
Such as embodiment 1, difference is in the N in ammonolysis reaction, 2.2 moles of N dimethyl propane diamine dosage, reaction temperature 80
DEG C, react 7 hours, sodium chloroacetate dosage is also 2.6 moles during quaterisation, is made into 30% aqueous solution, and backflow 2.5 is small
When, it is determined as sample 6, it is stand-by.
Embodiment 7
Such as embodiment 1, difference is in the N in ammonolysis reaction, 2.3 moles of N dimethyl propane diamine dosage, reaction temperature 75
DEG C, to react 8 hours, sodium chloroacetate dosage is 2.7 moles during quaterisation, is made into 30% aqueous solution, is flowed back 2.5 hours,
It is set to sample 7, it is stand-by.
Embodiment 8
Such as embodiment 1, difference is in the N in ammonolysis reaction, 2.4 moles of N dimethyl propane diamine dosage, reaction temperature 85
DEG C, react 8 hours, sodium chloroacetate dosage is 2.7 moles during quaterisation, is made into 20% aqueous solution, is flowed back 3 hours, fixed
It is stand-by for sample 8.
With the sample 1-8 obtained by embodiment 1-8, aqueous film-forming foam extinguishing agent is respectively configured, successively labeled as sample 9-
16, performance detection is carried out to it, it is as a result as follows：
Wherein, compound method is specially referring to patent of invention CN105013125 A：Surfactant of the present invention
5%, urea 5%, alpha-olefin sodium sulfonate 15%, lauryl sodium sulfate 10%%, APG (1412) 16%, remaining is
Water.
The sample 9-16 physicochemical properties of table 1 and performance indications table
As it can be seen from table 1 long-chain perfluoropolyether surfactants excellent performance of the present invention, is prepared as host
Aqueous film-forming foam extinguishing agent the control fire time it is short, fire-fighting efficiency is high, indices such as anti-freeze, melts performance, pH value, precipitation
Thing, diffusion coefficient, coefficient of foaming, 25% drainage time reach national sector standard.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art is not departing from the principle and objective of the present invention
In the case of above-described embodiment can be changed within the scope of the invention, change, replace and modification.
Claims (10)
- A kind of 1. long-chain perfluoropolyether surfactants, it is characterised in that：It is prepared according to following steps：Ammonolysis reaction：PFPE acyl fluorides ether, solvent are added in reactor, adds two aminates, heating response while stirring Kettle, reaction are cooled to room temperature after terminating；Reduced pressure treatment：Product after ammonolysis reaction is subjected to reduced pressure treatment, takes out 2-4h with vacuum pump pressure under the conditions of 100 DEG C；Column chromatography purifies：Product after upper step reduced pressure treatment is subjected to separating-purifying, chromatographic column is 100-200 mesh silica gel, between 1,3 Two pairs of benzotrifluorides make solvent, obtain compound A；Quaterisation：Chloracetate solution, water are added in compound A, heating stirring, it is complete that reaction obtains long-chain after terminating Perfluoroalkyl polyether surfactant；The molecular weight of described long-chain PFPE acyl fluorides ether is 3000-4000.
- 2. long-chain perfluoropolyether surfactants according to claim 1, it is characterised in that：Described ammonolysis reaction step In, raw material adding proportion is：PFPE acyl fluorides ether, solvent, the mol ratio of two aminates are 1:0.5:1.1-1.3.
- 3. long-chain perfluoropolyether surfactants according to claim 1, it is characterised in that：Described ammonolysis reaction step In, two described aminates are NH2(CH2)mN (R ') R, wherein, m=2,3,4；R=CH3Or C2H5；R '=CH3Or C2H5；Optional, two described aminates are N, and N- bis- substitutes propane diamine.
- 4. long-chain perfluoropolyether surfactants according to claim 1, it is characterised in that：Described ammonolysis reaction step In, described solvent is any one in isopropanol, dichloromethane, chloroform.
- 5. long-chain perfluoropolyether surfactants according to claim 1, it is characterised in that：Described ammonolysis reaction step In, reaction temperature is 90-130 DEG C, and the reaction time is 6-8 hours.
- 6. long-chain perfluoropolyether surfactants according to claim 1, it is characterised in that：Described quaterisation step In rapid, chloracetate solution is the aqueous solution for the chloracetate that mass concentration is 20%-30%.
- 7. long-chain perfluoropolyether surfactants according to claim 1, it is characterised in that：Described quaterisation step In rapid, the addition of chloracetate solution is that the quality of solute chloracetate is 1.3-1.6 times of PFPE acyl fluorides ether；It is optional, in described quaterisation step, the addition of water be added in reaction system PFPE acyl fluorides ether, 3.5 times of solvent, two aminates and chloracetate solution gross weight.
- 8. long-chain perfluoropolyether surfactants according to claim 1, it is characterised in that：Described quaterisation step In rapid, reaction condition is that 1.5-2.5 hours are reacted under reflux state.
- A kind of 9. purposes of the long-chain perfluoropolyether surfactants described in any one of claim 1-8, it is characterised in that：It is used as Heat transfer fluid, foam foaming agent, aerosol propellants, the host of flame retardant or aqueous film-forming foam extinguishing agent.
- 10. a kind of preparation method of the long-chain perfluoropolyether surfactants described in any one of claim 1-8, its feature exist In：Comprise the following steps：Ammonolysis reaction：PFPE acyl fluorides ether, solvent are added in reactor, adds two aminates, heating response while stirring Kettle, reaction are cooled to room temperature after terminating；Reduced pressure treatment：Product after ammonolysis reaction is subjected to reduced pressure treatment, takes out 2-4h with vacuum pump pressure under the conditions of 100 DEG C；Column chromatography purifies：Product after upper step reduced pressure treatment is subjected to separating-purifying, chromatographic column is 100-200 mesh silica gel, between 1,3 Two pairs of benzotrifluorides make solvent, obtain compound A；Quaterisation：Chloracetate solution, water are added in compound A, heating stirring, it is complete that reaction obtains long-chain after terminating Perfluoroalkyl polyether surfactant.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109054795A (en) * | 2018-08-08 | 2018-12-21 | 成都理工大学 | A kind of preparation method of extra-low-permeability reservoir displacement of reservoir oil hydridization fluorine-containing surfactant |
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