CN115197255B - Low-moisture solid boron trifluoride methyl ethyl carbonate complex and preparation method and application thereof - Google Patents
Low-moisture solid boron trifluoride methyl ethyl carbonate complex and preparation method and application thereof Download PDFInfo
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- CN115197255B CN115197255B CN202210920235.7A CN202210920235A CN115197255B CN 115197255 B CN115197255 B CN 115197255B CN 202210920235 A CN202210920235 A CN 202210920235A CN 115197255 B CN115197255 B CN 115197255B
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- VEWIGYNQVZOINO-UHFFFAOYSA-N C(OCC)(OC)=O.B(F)(F)F Chemical compound C(OCC)(OC)=O.B(F)(F)F VEWIGYNQVZOINO-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000007787 solid Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000010668 complexation reaction Methods 0.000 title description 9
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical class FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 claims abstract description 82
- 239000007788 liquid Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 150000001335 aliphatic alkanes Chemical class 0.000 claims abstract description 16
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 51
- 229910015900 BF3 Inorganic materials 0.000 claims description 40
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 35
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 18
- 230000000536 complexating effect Effects 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 4
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 3
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 claims description 3
- KNKRKFALVUDBJE-UHFFFAOYSA-N 1,2-dichloropropane Chemical compound CC(Cl)CCl KNKRKFALVUDBJE-UHFFFAOYSA-N 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052744 lithium Inorganic materials 0.000 abstract description 13
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000003792 electrolyte Substances 0.000 abstract description 5
- 239000002904 solvent Substances 0.000 abstract description 5
- 229910003002 lithium salt Inorganic materials 0.000 abstract description 4
- 159000000002 lithium salts Chemical class 0.000 abstract description 4
- 230000002194 synthesizing effect Effects 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 11
- 239000000203 mixture Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000012265 solid product Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- WIHMGGWNMISDNJ-UHFFFAOYSA-N 1,1-dichloropropane Chemical compound CCC(Cl)Cl WIHMGGWNMISDNJ-UHFFFAOYSA-N 0.000 description 1
- -1 1-dichloroethane Chemical compound 0.000 description 1
- FQUVVJDWJHHKKX-UHFFFAOYSA-N C(OC(C)C)(O)=O.B(F)(F)F Chemical class C(OC(C)C)(O)=O.B(F)(F)F FQUVVJDWJHHKKX-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/02—Boron compounds
- C07F5/022—Boron compounds without C-boron linkages
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0568—Liquid materials characterised by the solutes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
Abstract
The invention relates to the technical field of boron trifluoride complexes, and provides a low-moisture solid boron trifluoride methyl ethyl carbonate complex, a preparation method and application thereof. According to the invention, chlorinated alkane is used as a solvent to prepare the boron trifluoride methyl ethyl carbonate complex, and the water content in the complex is effectively carried out by the chlorinated alkane during solid-liquid separation by strictly controlling the dosage of the chlorinated alkane, so that the solid boron trifluoride methyl ethyl carbonate complex with low water content is obtained; the water content of the boron trifluoride methyl ethyl carbonate complex prepared by the method is less than 100ppm, can meet the requirement of the lithium battery field on the water content of production raw materials, can be used for synthesizing lithium battery electrolyte lithium salt, fills the application blank of the lithium battery field, and has wide prospect.
Description
Technical Field
The invention relates to the technical field of boron trifluoride complexes, in particular to a preparation method of a low-moisture solid boron trifluoride methyl ethyl carbonate complex.
Background
The methyl ethyl carbonate is colorless transparent liquid, is insoluble in water, can be used for organic synthesis, is an excellent solvent for lithium ion battery electrolyte, and the boron trifluoride methyl ethyl carbonate complex can be used for synthesizing lithium battery electrolyte lithium salt, so that the potential requirement on the lithium battery market is huge.
However, the water content of the raw materials for producing lithium batteries is very strict, and generally needs to be less than 100ppm to meet the requirement. At present, when boron trifluoride complex is prepared in the field, the boron trifluoride complex is generally prepared by directly introducing gaseous boron trifluoride into a liquid raw material, and the boron trifluoride gas and the methyl ethyl carbonate raw material both contain water, so that the boron trifluoride methyl ethyl carbonate obtained by the method has higher water content and cannot meet the market requirement. Therefore, the water content of the boron trifluoride methyl ethyl carbonate complex becomes a key constraint factor, and no boron trifluoride methyl ethyl carbonate complex with low water content exists in the market at present, and the application of the boron trifluoride methyl ethyl carbonate complex in the aspect of lithium batteries is also blank.
Disclosure of Invention
In view of the above, the invention provides a low-moisture solid boron trifluoride methyl ethyl carbonate complex, and a preparation method and application thereof. The boron trifluoride methyl ethyl carbonate complex prepared by the invention has the water content as low as below 100ppm, and fills the blank in the application aspect of lithium ion batteries.
In order to achieve the above object, the present invention provides the following technical solutions:
a preparation method of a low-moisture solid boron trifluoride methyl ethyl carbonate complex comprises the following steps:
mixing methyl ethyl carbonate and chloralkane to obtain a mixed solution; the mass ratio of the methyl ethyl carbonate to the chlorinated alkane is 1:1-6;
introducing boron trifluoride gas into the mixed solution for complex reaction to obtain complex reaction feed liquid;
under a closed condition, carrying out solid-liquid separation on the complex reaction feed liquid to obtain a low-moisture solid boron trifluoride methyl ethyl carbonate complex; the water content of the low-water solid boron trifluoride methyl ethyl carbonate complex is below 100 ppm.
Preferably, the chlorinated alkane is one or more of dichloromethane, 1 dichloroethane, 1,2 dichloroethane and dichloropropane.
Preferably, the boron trifluoride gas is industrial boron trifluoride gas.
Preferably, the molar ratio of the methyl ethyl carbonate to the boron trifluoride is 1:0.95-1.05.
Preferably, the temperature of the complexation reaction is-10-25 ℃ and the time is 3-24 h.
Preferably, the boron trifluoride gas is introduced at a rate of 50g/h to 27kg/h.
Preferably, the complexing reaction is carried out under stirring, and the stirring speed is 100-300 r/min.
Preferably, the solid-liquid separation method is centrifugation.
The invention also provides the low-moisture solid boron trifluoride methyl ethyl carbonate complex prepared by the preparation method of the scheme, and the moisture content of the low-moisture solid boron trifluoride methyl ethyl carbonate complex is below 100 ppm.
The invention also provides application of the low-moisture solid boron trifluoride methyl ethyl carbonate complex in the field of lithium batteries.
The invention provides a preparation method of a low-moisture solid boron trifluoride methyl ethyl carbonate complex, which comprises the following steps: mixing methyl ethyl carbonate and chloralkane to obtain a mixed solution; the mass ratio of the methyl ethyl carbonate to the chlorinated alkane is 1:1-6; introducing boron trifluoride gas into the mixed solution for complex reaction to obtain complex reaction feed liquid; under a closed condition, carrying out solid-liquid separation on the complex reaction feed liquid to obtain a low-moisture solid boron trifluoride methyl ethyl carbonate complex; the water content of the low-water solid boron trifluoride methyl ethyl carbonate complex is below 100 ppm. The methyl ethyl carbonate can be dissolved in chloralkane, and the chloralkane can dissolve the water in the complex, so that the boron trifluoride methyl ethyl carbonate complex is prepared by adopting chloralkane as a solvent based on the principle, and the water in the complex is effectively carried out by chloralkane during solid-liquid separation by strictly controlling the dosage of chloralkane, so that the solid boron trifluoride methyl ethyl carbonate complex with low water content is obtained; in the invention, the adding amount of chlorinated alkane is a key point of the process, and excessive adding amount of chlorinated alkane can lead to that boron trifluoride methyl ethyl carbonate complex is dissolved in chlorinated alkane, so that the yield of a solid complex product is greatly reduced, even a solid product cannot be obtained, the adding amount is too small, water cannot be effectively brought out, the water content of the product is higher, and the chlorinated alkane is not easy to discharge due to too small adding amount; in addition, the solid-liquid separation is carried out under the airtight condition, so that the influence of water in the air on the water content of the product can be avoided. Furthermore, if the method of directly introducing boron trifluoride gas is adopted to prepare the boron trifluoride methyl ethyl carbonate complex, 4N or 5N boron trifluoride gas is required to be adopted to reduce the water content of the product, the production cost is high, the method of the invention has lower requirement on the purity of the boron trifluoride gas, and industrial boron trifluoride gas is adopted, so that the production cost is low and the economic benefit is good.
The water content of the boron trifluoride methyl ethyl carbonate complex prepared by the method is less than 100ppm, can meet the requirement of the lithium battery field on the water content of production raw materials, can be used for synthesizing lithium battery electrolyte lithium salt, fills the application blank of the lithium battery field, and has wide prospect.
Drawings
FIG. 1 is a flow chart of a process for preparing a low-moisture solid boron trifluoride methyl ethyl carbonate complex in an embodiment of the invention.
Detailed Description
The invention provides a preparation method of a low-moisture solid boron trifluoride methyl ethyl carbonate complex, which comprises the following steps:
mixing methyl ethyl carbonate and chloralkane to obtain a mixed solution; the mass ratio of the methyl ethyl carbonate to the chlorinated alkane is 1:1-6;
introducing boron trifluoride gas into the mixed solution for complex reaction to obtain complex reaction feed liquid;
under a closed condition, carrying out solid-liquid separation on the complex reaction feed liquid to obtain a low-moisture solid boron trifluoride methyl ethyl carbonate complex; the water content of the low-water solid boron trifluoride methyl ethyl carbonate complex is below 100 ppm.
In the present invention, all raw material components are commercially available products well known to those skilled in the art unless specified otherwise.
The invention mixes methyl ethyl carbonate and chloralkane to obtain mixed solution. In the invention, the mass ratio of the methyl ethyl carbonate to the chlorinated alkane is 1:1-6, preferably 1:2-5, and more preferably 1:3-4; in the invention, the addition of the chlorinated alkane is less, so that the feed liquid is solid, the feeding is difficult, the addition is excessive, the product is dissolved in the liquid, the yield of the solid boron trifluoride methyl ethyl carbonate complex is reduced, the mass ratio is controlled within the range, and the higher yield can be ensured on the basis of easy feeding. In the present invention, the chlorinated alkane is preferably one or more of dichloromethane, 1-dichloroethane, 1, 2-dichloroethane and dichloropropane. The method has no special requirement on the mixing method, and the mixing is carried out uniformly under the stirring condition.
After the mixed solution is obtained, boron trifluoride gas is introduced into the mixed solution for complex reaction, so as to obtain complex reaction feed liquid. In the present invention, the complexation reaction has the following reaction formula:
C 4 H 8 O 3 +BF 3 ＝C 4 H 8 O 3· BF 3
in the present invention, the temperature of the complexing reaction is preferably-10 to 25 ℃, more preferably-5 to 20 ℃, still more preferably 0 to 15 ℃, and the time of the complexing reaction is preferably 3 to 24 hours, more preferably 5 to 20 hours, still more preferably 10 to 15 hours, the time of the complexing reaction being counted from the time when boron trifluoride gas is introduced. In the invention, the temperature of the complexation reaction is too low, which can lead to extremely slow complexation speed, the temperature of the complexation reaction is too high, and the methyl ethyl carbonate is easy to volatilize, so that the methyl ethyl carbonate becomes gas complexation, and forms solid to adhere to the wall of the reaction kettle, and the discharging can not be realized.
In the present invention, the molar ratio of the methylethyl carbonate to the boron trifluoride is preferably 1:0.95 to 1.05, more preferably 1:1.
In the present invention, the boron trifluoride gas is preferably industrial boron trifluoride gas, and the methyl ethyl carbonate is preferably battery grade methyl ethyl carbonate; the boron trifluoride gas is preferably introduced at a rate of 50g/h to 27kg/h, and in the embodiment of the present invention, the boron trifluoride gas is preferably introduced at a rate of 50 to 300g/h, more preferably 100 to 250g/h, in the case of laboratory preparation or pilot production, and in the case of mass production, the boron trifluoride gas and methyl ethyl carbonate are used in a large amount, and the boron trifluoride gas is preferably introduced at a rate of 5 to 27kg/h, more preferably 10 to 25kg/h, and in the embodiment of the present invention, the boron trifluoride gas is preferably introduced in 2 to 10h, more preferably 3 to 7h, and after the boron trifluoride gas is introduced, the reaction is preferably continued for 1 to 14h, more preferably 3 to 8h. In the invention, the air inlet rate of the boron trifluoride is too small, the complexing reaction is slow, the air inlet rate is too fast, the complexing reaction rapidly releases heat, the temperature of materials can be rapidly increased, the stable control of the reaction temperature is not facilitated, the air inlet rate of the boron trifluoride is preferably controlled within the range, the speed of the complexing reaction can be ensured, and the stable reaction temperature is ensured.
In the present invention, the complexing reaction is preferably carried out under stirring conditions, and the stirring rate is preferably 100 to 300r/min, more preferably 150 to 250r/min. In the invention, the stirring speed is too low, which is unfavorable for the complex reaction, and the stirring speed is not too high, which can cause liquid splashing and is unfavorable for crystallization; the stirring speed is preferably controlled within the range, so that the complex reaction is facilitated, and good precipitation of crystals is ensured. In the specific embodiment of the invention, after boron trifluoride gas is introduced, as the reaction proceeds, solids appear in the material, namely boron trifluoride methyl ethyl carbonate complex, and the obtained feed liquid is a solid-liquid mixture after the complexation reaction is completed.
After the complex reaction feed liquid is obtained, the complex reaction feed liquid is subjected to solid-liquid separation under a closed condition to obtain a low-moisture solid boron trifluoride methyl ethyl carbonate complex; the water content of the low-water solid boron trifluoride methyl ethyl carbonate complex is below 100 ppm. In the present invention, the solid-liquid separation method is preferably centrifugation; the invention has no special requirements on specific operation conditions of centrifugation, and can realize solid-liquid separation. In the invention, the liquid obtained by solid-liquid separation is chloralkane, and the chloralkane is preferably recycled after being recovered, so that the production cost is further reduced.
The invention also provides a low-moisture solid boron trifluoride methyl ethyl carbonate complex prepared by the preparation method. The water content of the low-water solid boron trifluoride methyl ethyl carbonate complex is 100ppm or less, preferably 80ppm or less, and more preferably 40 to 70ppm.
The invention also provides application of the low-moisture solid boron trifluoride methyl ethyl carbonate complex in the field of lithium batteries. The solid boron trifluoride methyl ethyl carbonate complex provided by the invention has low water content, can meet the requirement of synthesizing lithium battery electrolyte lithium salt, and has wide application prospect.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
FIG. 1 is a flow chart of a process for preparing a low-moisture solid boron trifluoride methyl ethyl carbonate complex in the embodiment of the invention, wherein methyl ethyl carbonate and chloralkane are proportionally put into a reaction kettle, the reaction kettle is cooled, then a certain amount of boron trifluoride gas is introduced for complexing, and the solid-liquid separation is carried out, so that a product is obtained, and the operation sequence of steps is shown in (1), (2) and (3) in FIG. 1.
Example 1
892.1g of methyl ethyl carbonate and 2676.0g of methylene dichloride are weighed and put into a reaction kettle, and stirring is started to uniformly mix. 582.6g of boron trifluoride gas is introduced according to the air inlet rate of 100g/h, the complexing reaction is carried out at the temperature of minus 5 ℃, and the stirring is carried out fully (the speed is 250 r/min) until the solid appears in the materials, and the total reaction is carried out for 10h.
The solid-liquid mixture obtained by the reaction was separated to obtain 1407.6g of a solid boron trifluoride ethyl methyl carbonate complex with a yield of 95.44%.
Example 2
500.7g of methyl ethyl carbonate and 1522.9g of methylene dichloride are weighed and put into a reaction kettle, and stirring is started to uniformly mix. 328.5g of boron trifluoride gas is introduced according to the air inlet rate of 50g/h, the complexing reaction is carried out at 5 ℃, and the stirring is carried out fully (the speed is 300 r/min) until the solid appears in the materials, and the total reaction is carried out for 10h.
The solid-liquid mixture obtained by the reaction was separated to obtain 805.4g of a solid boron trifluoride ethyl methyl carbonate complex with a yield of 97.13%.
Example 3
326.9g of methyl ethyl carbonate and 1107.3g of methylene dichloride are weighed and put into a reaction kettle, and stirring is started to uniformly mix. 211.0g of boron trifluoride gas is introduced according to the air inlet rate of 50g/h, the complexing reaction is carried out at 0 ℃, and the stirring is carried out fully (the speed is 100 r/min) until the solid appears in the materials, and the total reaction is carried out for 8h.
The solid-liquid mixture obtained by the reaction was separated to obtain 521.0g of a solid boron trifluoride ethyl methyl carbonate complex with a yield of 96.86%.
Example 4
461.3g of methyl ethyl carbonate and 1401.0g of 1, 1-dichloroethane are weighed and put into a reaction kettle, and stirring is started to uniformly mix. 306.6g of boron trifluoride gas is introduced according to the air inlet rate of 100g/h, the complexing reaction is carried out at 15 ℃, and the stirring is carried out fully (the speed is 200 r/min) until the solid appears in the materials, and the total reaction is carried out for 10h.
The solid-liquid mixture was separated to obtain 735.5g of solid boron trifluoride methyl ethyl carbonate complex with a yield of 95.78%.
Example 5
Other conditions were the same as in example 1, except that the amount of methylene chloride was adjusted to 892.1g.
Example 6
Other conditions were the same as in example 1, except that the amount of methylene chloride was adjusted to 5352.6g.
Comparative example 1
Otherwise, the conditions were the same as in example 1, and the amount of methylene dichloride was only 600g, and the result showed that the feed liquid was solid, and it was difficult to discharge, and the product was stuck to the wall of the reactor during the discharge, resulting in a lower yield.
Comparative example 2
Otherwise, the conditions were the same as in example 1, and the amount of methylene chloride was adjusted to 6000g only, and as a result, it was revealed that most of the boron trifluoride methyl ethyl carbonate complex was dissolved in the solvent, and that only a very small amount of solid product was present in the product solution, and that the yield of the solid boron trifluoride methyl ethyl carbonate complex was extremely low.
The solid boron trifluoride methylethyl carbonate complexes obtained in examples 1 to 6 and comparative example 1 were examined for moisture and boron trifluoride content, and the results obtained are shown in Table 1.
TABLE 1 test results of solid boron trifluoride methyl ethyl carbonate complex obtained in examples 1-4
As can be seen from the data in Table 1, the solid boron trifluoride methyl ethyl carbonate complex prepared by the invention has low water content and high yield; when the using amount of dichloromethane is small (comparative example 1), water cannot be effectively carried out, the water content of the obtained product is high, and the yield is reduced because part of solid products adhere to the kettle wall during discharging; in the case of using a large amount of methylene chloride (comparative example 2), the solid product is dissolved in the solvent, resulting in extremely low yield of the product and waste of a large amount of methylene chloride.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (3)
1. The preparation method of the low-moisture solid boron trifluoride methyl ethyl carbonate complex is characterized by comprising the following steps:
mixing methyl ethyl carbonate and chloralkane to obtain a mixed solution; the mass ratio of the methyl ethyl carbonate to the chlorinated alkane is 1:1-6;
introducing boron trifluoride gas into the mixed solution for complex reaction to obtain complex reaction feed liquid;
under a closed condition, carrying out solid-liquid separation on the complex reaction feed liquid to obtain a low-moisture solid boron trifluoride methyl ethyl carbonate complex; the water content of the low-water solid boron trifluoride methyl ethyl carbonate complex is below 100 ppm;
the chlorinated alkane is one or more of dichloromethane, 1 dichloroethane, 1,2 dichloroethane and dichloropropane; the molar ratio of the methyl ethyl carbonate to the boron trifluoride is 1:0.95-1.05; the temperature of the complex reaction is-10 to 25 ℃ and the time is 3 to 24 hours; the introducing rate of the boron trifluoride gas is 50 g/h-27 kg/h; the complexing reaction is carried out under the stirring condition, and the stirring speed is 100-300 r/min.
2. The production method according to claim 1, wherein the boron trifluoride gas is industrial boron trifluoride gas.
3. The method of claim 1, wherein the solid-liquid separation is centrifugation.
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