CN102372689A - Preparation method of trifluoromethyl ethylene carbonate - Google Patents
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- CN102372689A CN102372689A CN2011103675467A CN201110367546A CN102372689A CN 102372689 A CN102372689 A CN 102372689A CN 2011103675467 A CN2011103675467 A CN 2011103675467A CN 201110367546 A CN201110367546 A CN 201110367546A CN 102372689 A CN102372689 A CN 102372689A
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- LEGITHRSIRNTQV-UHFFFAOYSA-N carbonic acid;3,3,3-trifluoroprop-1-ene Chemical compound OC(O)=O.FC(F)(F)C=C LEGITHRSIRNTQV-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 150000005690 diesters Chemical class 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 23
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 19
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 10
- 235000017550 sodium carbonate Nutrition 0.000 claims description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 4
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 235000015320 potassium carbonate Nutrition 0.000 claims description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 4
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 4
- 239000011667 zinc carbonate Substances 0.000 claims description 4
- 235000004416 zinc carbonate Nutrition 0.000 claims description 4
- 229910000010 zinc carbonate Inorganic materials 0.000 claims description 4
- MFEVGQHCNVXMER-UHFFFAOYSA-L 1,3,2$l^{2}-dioxaplumbetan-4-one Chemical compound [Pb+2].[O-]C([O-])=O MFEVGQHCNVXMER-UHFFFAOYSA-L 0.000 claims description 3
- 229910000003 Lead carbonate Inorganic materials 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 2
- 235000012204 lemonade/lime carbonate Nutrition 0.000 claims description 2
- 125000005587 carbonate group Chemical group 0.000 claims 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 abstract description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 2
- QMASYWGIMXQPEJ-UHFFFAOYSA-N 3,3,3-trifluoropropane-1,2-diol Chemical compound OCC(O)C(F)(F)F QMASYWGIMXQPEJ-UHFFFAOYSA-N 0.000 abstract 2
- AQZRARFZZMGLHL-UHFFFAOYSA-N 2-(trifluoromethyl)oxirane Chemical compound FC(F)(F)C1CO1 AQZRARFZZMGLHL-UHFFFAOYSA-N 0.000 abstract 1
- FJNZCBUVTKMTNI-UHFFFAOYSA-N 2-bromo-3,3,3-trifluoropropan-1-ol Chemical compound OCC(Br)C(F)(F)F FJNZCBUVTKMTNI-UHFFFAOYSA-N 0.000 abstract 1
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 238000000605 extraction Methods 0.000 description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- CXHHBNMLPJOKQD-UHFFFAOYSA-M methyl carbonate Chemical compound COC([O-])=O CXHHBNMLPJOKQD-UHFFFAOYSA-M 0.000 description 6
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 5
- 150000005676 cyclic carbonates Chemical class 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 239000011255 nonaqueous electrolyte Substances 0.000 description 3
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- IVSZLXZYQVIEFR-UHFFFAOYSA-N m-xylene Chemical group CC1=CC=CC(C)=C1 IVSZLXZYQVIEFR-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 229910000733 Li alloy Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical compound CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 1
- 229940043232 butyl acetate Drugs 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 125000005911 methyl carbonate group Chemical class 0.000 description 1
- PQIOSYKVBBWRRI-UHFFFAOYSA-N methylphosphonyl difluoride Chemical group CP(F)(F)=O PQIOSYKVBBWRRI-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation method of trifluoromethyl ethylene carbonate, which comprises the steps of taking 2-bromo-3, 3, 3-trifluoropropanol as a raw material, hydrolyzing an alkali liquor to prepare 3,3, 3-trifluoro-1, 2-propanediol, mixing the obtained 3,3, 3-trifluoro-1, 2-propanediol with carbonic diester according to a proportion, taking methylbenzene, dimethylbenzene and the like as solvents, and taking carbonate as a catalyst to react to prepare the trifluoromethyl ethylene carbonate, wherein the purity of the product is more than 99.8%. The invention has the advantages that the expensive 3,3, 3-trifluoro-1, 2-epoxypropane is avoided being used as the raw material, the unreacted raw material can be recycled, the solvent can be reused, the preparation process is simple, and the high-purity trifluoromethyl ethylene carbonate can be obtained.
Description
Technical field
The present invention relates to organic synthesis field and lithium ion battery electrolytic solution field, particularly, relate to a kind of preparation method of trifluoromethyl ethylene carbonate.
Background technology
Cyclic carbonate comprises ethylene carbonate, Texacar PC and analogue thereof, is one type of important organic solvent, can fully dissolve various organism and inorganics, has very strong physics, chemicalstability and high specific inductivity.Therefore has very high industrial application value.
Cyclic carbonate is widely used in weaving, printing and dyeing, Polymer Synthesizing and electrochemical field (seeing JP 08-325258), simultaneously in the synthesizing of medicine and fine-chemical intermediate, also occupies critical role.
Because cyclic carbonate has stable physicochemical property, and can dissolve various organism and inorganics and high specific inductivity, is widely used as the non-aqueous electrolyte solvent of battery.Along with the develop rapidly of battery industry, the research of cyclic carbonate also increased gradually in recent years, and part has been carried out scale operation.But as electrolyte solvent; Also exist certain defective, for example: though its molecular weight of ethylene carbonate is low HMP up to 38 ℃ being arranged, at room temperature is solid-state; Must be when using through heating liquefaction, as the use temperature narrow range of solvent as solvent.Texacar PC is widely used as the non-aqueous electrolyte solvent of battery; But being used as with the graphite material is the solvent of the lithium ion battery of negative pole; Or when being the battery solvent of negative material with lithium or lithium alloy, Texacar PC can react with negative material, thereby has shortened the life-span of battery.
In order to remedy above defective; The external proposition replaces existing solvent with the cyclic carbonate of fluorine modification; Mainly contain a fluorine and replace ethylene carbonate, difluoro replacement ethylene carbonate and trifluoro replacement ethylene carbonate, and be applied in the electrolytic solution, effect is (seeing JP 07-165750) obviously.When particularly the trifluoromethyl ethylene carbonate uses as the non-aqueous electrolyte solvent, have the use temperature wide ranges, physical and chemical stability is good; Proof voltage is excellent; Charge-discharge cycle is good, and has high flash point and high security, is the ideal solvent of following battery electrolyte.
At present less about the research of trifluoromethyl ethylene carbonate, roughly there are two kinds of thinkings synthetic aspect: a kind of is with 3,3; 3-three fluoro-1; 2-propylene oxide and carbonic acid gas are raw material, and be directly synthetic under high temperature, high pressure, catalyzer condition, this method severe reaction conditions; Yield is very low, is unfavorable for suitability for industrialized production; Another kind is by 3,3, and the hydrolysis of 3-three fluoro-1,2 epoxy prapanes elder generation generates 3,3; 3-three fluoro-1, the 2-Ucar 35, again with 3,3,3-three fluoro-1; The 2-Ucar 35 joins in a large amount of methylcarbonates, is that catalyzer is synthetic with alkali, and this method is simple to operate, but reaction efficiency very low (seeing US 6010806).In addition, more than two kinds of methods also have a common shortcoming, just be to use expensively 3,3,3-three fluoro-1,2 epoxy prapanes are done raw material, have directly restricted the application process of trifluoromethyl ethylene carbonate.
In sum, the preparation method of the novel trifluoromethyl ethylene carbonate of development has very important significance.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of trifluoromethyl ethylene carbonate is to overcome the existing problem of prior art and cost aspect.
The present invention provides a kind of preparation method of trifluoromethyl ethylene carbonate, comprises with 2-bromo-3,3, and the 3-trifluoropropanol is a feedstock production 3,3,3-three fluoro-1,2-Ucar 35 and be Preparation of Catalyst trifluoromethyl ethylene carbonate with carbonate.
The present invention carries out in two steps, the first step, and 2-bromo-3,3, the hydrolysis of 3-trifluoropropanol generates midbody 3,3,3-three fluoro-1,2-Ucar 35; Second step, 3,3,3-three fluoro-1,2-Ucar 35 and carbonic diester reaction generate title product trifluoromethyl ethylene carbonate.
Particularly, the first step reaction is with 2-bromo-3,3, and the 3-trifluoropropanol joins in the alkali lye, reacts 6 ~ 8h at a certain temperature.Be cooled to room temperature then, extraction, distillating recovering solvent obtains midbody 3,3,3-three fluoro-1,2-Ucar 35.
Described alkali lye does not have particular requirement, sodium hydroxide, Pottasium Hydroxide, yellow soda ash, sodium hydrogencarbonate, salt of wormwood, saleratus etc. all can, can be one or more mixing solutionss wherein, preferred yellow soda ash, sodium hydrogencarbonate.
The concentration of described alkali lye between 1% ~ 60%, preferred 5% ~ 45%.
Described temperature of reaction is at 30 ~ 100 ℃, and preferred 50 ~ 80 ℃, more preferably 65 ~ 75 ℃.
Described extraction liquid does not have particular requirement, ETHYLE ACETATE, butylacetate etc. all can, ethyl acetate.
Particularly, the second step reaction be with obtain 3,3,3-three fluoro-1, the 2-Ucar 35 mixes with carbonic diester by a certain percentage, join then in the solvent, be catalyzer with carbonate, be heated to certain temperature and react 10 ~ 14h, rectifying obtains title product.
Described solvent can not be participated in chemical reaction, can control alcohol and carbonic diester azeotropic, with this understanding, and preferred normal hexane, heptane, toluene, o-Xylol, m-xylene, p-Xylol etc., more preferably normal hexane, o-Xylol, toluene, most preferably toluene.
Described carbonic diester does not have particular requirement, methylcarbonate, diethyl carbonate etc. all can, preferred methylcarbonate.
Described 3,3,3-three fluoro-1, the ratio of 2-Ucar 35 and carbonic diester is 1:1 ~ 1:10 in molar ratio, preferred 1:2 ~ 1:7, more preferably 1:3 ~ 1:5.
Described carbonate catalyst does not have particular requirement, salt of wormwood, yellow soda ash, zinc carbonate, lime carbonate, lead carbonate etc. all can, preferred zinc carbonate, yellow soda ash.
Described catalyst levels is 3,3,3-three fluoro-1,0.1 ~ 10%, preferred 0.1 ~ 5% of 2-Ucar 35 consumption.
Described temperature of reaction is at 65 ~ 135 ℃, along with the carrying out that reacts progressively raises.
The yield of title product of the present invention is more than 60%, and purity is more than 99.8%, and the gained compound is identified through nmr spectrum and mass spectrum, and is accurate.
The present invention compares with the compound method of before this trifluoromethyl ethylene carbonate; Advantage is that required cost significantly reduces; Do not use severe toxicity or the reagent of environmental protection pressure is arranged, reaction conditions is gentle, and is workable; Raw material is easy to get and recyclable utilization, is a kind of method that simply makes the trifluoromethyl ethylene carbonate.
Embodiment
Following examples are used to explain the present invention, but are not used for limiting scope of the present invention.
Embodiment 1:
The aqueous sodium carbonate 1000g of adding 20% in the 2000mL there-necked flask stirs adding 164g 2-bromo-3,3, and the 3-trifluoropropanol is heated to 70 ℃ of reaction 6h.Be cooled to room temperature then, divide three extractions with 1600mL ETHYLE ACETATE, to neutral, distillation extraction liquid reclaims ETHYLE ACETATE to extraction liquid, obtains 3,3,3-three fluoro-1,2-Ucar 35, yield 80%, product purity 94% with the saturated common salt water washing.
In 1000mL there-necked flask (having rectifying tower), add 540g toluene, stir adding 180g methylcarbonate, 130g3 then, 3; 3-three fluoro-1,2-Ucar 35,5g zinc carbonate; Be heated to 65 ℃ of reactions,, improve Heating temperature gradually along with the carrying out of reaction; In heat-processed, constantly steam methyl alcohol, approximately react 10h.After reaction finished, unreacted methylcarbonate and solvent toluene were reclaimed in rectifying, and obtain product trifluoromethyl ethylene carbonate.Product yield is 77%, product purity 99.8%.
Embodiment 2:
The sodium bicarbonate aqueous solution 1000g of adding 15% adds 130g 2-bromo-3,3 then in the 2000mL there-necked flask, and the 3-trifluoropropanol is heated to 75 ℃ of reaction 6h.Be cooled to room temperature, divide three extractions with 1600mL ETHYLE ACETATE, to neutral, distillation extraction liquid reclaims ETHYLE ACETATE to extraction liquid, obtains 3,3,3-three fluoro-1,2-Ucar 35, yield 78%, product purity 96% with the saturated common salt water washing.
In 1000mL there-necked flask (having rectifying tower), add the 400g o-Xylol, stir adding 252g diethyl carbonate, 134g3,3; 3-three fluoro-1,2-Ucar 35,3.2g yellow soda ash; Be heated to 80 ℃ of reactions,, constantly steam ethanol in the reaction process along with reaction improves constantly Heating temperature.After reaction finished, diethyl carbonate and solvent were reclaimed in rectifying, obtain the trifluoromethyl ethylene carbonate.Product yield is 68%, product purity 99.8%.
Embodiment 3:
In the 2000mL there-necked flask, add 180g yellow soda ash, 20g sodium hydroxide, be configured to the mixed aqueous solution 1000g of yellow soda ash-sodium hydroxide of 20%, stir, add 190g2-bromo-3,3 then; The 3-trifluoropropanol is heated to 70 ℃ of reaction 6h, is cooled to room temperature, divides three extractions with 1600mL ETHYLE ACETATE; To neutral, distillation extraction liquid reclaims ETHYLE ACETATE to extraction liquid, obtains 3,3 with the saturated common salt water washing; 3-three fluoro-1,2-Ucar 35, yield 83%, product purity 95%.
In 1000mL there-necked flask (having rectifying tower), add 500g toluene, the 234g methylcarbonate stirs, and adds 113g3 then; 3,3-three fluoro-1,2-Ucar 35,2.5g lead carbonate; Be heated to 65 ℃ of reactions,, constantly steam methyl alcohol in the reaction process along with reaction improves constantly Heating temperature.Reaction finishes back rectifying and reclaims unreacted methylcarbonate and solvent, obtains the trifluoromethyl ethylene carbonate.Product yield is 65%, product purity 99.8%.
Claims (9)
1. the preparation method of a trifluoromethyl ethylene carbonate comprises with 2-bromo-3,3, and the 3-trifluoropropanol is a feedstock production 3,3,3-three fluoro-1, and the 2-Ucar 35, and with 3,3,3-three fluoro-1,2-Ucar 35 are intermediate preparation trifluoromethyl ethylene carbonate.
2. according to the preparation method of claim 1, it is characterized in that the preparation process carries out in two steps, 3,3,3-three fluoro-1, the 2-Ucar 35 is as synthetic intermediate.
3. according to the preparation method of claim 1, it is characterized in that the 3-trifluoropropanol is main raw material preparation 3,3,3-three fluoro-1,2-Ucar 35 with 2-bromo-3,3.
4. according to the preparation method of claim 1, it is characterized in that 3,3; 3-three fluoro-1; 2-Ucar 35 and carbonic diester react in solvent, and through the azeotropic of solvent control alcohol with carbonic diester, make the two be able to separate; Solvent for use is normal hexane, heptane, toluene, YLENE etc., and consumption is 1 ~ 10 times of carbonic diester consumption.
5. according to claim 1,3 preparation method, it is characterized in that with alkali lye 2-bromo-3,3; The 3-trifluoropropanol is hydrolyzed and prepares 3; 3,3-three fluoro-1,2-Ucar 35; Alkali lye comprises one or more the aqueous solution in yellow soda ash, sodium hydrogencarbonate, salt of wormwood, saleratus, sodium hydroxide, the Pottasium Hydroxide etc., and concentration of lye is 1% ~ 60%.
6. according to claim 1,3 preparation method, it is characterized in that temperature of reaction is at 30 ~ 100 ℃.
7. according to claim 1,4 preparation method, it is characterized in that by 3,3; 3-three fluoro-1, it is carbonate that the 2-Ucar 35 prepares trifluoromethyl ethylene carbonate catalyst system therefor, comprises one or more of salt of wormwood, yellow soda ash, zinc carbonate, lime carbonate, lead carbonate etc.; Consumption is 3; 3,3-three fluoro-1,0.1 ~ 10% of 2-Ucar 35 consumption.
8. according to claim 1,4 preparation method, it is characterized in that Heating temperature raises with the carrying out of reaction gradually, TR is 65 ~ 135 ℃.
9. according to the preparation method of claim 4, it is characterized in that 3,3,3-three fluoro-1, the mol ratio of 2-Ucar 35 and carbonic diester is 1:1 ~ 1:10.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105399607A (en) * | 2015-11-06 | 2016-03-16 | 西安近代化学研究所 | Method for preparing 3,3,3-trifluoro propanol |
| CN108178752A (en) * | 2017-12-19 | 2018-06-19 | 西安近代化学研究所 | A kind of method that coproduction prepares 3,3,3- trifluoro propenes carbonic ester and tri- fluoro- 1,2- propylene glycol of 3,3,3- |
| CN111892481A (en) * | 2019-05-05 | 2020-11-06 | 石家庄圣泰化工有限公司 | Preparation method of 3,3, 3-propylene trifluorocarbonate |
| CN113087695A (en) * | 2021-03-31 | 2021-07-09 | 武汉大学 | Rapid energy-saving integrated method for preparing aliphatic polycarbonate monomer |
| CN114421012A (en) * | 2022-01-25 | 2022-04-29 | 河北松辰医药科技有限公司 | Lithium battery electrolyte additive and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105399607A (en) * | 2015-11-06 | 2016-03-16 | 西安近代化学研究所 | Method for preparing 3,3,3-trifluoro propanol |
| CN105399607B (en) * | 2015-11-06 | 2017-12-22 | 西安近代化学研究所 | A kind of preparation method of 3,3,3 trifluoropropanol |
| CN108178752A (en) * | 2017-12-19 | 2018-06-19 | 西安近代化学研究所 | A kind of method that coproduction prepares 3,3,3- trifluoro propenes carbonic ester and tri- fluoro- 1,2- propylene glycol of 3,3,3- |
| CN108178752B (en) * | 2017-12-19 | 2021-02-23 | 西安近代化学研究所 | Method for preparing 3,3, 3-trifluoropropene carbonate and 3,3, 3-trifluoro-1, 2-propylene glycol in co-production mode |
| CN111892481A (en) * | 2019-05-05 | 2020-11-06 | 石家庄圣泰化工有限公司 | Preparation method of 3,3, 3-propylene trifluorocarbonate |
| CN113087695A (en) * | 2021-03-31 | 2021-07-09 | 武汉大学 | Rapid energy-saving integrated method for preparing aliphatic polycarbonate monomer |
| CN114421012A (en) * | 2022-01-25 | 2022-04-29 | 河北松辰医药科技有限公司 | Lithium battery electrolyte additive and preparation method thereof |
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