CN102030618A - Method for preparing heptafluoroisobutenyl methyl ether - Google Patents
Method for preparing heptafluoroisobutenyl methyl ether Download PDFInfo
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- CN102030618A CN102030618A CN2010105348234A CN201010534823A CN102030618A CN 102030618 A CN102030618 A CN 102030618A CN 2010105348234 A CN2010105348234 A CN 2010105348234A CN 201010534823 A CN201010534823 A CN 201010534823A CN 102030618 A CN102030618 A CN 102030618A
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Abstract
The invention discloses a method for preparing heptafluoroisobutenyl methyl ether. The method comprises the following steps of: (1) providing10 to 55 weight percent aqueous alkali; (2) providing octafluoroisobutyl methyl ether, wherein the molar ratio of the alkali to the octafluoroisobutyl methyl ether is between 0.5 and 5.0; and (3) mixing the octafluoroisobutyl methyl ether and the aqueous alkali to react with stirring at the temperature from room temperature to octafluoroisobutyl methyl ether boiling point (56 DEG C), even the temperature of 35 DE C below the octafluoroisobutyl methyl ether boiling point to obtain the heptafluoroisobutenyl methyl ether; and the method is characterized in that the stirring is performed by rotor and stator stirring technology.
Description
Technical field
The present invention relates to a kind of method of under normal pressure, making seven fluorine iso-butylene methyl ethers.
Background technology
The tetrafluoroethylene pyrolysis method that adopts is produced the R 1216 Technology at present, can produce about 10% perfluoroisobutylene by product.The high toxicity of perfluoroisobutylene and poison after be difficult to healing property, limited the direct application of perfluoroisobutylene; For reducing the influence of perfluoroisobutylene to the operator, the organic fluorine industry has been popularized and has been used methyl alcohol to absorb perfluoroisobutylene, becomes the perfluoroisobutylene methyl alcohol absorption liquid that toxicity reduces, and carries out the technology of burning disposal perfluoroisobutylene methyl alcohol absorption liquid then.But burning disposal has also been wasted resource except meeting produces environmental problem.Therefore more existing both at home and abroad enterprises attempt making a silk purse out of a sow's ear, the technology of exploitation comprehensive utilization perfluoroisobutylene methyl alcohol absorption liquid.
The first step of many comprehensive utilization perfluoroisobutylene methyl alcohol absorption liquid technology all is that perfluoroisobutylene methyl alcohol absorption liquid is made seven more stable fluorine iso-butylene methyl ethers of structure, adopts different method for oxidation manufacturing purpose product Perfluoroacetones then.
For example, U.S. Pat 4,660,947 have introduced O
2Catalyzed oxidation technology, U.S. Pat 4,734,169 have been introduced hydrogen peroxide-electrochemistry co-oxidation technology, U.S. Pat 4,960, and 947 introduce O
3Oxidation technology, Japanese Patent JP61-277645 introduce hydrogen peroxide-photoxidation technology.
Chinese patent CN1583693 and CN1827567 provide a kind of method and apparatus that is used to handle perfluoroisobutylene methyl alcohol absorption liquid, adopt this method can make octafluoro isobutyl-methyl crude product; Further separate and the thick ether of purification octafluoro isobutyl-methyl, can obtain purity at the octafluoro isobutyl-methyl ether more than 90%.
Susumu Misaki is at fluorine chemistry magazine (Journal of Fluorine Chemistry, 29 (1985) 471-474) disclose a kind of in the presence of alkali (as the potassium hydroxide of 25-50%) on, octafluoro isobutyl-methyl ether dehydrofluorination is degraded into the method for seven fluorine iso-butylene methyl ethers and 2-trifluoromethyl-3-methoxyl group-1-perfluoro propylene, and its chemical equation and test situation are as follows:
(CF
3)
2CHCF
2OCH
3→(CF
3)
2C＝CFOCH
3+CF
2＝C(CF
3)CF
2OCH
3
(1) (2) (3)
Annotate: (1) is raw material; (2) be the purpose product; (3) be by product.
As seen from the above table, the yield of the method that proposes of Susumu Misaki with high transformation efficiency, seven fluorine iso-butylene methyl ethers can reach about 78-83%.
In addition, Susumu Misaki thinks that for reaching the above-mentioned high transformation efficiency and the yield of seven fluorine iso-butylene methyl ethers, the temperature of reaction of alkali lye and octafluoro isobutyl-methyl ether is proper about 65～85 ℃.But 56 ℃ of octafluoro isobutyl-methyl ether boiling points, so the reaction of Susumu Misaki proposition alkali lye and octafluoro isobutyl-methyl ether is carried out under pressure.
The thermopositive reaction of under pressure, carrying out for alkali lye and this class of octafluoro isobutyl-methyl ether, the semi-continuous charging method is often adopted in this area, be exactly to add earlier octafluoro isobutyl-methyl ether or alkali lye, then under 65～85 ℃ of temperature, under pressure, slowly add another kind of material.This technology not only needs withstand voltage reactor, pressurised metered pump, and under stress carries out deleterious octafluoro isobutyl-methyl ether and alkaline reaction, has the hidden danger of leaking in the junction of reactor, pipeline, valve etc.
In addition, the surface tension of the fluorine-containing ether octafluoro of known height isobutyl-methyl ether own is lower, but there is bigger interfacial tension between it and the alkali aqueous solution, makes and sprawl, permeate difficulty mutually between high fluorine-containing ether and the alkali lye, become immiscible two-phase (be commonly called as and hate effect mutually); There is difference in specific gravity between high fluorine-containing ether and the alkali lye simultaneously, aggravated the two-phase layering.This area adopts following method to improve the two-phase demixing phenomenon usually:
(a) known to temperature raises, hate the two phase liquid interfacial tension to descend mutually, when temperature during near critical temperature, interfacial tension levels off to disappearance; Along with temperature raises, speed of response is accelerated simultaneously.Therefore the SusumuMisaki disclosed method has been utilized this principle exactly, with the fluorine-containing ether octafluoro of height isobutyl-methyl ether (bp:56 ℃) and 65～85 ℃ of reactions of alkali lye more than octafluoro isobutyl-methyl ether boiling point;
(b) use organic synthesis agitator commonly used at normal temperatures and pressures, as frame, oar formula, turbine type, propeller type stirrer.But when adopting this conventional alr mode, long reaction time, the transformation efficiency of liquid phase octafluoro isobutyl-methyl ether and alkaline reaction are low, so this alr mode commonly used does not almost have use value.Though the raising mixing speed can improve some octafluoro isobutyl-methyl ethers and alkaline reaction yield, reaction yield improves and is few, does not still have use value;
(c) adopt fluorochemical surfactant, can at normal temperatures the emulsification of fluorine ether octafluoro isobutyl-methyl ether be dispersed in the alkali aqueous solution as the tripolymer acid of the cationic perfluor decoylamide third ammonium trimethylammonium iodide, anionic Perfluorocaprylic Acid or solvable perfluorooctanoic acid salt, perfluoro propene oxid or the tripolymer hydrochlorate of soluble perfluoro propene oxid, increase the contact area of immiscible two-phase, fast reaction speed realizes temperature of reaction is reduced to the purpose of reacting below the octafluoro isobutyl-methyl ether boiling point.But obtain emulsion after the reaction, need to add methods such as emulsion splitter, impel breakdown of emulsion to be divided into two-phase, separate obtaining seven fluorine iso-butylene methyl ether crude products.This method not only needs expensive fluorochemical surfactant, and the waste water that contains fluorochemical surfactant can not arbitrarily discharge, and needs research to reclaim the technology of fluorine surfactant from waste water, and this is the work that difficulty is big, cost is high.
Therefore the method that needs the exploitation manufacturing seven fluorine iso-butylene methyl ethers that a kind of security is good, equipment cost is low, working cost is low, preferably a kind of method that under normal pressure, makes octafluoro isobutyl-methyl and alkaline reaction.
Summary of the invention
The purpose of this invention is to provide the method for under normal pressure, making seven fluorine iso-butylene methyl ethers that a kind of security is good, equipment cost is low, working cost is low.
Therefore, the invention provides a kind of manufacture method of seven fluorine iso-butylene methyl ethers, it comprises the steps:
(1) providing concentration is the alkaline solution of 10-55 weight %;
(2) provide octafluoro isobutyl-methyl ether, the mole number of described alkali is 0.5～5.0 with the ratio of described octafluoro isobutyl-methyl ether mole number;
(3) under the temperature from room temperature to 56 ℃ of octafluoro isobutyl-methyl ether boiling points even under 35 ℃ temperature below the octafluoro isobutyl-methyl ether boiling point, under agitation condition, make octafluoro isobutyl-methyl ether and alkaline solution hybrid reaction, obtain seven fluorine iso-butylene methyl ethers;
It is characterized in that described stirring is to adopt to change the realization of stator stirring technique.
The commentaries on classics stator stirring technique that the present invention uses should meet the following conditions:
1) changeing the stator agitator should go deep into or be immersed in the liquid, but liquid sucting port is not deep into the degree that contacts with jar end or tank skin, should with at the bottom of the still or wall at a distance of a segment distance, this distance is generally 0.1～10 times of rotor diameter, be preferably 0.5～5 times of rotor diameter, more preferably 0.7～3 times of rotor diameter;
2) rotor diameter of commentaries on classics stator agitator should mate with the reactor diameter, and general reactor diameter is 100: 1～2: 1 with the ratio of rotor diameter, is preferably 50: 1～3: 1, more preferably 20: 1～4: 1;
3) spinner velocity is generally 3～50 meter per seconds, and fast more emulsifying effectiveness is good more, but fast more watt consumption is big more, and commonly used is 7～30 meter per seconds, and it is 10～20 meter per seconds that Technological Economy is preferably.
Changeing the stator agitator is a kind of special agitator that utilizes rotating rotor to match and stir with the fixed stator, is mainly used in manufacture field.This agitator and emulsifying agent synergy is used to make stable emulsion in manufacture field.As two kinds of insoluble liquid are cooperated with emulsifying agent, under the effect of changeing the stator agitator, can form stability emulsion preferably, this emulsifying technology is usually used in diesel oil emulsification, heavy oil etc.; Perhaps liquid, with the immiscible powder of this liquid, at emulsifying agent with change under the synergy of stator agitator and form emulsion,, obtain whiteruss as microcrystalline wax is dispersed in the water.
Specific implementation method
In the present invention, term " commentaries on classics stator stirring technique " is meant and utilizes rotating rotor to cooperate a kind of agitator hybrid technology that plays the Special Mixed effect with the fixed stator.
The manufacture method of the present invention's seven fluorine iso-butylene methyl ethers comprises that it is the step of the alkaline solution of 10-55 weight % that concentration is provided.The alkali that is applicable to the inventive method is without particular limitation, as long as can form seven fluorine iso-butylene methyl ethers with the reaction of octafluoro isobutyl-methyl ether.In an example of the present invention, described alkali is selected from alkali metal hydroxide, alkaline carbonate, alkaline earth metal hydroxides etc.The example of its indefiniteness has, for example two or more mixture of potassium hydroxide, salt of wormwood, sodium hydroxide, yellow soda ash, alkaline earth metal hydroxides soluble in water or its.
The solvent that is used to form described alkaline solution is without particular limitation, can be the solvent of any routine known in the art.The indefiniteness example of described solvent has, for example water, C1-6 lower alcohol (as methyl alcohol, ethanol, n-propyl alcohol, Virahol, propyl carbinol etc.), acid amides are (as N, dinethylformamide, N,N-dimethylacetamide etc.), two or more mixture etc. of sulfone (as dimethyl sulfoxide (DMSO), tetramethylene sulfone etc.), ether (as ethylene-propylene ether, isopropyl ether etc.) or its.Consider that water price is honest and clean, nontoxic and environmentally friendly, therefore preferential employing water is as solvent.
The concentration of described alkaline solution is generally 10-55 weight %, is preferably 25-50 weight %, more preferably 35-50 weight %.
The potassium hydroxide of operating weight concentration 10～55% or solution of potassium carbonate in an example of the present invention, the solution that adopts alkali than use the solid alkali reaction temperature and, be convenient to the control reaction.
The inventive method also comprises the step that octafluoro isobutyl-methyl ether is provided, and the amount of described octafluoro isobutyl-methyl ether makes that the ratio of mole number and described octafluoro isobutyl-methyl ether mole number of described alkali is 0.5～5.0, is preferably 0.8～3.5, more preferably 1.1～2.1.
The inventive method also comprises under the temperature from room temperature to octafluoro isobutyl-methyl ether boiling point (56 ℃) even under 35 ℃ temperature below the octafluoro isobutyl-methyl ether boiling point, under agitation condition, make octafluoro isobutyl-methyl ether and alkaline solution hybrid reaction, obtain the step of seven fluorine iso-butylene methyl ethers.
The inventive method makes octafluoro isobutyl-methyl ether and alkaline solution react under the temperature of octafluoro isobutyl-methyl ether boiling point (56 ℃) in room temperature, better to the temperature that is lower than 10 ℃ of octafluoro isobutyl-methyl ether boiling points, react from room temperature, better to the temperature that is lower than 20 ℃ of octafluoro isobutyl-methyl ether boiling points, react, thereby avoided that octafluoro isobutyl-methyl ether seethes with excitement in the reaction process from room temperature.The result is controlled at reaction under the normal pressure and carries out, and need not expensive complicated high pressure reactor.
The inventive method is carried out under normal pressure, and the present inventor is surprised to find to choose especially from the known multiple stirring technique of prior art changes that the stator stirring technique carries out octafluoro isobutyl-methyl ether and alkaline reaction can obtain high octafluoro isobutyl-methyl ether transformation efficiency.For example, when temperature of reaction be the boiling temperature of octafluoro isobutyl-methyl ether to 35 ℃ of boiling temperatures that is lower than octafluoro isobutyl-methyl ether and adopt when changeing the stator stirring technique, octafluoro isobutyl-methyl ether transformation efficiency is 95.2%-99.8%.Under similarity condition, when adopting other stirring techniques, octafluoro isobutyl-methyl ether transformation efficiency will hang down more than 1 times.
Carry out octafluoro isobutyl-methyl ether and alkaline reaction being lower than under the octafluoro isobutyl-methyl ether boiling point, be in atmospheric pressure state naturally, do not need withstand voltage still and pressurised metered pump, reduced facility investment and process cost, improved production efficiency.
Advantage of the present invention
Adopt conventional stirring,, need be more than octafluoro isobutyl-methyl ether boiling point 65～85 ℃, in withstand voltage reactor, carry out octafluoro isobutyl-methyl ether and react, just can obtain higher reaction yield with potassium hydroxide aqueous solution as oar formula, spiral stirring etc.Adopting changes the stator stirring technique, octafluoro isobutyl-methyl and potassium hydroxide aqueous solution temperature of reaction can be dropped to 56 ℃ of octafluoro isobutyl-methyl ether boiling points, even temperature of reaction can be dropped to below the octafluoro isobutyl-methyl ether boiling point 35 ℃ reaction, do not need to use withstand voltage reactor, still can obtain higher yield, become valuable manufacture method.
Further specify the present invention below in conjunction with embodiment.
Embodiment
In this article except as otherwise noted, otherwise all concentration is weight concentration.
Comparative example 1
In 5 liters of reactor (length-to-diameter ratios 1.1: 1 that thermometer, chuck cooling, frame stirring are housed; 5 millimeters in frame and still inwall gap) the middle octafluoro isobutyl-methyl ether that adds 1.5 kilogram of 95% concentration; Under the effect of 5 revolutions per seconds of rotating speeds, add 3 kilograms of saturated potassium hydroxide aqueous solutions (about 55%) [alkali: ether mol ratio=4.79] gradually, temperature of reaction control is consistent with envrionment temperature to be 10 ℃, drips off in 1 hour; 10 ℃ of holding temperatures continue to stir 0.5 hour.Octafluoro isobutyl-methyl ether transformation efficiency 30.5%, seven fluorine iso-butylene methyl ether yield 26.7%.
Comparative example 2
Thermometer, chuck cooling, 45 ° of 5 liters of reactor (length-to-diameter ratios 1.1: 1 that double leaf folding oar stirs are being housed; Diameter of propeller blade and still internal diameter were than 0.5: 1) in add the octafluoro isobutyl-methyl ether of 2 kilogram of 90% concentration; Under the effect of 15 revolutions per seconds of rotating speeds, add 2.5 kilogram of 45% potassium hydroxide aqueous solution [alkali: ether mol ratio=2.59] gradually, temperature of reaction control is consistent with envrionment temperature to be 20 ℃, drips off in 1 hour; 20 ℃ of holding temperatures continue to stir 0.5 hour.Octafluoro isobutyl-methyl ether transformation efficiency 34.8%, seven fluorine iso-butylene methyl ether yield 32.5%.
Comparative example 3
Thermometer, chuck cooling, the pusher 5 liters of reactor (length-to-diameter ratios 1.1: 1 that stir of 3 leaves are being housed; Diameter of propeller blade and still internal diameter were than 0.25: 1) in add the octafluoro isobutyl-methyl ether of 2 kilogram of 85% concentration; Under the effect of 32 revolutions per seconds of rotating speeds, add 2 kilogram of 40% potassium hydroxide aqueous solution [alkali: ether mol ratio=1.88] gradually, temperature of reaction is controlled at 30 ℃, drips off in 1 hour; 30 ℃ of holding temperatures continue to stir 0.5 hour.Octafluoro isobutyl-methyl ether transformation efficiency 41.6%, seven fluorine iso-butylene methyl ether yield 39.2%.
Comparative example 4
In 5 liters of reactor (length-to-diameter ratios 1.1: 1 that thermometer, chuck cooling, the stirring of 4 leaf worm gears are housed; Diameter of propeller blade and still internal diameter were than 0.3: 1) in add the octafluoro isobutyl-methyl ether of 2 kilogram of 88% concentration; Under the effect of 25 revolutions per seconds of rotating speeds, add 1.8 kilogram of 40% potassium hydroxide aqueous solution [alkali: ether mol ratio=1.69] gradually, temperature of reaction is controlled at 45 ℃, drips off in 1 hour; 45 ℃ of holding temperatures continue to stir 0.5 hour.Octafluoro isobutyl-methyl ether transformation efficiency 38.8%, seven fluorine iso-butylene methyl ether yield 36.9%.
Comparative example 5
In 5 liters of reactor (length-to-diameter ratios 1.1: 1 that thermometer, chuck cooling, the stirring of 4 leaf worm gears are housed; Diameter of propeller blade and still internal diameter were than 0.3: 1; Built-in two symmetries long 15 centimetres, wide 1 centimetre of baffle plate) the middle octafluoro isobutyl-methyl ether that adds 2 kilogram of 92% concentration; Under the effect of 25 revolutions per seconds of rotating speeds, add 1.8 kilogram of 30% potassium hydroxide aqueous solution [alkali: ether mol ratio=1.22] gradually, temperature of reaction is controlled at 56 ℃, drips off in 1 hour; 56 ℃ of holding temperatures continue to stir 0.5 hour.Octafluoro isobutyl-methyl ether transformation efficiency 48.8%, seven fluorine iso-butylene methyl ether yield 44.7%.
Embodiment 1
(liquid sucting port that changes the stator agitator and Polycondensation Reactor and Esterification Reactor be at a distance of at a distance of 3 times of rotor diameters, with reactor wall 0.5 times of rotor diameter apart the cooling of thermometer, chuck is housed, changes in 500 liters of reactors that stator stirs (three leaves are tiltedly starched rotor, uniform aperture stator); Rotor diameter should be 1: 2 with the reactor diameter ratio), the octafluoro isobutyl-methyl ether of 150 kilogram of 95% concentration of adding; Under the effect of rotor speed 40 meter per seconds, add 300 kilograms of saturated potassium hydroxide aqueous solutions (about 55%) [alkali: ether mol ratio=4.79] gradually, temperature of reaction control is consistent with envrionment temperature to be 10 ℃, drips off in 1 hour; 10 ℃ of holding temperatures continue to stir 0.5 hour.Octafluoro isobutyl-methyl ether transformation efficiency 95.2%, seven fluorine iso-butylene methyl ether yield 80.3%.
Embodiment 2
The cooling of thermometer, chuck is being housed, is changeing stator and stir in 500 liters the reactor that (the curved slurry of three leaves band rotor, vertical bar hole stator) mix that (liquid sucting port that changes the stator agitator and Polycondensation Reactor and Esterification Reactor be at a distance of at a distance of 2 times of rotor diameters, with reactor wall 1 times of rotor diameter apart; Rotor diameter should be 1: 3 with the reactor diameter ratio), the octafluoro isobutyl-methyl ether of 200 kilogram of 90% concentration of adding; Under the effect of rotor speed 30 meter per seconds, add 250 kilogram of 45% potassium hydroxide aqueous solution [alkali: ether mol ratio=2.59] gradually, temperature of reaction control is consistent with envrionment temperature to be 20 ℃, adds in 1 hour; 20 ℃ of holding temperatures remained in operation 0.5 hour.Octafluoro isobutyl-methyl ether transformation efficiency 95.5%, seven fluorine iso-butylene methyl ether yield 82.5%.
Embodiment 3
(liquid sucting port that changes the stator agitator and Polycondensation Reactor and Esterification Reactor be at a distance of at a distance of 1.5 times of rotor diameters, with reactor wall 1.5 times of rotor diameters apart the cooling of thermometer, chuck is housed, changes in 500 liters the reactor that stator stirs (three leaves are tiltedly starched rotor, oblique slot type stator); Rotor diameter should be 1: 4 with the reactor diameter ratio), the octafluoro isobutyl-methyl ether of 200 kilogram of 85% concentration of adding; Under the effect of rotor speed 25 meter per seconds, add 200 kilogram of 40% potassium hydroxide aqueous solution [alkali: ether mol ratio=1.88] gradually, control reaction liquid temperature is 30 ℃, adds in 1 hour; 30 ℃ of holding temperatures continue operation 0.5 hour.Octafluoro isobutyl-methyl ether transformation efficiency 98.1%, seven fluorine iso-butylene methyl ether yield 84.7%.
Embodiment 4
(liquid sucting port that changes the stator agitator and Polycondensation Reactor and Esterification Reactor be at a distance of at a distance of 3 times of rotor diameters, with reactor wall 3 times of rotor diameters apart the cooling of thermometer, chuck is housed, changes in 500 liters the reactor that stator stirs (four leaves are tiltedly starched rotor, small sircle hole stator); Rotor diameter should be 1: 7 with the reactor diameter ratio), the octafluoro isobutyl-methyl ether of 200 kilogram of 88% concentration of adding; Under the effect of rotor speed 20 meter per seconds, add 180 kilogram of 40% potassium hydroxide aqueous solution [alkali: ether mol ratio=1.69] gradually, temperature of reaction is controlled to be 45 ℃, drips off in 1 hour; 45 ℃ of holding temperatures continue operation 0.5 hour.Octafluoro isobutyl-methyl ether transformation efficiency 99.0%, seven fluorine iso-butylene methyl ether yield 83.5%.
Embodiment 5
(liquid sucting port that changes the stator agitator and Polycondensation Reactor and Esterification Reactor be at a distance of at a distance of 0.7 times of rotor diameter, with reactor wall 4 times of rotor diameters apart the cooling of thermometer, chuck is housed, changes in 500 liters the reactor that stator stirs (the straight oar rotor of four leaves, vertical bar pore stator); Rotor diameter should be 1: 9 with the reactor diameter ratio), the octafluoro isobutyl-methyl ether of 200 kilogram of 95% concentration of adding; Under the effect of rotor speed 27 meter per seconds, add 180 kilogram of 40% potassium hydroxide aqueous solution [alkali: ether mol ratio=1.57] gradually, temperature of reaction control is warmed up to 35 ℃ naturally from 11 ℃ of envrionment temperatures, and 35 ℃ of controlled temperature dripped off in 1 hour; 35 ℃ of holding temperatures continue to stir 1 hour.Octafluoro isobutyl-methyl ether transformation efficiency 99.8%, seven fluorine iso-butylene methyl ether yield 85.1%.
Embodiment 6
(liquid sucting port that changes the stator agitator and Polycondensation Reactor and Esterification Reactor be at a distance of at a distance of 3 times of rotor diameters, with reactor wall 5 times of rotor diameters apart the cooling of thermometer, chuck is housed, changes in 500 liters the reactor that stator stirs (the straight oar rotor of four leaves, vertical bar pore stator); Rotor diameter should be 1: 11 with the reactor diameter ratio), the octafluoro isobutyl-methyl ether of 200 kilogram of 97% concentration of adding; Under the effect of rotor speed 16 meter per seconds, add 180 kilogram of 25% potassium hydroxide aqueous solution [alkali: ether mol ratio=0.96] gradually, temperature of reaction is warmed up to 56 ℃ of octafluoro isobutyl-methyl ether boiling temperatures naturally from 15 ℃ of envrionment temperatures, keeps 56 ℃ of temperature of reaction, drips off in 1 hour; Holding temperature is 56 ℃ again, continues to stir 1 hour.Octafluoro isobutyl-methyl ether transformation efficiency 85.1%, seven fluorine iso-butylene methyl ether yield 78.1%.
Claims (10)
1. the manufacture method of a fluorine iso-butylene methyl ether, it comprises the steps:
(1) providing concentration is the alkaline solution of 10-55 weight %;
(2) provide octafluoro isobutyl-methyl ether, the mole number of described alkali is 0.5～5.0 with the ratio of described octafluoro isobutyl-methyl ether mole number;
(3) in reactor, under octafluoro isobutyl-methyl ether boiling temperature, under agitation condition, make octafluoro isobutyl-methyl ether and alkaline solution hybrid reaction, obtain seven fluorine iso-butylene methyl ethers in room temperature;
It is characterized in that
Described stirring is to adopt to change the stator agitator, utilizes commentaries on classics stator stirring technique to finish.
2. the method for claim 1 is characterized in that described alkali is selected from two or more mixture of alkali metal hydroxide, alkaline carbonate, alkaline earth metal hydroxides or its.
3. method as claimed in claim 2 is characterized in that described alkali is selected from two or more mixture of potassium hydroxide, salt of wormwood, sodium hydroxide, yellow soda ash or its.
4. the method for claim 1, the concentration that it is characterized in that described alkali is 25～50 weight %.
5. as each described method among the claim 1-4, it is characterized in that the described alkali and the ratio of octafluoro isobutyl-methyl ether mole number are 1.1-2.1.
6. as each described method among the claim 1-4, it is characterized in that described alkali is selected from potassium hydroxide and salt of wormwood.
7. the method for claim 1 is characterized in that described alkaline solution is an aqueous alkali solution.
8. as each described method among the claim 1-7, it is characterized in that changeing at the bottom of the liquid sucting port of stator agitator and the still and/or wall at a distance of 0.1～10 times of rotor diameter, be preferably 0.5～5 times of rotor diameter, more preferably 0.7～3 times of rotor diameter.
9. as each described method among the claim 1-8, it is characterized in that the described reactor diameter and the ratio of rotor diameter are 100: 1～2: 1, be preferably 50: 1～3: 1, more preferably 20: 1～4: 1.
10. as each described method among the claim 1-8, it is characterized in that spinner velocity is 3～50 meter per seconds, be preferably 7～30 meter per seconds, more preferably 10～20 meter per seconds.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102500307A (en) * | 2011-10-20 | 2012-06-20 | 上海三爱富新材料股份有限公司 | Stirring equipment and use thereof in preparation of heptafluoroisobutenyl methyl ether |
| CN102744025A (en) * | 2012-07-25 | 2012-10-24 | 武汉大学 | Reaction equipment for manufacturing inorganic materials with micro-nano structure |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6335534A (en) * | 1986-07-31 | 1988-02-16 | Nippon Mektron Ltd | Production of heptafluoroisobutenyl alkyl ether |
| CN2532510Y (en) * | 2001-12-18 | 2003-01-22 | 中国乐凯胶片集团公司 | Agitator |
| CN1827567A (en) * | 2004-06-04 | 2006-09-06 | 上海三爱富新材料股份有限公司 | Device for treating perfluoroisobutylene methanol absorption liquid |
-
2010
- 2010-11-08 CN CN2010105348234A patent/CN102030618A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6335534A (en) * | 1986-07-31 | 1988-02-16 | Nippon Mektron Ltd | Production of heptafluoroisobutenyl alkyl ether |
| CN2532510Y (en) * | 2001-12-18 | 2003-01-22 | 中国乐凯胶片集团公司 | Agitator |
| CN1827567A (en) * | 2004-06-04 | 2006-09-06 | 上海三爱富新材料股份有限公司 | Device for treating perfluoroisobutylene methanol absorption liquid |
Non-Patent Citations (2)
| Title |
|---|
| ROBERT J. KOSHA等: "The Addition of Alcohols to Octafluoroisobutene", 《JOURNAL OF AMERICAN CHEMICAL SOCIETY》, vol. 79, no. 7, 30 April 1957 (1957-04-30), pages 1741 - 1744 * |
| 刘存玉: "转子-定子式混合器及其应用", 《化工装备技术》, vol. 26, no. 4, 30 August 2005 (2005-08-30), pages 20 - 22 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102500307A (en) * | 2011-10-20 | 2012-06-20 | 上海三爱富新材料股份有限公司 | Stirring equipment and use thereof in preparation of heptafluoroisobutenyl methyl ether |
| CN102744025A (en) * | 2012-07-25 | 2012-10-24 | 武汉大学 | Reaction equipment for manufacturing inorganic materials with micro-nano structure |
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