Method for preparing vinylene carbonate

Abstract

The present invention relates to a method for preparing vinylene carbonate, comprising: (1) providing a first material, wherein the first material comprises vinyl chloride carbonate, borohydride and a solvent S1 capable of dissolving vinyl chloride carbonate and the borohydride; (2) providing a second material, wherein the second material comprises triethylamine; (3) feeding the first material and the second material into a reaction zone of a reactor to react and form vinylene carbonate. The synthesis method provided by the present invention effectively improves the efficiency of the reaction and has outstanding economic value.

Description

Technical Field

[0001] The present invention relates to the field of chemical technology, and in particular to a method for preparing vinylene carbonate. Background Art

[0002] Vinylene carbonate, also known as 1,3-dioxolane-2-one or ethylene carbonate, is a colorless transparent liquid that can be used as a new organic film-forming additive and overcharge protection additive for lithium-ion batteries, and can also be used as a monomer for the preparation of polyvinyl carbonate. With the continuous expansion of the use of lithium-ion batteries, the technology of lithium-ion batteries is also constantly improving. Adding some additives to the electrolyte, which is the "blood" of lithium-ion batteries, can improve many performances of the battery. Among them, vinylene carbonate is an organic film-forming additive and overcharge protection additive in the electrolyte. It has good high and low temperature performance and anti-swelling function, which can increase the stability of the solvent, effectively inhibit the decomposition of the solvent, promote the formation of SEI film, and improve the cycle performance of the battery. However, due to the thermal sensitivity of vinylene carbonate itself, it is easy to decompose and free radical polymerization at high temperatures, making it difficult to achieve a high yield of vinylene carbonate.

[0003] Therefore, it is necessary to develop a new synthesis method of vinylene carbonate to solve the deficiencies of the prior art, thereby improving the yield of vinylene carbonate. Summary of the invention

[0004] In order to solve the problems existing in the prior art, the present invention provides a method for synthesizing vinylene carbonate. The method uses vinyl chloride carbonate and triethylamine as raw materials to synthesize vinylene carbonate.

[0005] In one aspect, the present invention provides a method for preparing vinylene carbonate, comprising:

[0006] (1) providing a first material, wherein the first material comprises ethylene chlorocarbonate, borohydride, and a solvent S1 capable of dissolving ethylene chlorocarbonate and the borohydride;

[0007] (2) providing a second material, wherein the second material comprises triethylamine;

[0008] (3) Feeding the first material and the second material into a reaction zone of a reactor to react and form vinylene carbonate.

[0009] In some embodiments of the present invention, the reaction temperature in the reaction zone of the reactor is set at 60-160° C. In some embodiments of the present invention, the reaction temperature in the reaction zone of the reactor is maintained at 60-160° C. for constant temperature reaction.

[0010] In some embodiments of the present invention, the borohydride comprises one or more of sodium borohydride, sodium cyanoborohydride, sodium tris(1,1,1,3,3,3-hexafluoroisopropoxy)borohydride, sodium tri-sec-butylborohydride, sodium triacetoxyborohydride, sodium trimethoxyborohydride, and sodium triethylborohydride.

[0011] In some embodiments of the present invention, the mass ratio of chloroethylene carbonate to borohydride in the first material is (4-1000):1, preferably (50-100):1.

[0012] In some embodiments of the present invention, the solvent S1 comprises one or more of tetrahydrofuran, chloroform, N,N-dimethylformamide, propylene carbonate, dimethyl carbonate, diethyl carbonate, and 2-methyltetrahydrofuran; and the mass concentration of chloroethylene carbonate in the first material is in the range of 10-30%.

[0013] In some embodiments of the present invention, the second material comprises a solvent S2 capable of dissolving triethylamine.

[0014] In some embodiments of the present invention, the solvent S2 comprises one or more of tetrahydrofuran, chloroform, N,N-dimethylformamide, propylene carbonate, dimethyl carbonate, diethyl carbonate, and 2-methyltetrahydrofuran; and the mass concentration of triethylamine in the second material is in the range of 10-50%.

[0015] In some embodiments of the present invention, the molar ratio of ethylene chlorocarbonate in the first material to triethylamine in the second material is 1:(1-4).

[0016] In some embodiments of the present invention, the residence time of the reaction in the reaction zone is 1 to 300 minutes.

[0017] In some embodiments of the present invention, the reactor is a continuous flow reactor, and the flow rate of the first material entering the reaction zone is 10-400 g / min, and the flow rate of the second material entering the reaction zone is 10-400 g / min.

[0018] In some embodiments of the present invention, the reactor is selected from a tank reactor, a tubular reactor, a microchannel reactor, a high-throughput reactor, and a flow reactor.

[0019] In some embodiments of the present invention, the reactor may be a reactor combination in which the number of reactors is greater than 1, and the types of reactors selected in the reactor combination may be the same or different; when reactions occur in the reactors in the reactor combination, the reaction temperatures of the reaction zones of the reactors may be the same or different.

[0020] In the present invention, the method achieves the following excellent technical effects: the present invention adopts borohydride as an additive in the reaction of synthesizing vinylene carbonate, which greatly improves the yield of the reaction: compared with the reaction without adding borohydride, the yield after adding borohydride is increased from 55-60% to as high as 94%. At the same time, the selectivity of the reaction is also improved to a certain extent, from 80%-85% to 90-95%. In addition, when a microchannel reactor is used for the reaction, the total residence time of the reaction is also greatly shortened. Therefore, the synthesis method provided by the present invention effectively improves the efficiency of the reaction and has outstanding economic value. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 is a schematic diagram of a Corning G1-glass reactor used in some embodiments of the present invention.

[0022] Figure 2 is a schematic diagram of a reactor assembly used in some embodiments of the present invention.

[0023] Figure 3 is a schematic diagram of a Corning G5-SiC reactor used in some embodiments of the present invention.

[0024] Description of Reference Numerals

[0025] 10, 20, and 40 are microchannel reactor modules.

[0026] 11, 12, 21, 22, 31, 41 and 42 are the feed ports of the reactor.

[0027] 13, 23, 32 and 43 are the discharge ports of the microchannel reactor. DETAILED DESCRIPTION

[0028] The technical solution of the present invention is now described in conjunction with specific embodiments. It should be understood that the following examples are only used to illustrate the present invention and are not used to limit the scope of the present invention.

[0029] In the present invention, the reaction formula for synthesizing vinylene carbonate is as follows:

[0030]

[0031] In the present invention, the method for synthesizing vinylene carbonate may comprise the following steps:

[0032] (1) providing a first material, wherein the first material comprises ethylene chlorocarbonate, borohydride, and a solvent S1 capable of dissolving ethylene chlorocarbonate and the borohydride;

[0033] (2) providing a second material, wherein the second material comprises triethylamine;

[0034] (3) Feeding the first material and the second material into a reaction zone of a reactor to react and form vinylene carbonate.

[0035] In some embodiments of the present invention, the reaction temperature in the reaction zone of the reactor is set at 60-160°C, 60-150°C, 60-140°C, 60-130°C, 60-120°C, 60-110°C, 60-100°C, 60-90°C, 60-80°C, 60-70°C, 70-160°C, 70-150°C, 70-140°C, 70-130°C, 70-120°C, 70-110°C, 70-100°C, 70-90°C, 70-80°C, 80-160°C, 80-150°C, 80-140°C, 80-130°C, 80-120°C, 80-110°C, 80-100°C, 80-90°C, 90-160°C, 90 -150℃, 90-140℃, 90-130℃, 90-120℃, 90-110℃, 90-100℃, 100-160℃, 100-150℃, 100-140℃, 100-130℃, 100-120℃, 100-110℃, 110-160℃, 110-150℃, 110-140℃, 110-130℃, 110-120℃, 120-160℃, 120-150℃, 120-140℃, 120-130℃, 130-160℃, 130-150℃, 130-140℃, 140-160℃, 140-150℃, 150-160℃, and keep constant temperature reaction within this temperature range.

[0036] In some embodiments of the present invention, the borohydride comprises one or more of sodium borohydride, sodium cyanoborohydride, sodium tris(1,1,1,3,3,3-hexafluoroisopropoxy)borohydride, sodium tri-sec-butylborohydride, sodium triacetoxyborohydride, sodium trimethoxyborohydride, and sodium triethylborohydride.

[0037] In some embodiments of the present invention, the mass ratio of chloroethylene carbonate to borohydride in the first material is (4-1000):1, preferably (50-100):1.

[0038] In some embodiments of the present invention, the solvent S1 comprises one or more of tetrahydrofuran, chloroform, N,N-dimethylformamide, propylene carbonate, dimethyl carbonate, diethyl carbonate, and 2-methyltetrahydrofuran; the mass concentration of chloroethylene carbonate in the first material is 10-30%, 10-20% and 20-30%.

[0039] In some embodiments of the present invention, the second material comprises a solvent S2 capable of dissolving triethylamine.

[0040] In some embodiments of the present invention, the solvent S2 comprises one or more of tetrahydrofuran, chloroform, N,N-dimethylformamide, propylene carbonate, dimethyl carbonate, diethyl carbonate, and 2-methyltetrahydrofuran; the mass concentration of triethylamine in the second material is 10-50%, 10-40%, 10-30%, 10-20%, 20-50%, 20-40%, 20-30%, 30-50%, 30-40%, and 40-50%.

[0041] In some embodiments of the present invention, the molar ratio of ethylene chlorocarbonate in the first material to triethylamine in the second material is 1:(1-4).

[0042] In some embodiments of the present invention, the residence time of the reaction in the reaction zone is 1 to 300 minutes.

[0043] In some embodiments of the present invention, the reactor is a continuous flow reactor, and the flow rate of the first material entering the reaction zone is 10-400 g / min, and the flow rate of the second material entering the reaction zone is 10-400 g / min.

[0044] In some embodiments of the present invention, the reactor is selected from a tank reactor, a tubular reactor, a microchannel reactor, a high-throughput reactor, and a flow reactor.

[0045] In some embodiments of the present invention, the reactor may be a reactor combination in which the number of reactors is greater than 1, and the types of reactors selected in the reactor combination may be the same or different; when reactions occur in the reactors in the reactor combination, the reaction temperatures of the reaction zones of the reactors may be the same or different.

[0046] In some embodiments of the present invention, the reactor may be a reactor combination having two reactors, and the types of reactors selected in the reactor combination may be the same or different; when reactions occur in the reactors in the reactor combination, the reaction temperatures of the reaction zones of the reactors may be the same or different.

[0047] The term "borohydride" as used herein refers to a class of compounds containing a borohydride anion (BH 4- ) inorganic or organic compounds. The "borohydride" described herein includes, but is not limited to, sodium borohydride, sodium cyanoborohydride, sodium tris(1,1,1,3,3,3-hexafluoroisopropoxy)borohydride, sodium tri-sec-butylborohydride, sodium triacetoxyborohydride, sodium trimethoxyborohydride, sodium triethylborohydride.

[0048] The "dissolution" mentioned in this article refers to the process in which two or more substances are mixed to form a uniform phase in a state. It can be a process in which a solid and a liquid are mixed to form a uniform phase in a molecular state, or it can be a process in which a liquid and another liquid are mixed to form a uniform phase in a molecular state.

[0049] The "reaction zone" as used herein refers to the area in the reactor where the chemical reaction takes place.

[0050] The "reaction temperature" described herein refers to the temperature at which the reactants in the reaction zone are in contact.

[0051] The method described herein can be carried out under isothermal or non-isothermal conditions. The isothermal method described herein means that the reaction temperature varies within the range of ±5°C (preferably ±4, 3, 2, 0.5°C) of the set temperature value.

[0052] The "reaction residence time" described herein = total volume flow rate of reaction materials (ml / min) / internal volume of reactor (ml).

[0053] The "reactor combination" described herein includes more than one reactor, and the types of the reactors can be the same or different and connected in series and / or in parallel.

[0054] The method described herein can be carried out in a continuous reaction, a semi-batch reaction or a batch reaction.

[0055] The methods described herein can be carried out at normal pressure or elevated pressure. The pressure in any reaction zone of the methods described herein can be 0.1-5 MPa, preferably 0.1-2 MPa, for example, 0.1 MPa, 0.2 MPa, 0.3 MPa, 0.4 MPa, 0.5 MPa, 0.6 MPa, 0.7 MPa, 0.8 MPa, 0.9 MPa or 1.0 MPa.

[0056] Selectivity as described herein = target product formation / reactant consumption

[0057] Yield as described herein = amount of target product generated / total amount of reactants fed

[0058] In some embodiments of the present invention, a microchannel reactor of Corning is used for the reaction, and the microchannel reaction zone module includes but is not limited to Corning G1-glass reactor and Corning G5-SiC reactor. In some embodiments of the present invention, a kettle or tubular reactor is used for the reaction.

[0059] In some specific embodiments of the present invention, the first material and the second material are sampled by a sampling device, and the sampling device includes but is not limited to sampling by pump, extrusion, osmosis, injection, etc. In some embodiments, the delivery described herein is delivered by a pump, such as a conventional plunger pump in the art.

[0060] In some specific embodiments of the present invention, a preheating device is also used to preheat the first material and the second material. The preheating device includes a heating device commonly used in the chemical industry, including a preheating pipeline and an insulated storage tank.

[0061] In some specific embodiments of the present invention, a heat exchange device is also used to control the temperature of the reactor. The heat exchange device may include at least one heat exchange passage through which other liquid or gaseous media pass, which is arranged adjacent to the reaction passage of the reactor, and the temperature of the reactants in the reaction passage is controlled by controlling the temperature of the liquid or gaseous medium in the heat exchange passage.

[0062] In some specific embodiments of the present invention, a separation device is further used to separate the product obtained after the first material and the second material react, and the separation device includes but is not limited to a separation tank and a liquid separator. The "separation" described herein refers to separating and collecting components with different properties using methods commonly used in the chemical industry.

[0063] In some specific embodiments of the present invention, a detection device is also used to analyze the reaction product, and the detection device includes but is not limited to a gas chromatograph and a liquid chromatograph.

[0064] Figure 1 Corning G1-glass microchannel reactor used in some specific embodiments of the present invention includes a microchannel reactor module 10, a heat exchanger device (not marked in the figure) and an injection device (not marked in the figure). The heat exchange device includes a heat exchange passage adjacent to the reaction passage of the microchannel reactor module, which is connected to other liquid or gaseous media, and a control device located outside that can keep the medium in the heat exchange passage circulating and control its temperature. The injection device includes a plunger pump and a matching injection frame, which can pump the reactants into the microchannel reactor module. The first material is introduced into the microchannel reactor module 10 from the feed port 11, and the second material flow is introduced into the microchannel reactor module 10 from the feed port 12. After the reaction is completed, the reaction product flows out of the reactor from the discharge port 13.

[0065] Figure 2The reactor combination used in some specific embodiments of the present invention includes a Corning G1-glass microchannel reactor module 20 and a tubular reactor module 30, and also includes a heat exchanger device (not marked in the figure) and an injection device (not marked in the figure). The heat exchange device includes a heat exchange passage with other liquid or gaseous media arranged adjacent to the reaction passages of the microchannel reactor module and the tubular reactor module, and a control device located outside that can keep the medium in the heat exchange passage circulating and control its temperature. The injection device includes a plunger pump and a matching injection frame, which can pump the reactants into the microchannel reactor module. The first material is introduced into the microchannel reactor module 20 from the feed port 21, and the second material flow flows into the microchannel reactor module 20 from the feed port 22. The reactants then flow out from the discharge port 23 and enter the tubular reactor module 30 from the feed port 31, and the product then flows out of the reactor from the discharge port 32.

[0066] Figure 3 Corning G5-SiC reactor used in some specific embodiments of the present invention. It includes a microchannel reactor module 40, a heat exchanger device (not marked in the figure) and an injection device (not marked in the figure). The heat exchange device includes a heat exchange passage adjacent to the reaction passage of the microchannel reactor module through which other liquid or gaseous media pass, and a control device located outside that can keep the medium in the heat exchange passage circulating and control its temperature. The injection device includes a plunger pump and a matching injection frame, which can pump the reactants into the microchannel reactor module. The first material is introduced into the microchannel reactor module 40 from the feed port 41, and the second material flow is introduced into the microchannel reactor module 40 from the feed port 42. After the reaction is completed, the reaction product flows out of the reactor from the discharge port 43.

[0067] Unless otherwise specified, the raw materials used in the present invention are all industrial grade raw materials. In the embodiment, the raw material chloroethylene carbonate can be purchased from Shanghai Bid Pharmaceutical Technology Co., Ltd., with a purity of ≥80%; propylene carbonate can be purchased from TCI (Shanghai) Chemical Industry Development Co., Ltd., with a purity of ≥99%; triethylamine can be purchased from Shanghai Yien Chemical Technology Co., Ltd., with a purity of ≥99%; diethyl carbonate can be purchased from Shanghai Aladdin Biochemical Technology Co., Ltd., with a purity of ≥99%; dimethyl carbonate can be purchased from Shanghai Aladdin Biochemical Technology Co., Ltd., with a purity of ≥99%; sodium cyanoborohydride is purchased from Shanghai Mairui Chemical Technology Co., Ltd., with a purity of ≥95%; sodium triacetoxyborohydride is purchased from Jiangsu Aikang Biomedicine Research and Development Co., Ltd., with a purity of ≥97%.

[0068] Example 1

[0069] Vinyl chloride carbonate (300 g), sodium triacetoxyborohydride (6 g), and dimethyl carbonate (900 g) were added to a tank reactor, mixed and dissolved, and heated. When heated to 60° C., triethylamine (401.5 g) was added to the tank reactor, and then the temperature was raised to maintain the reaction temperature at about 67° C. The reaction was maintained at this temperature for 5 hours. After the reaction was completed, the reaction product was filtered with a Buchner funnel after cooling to room temperature, and the filtrate was washed with 500 g of dimethyl carbonate. After quantitative analysis of the vinylene carbonate in the product, it was calculated that the selectivity of the reaction was 93%, and the yield was 89%.

[0070] Example 2

[0071] Vinyl chloride carbonate (300 g), sodium cyanoborohydride (6 g), and dimethyl carbonate (900 g) were added to a tank reactor, mixed, dissolved, and heated. When heated to 60° C., triethylamine (803 g) was added to the tank reactor, and then the temperature was raised to maintain the reaction temperature at about 67° C. The reaction was maintained at this temperature for 5 hours. After the reaction was completed, the reaction product was filtered with a Buchner funnel after cooling to room temperature, and the filtrate was washed with 500 g of dimethyl carbonate. After quantitative analysis of the vinylene carbonate in the product, it was calculated that the selectivity of the reaction was 95%, and the yield was 93.5%.

[0072] Example 3

[0073] This embodiment adopts Figure 1 The microchannel reactor shown in the figure is reacted. Vinyl chloride (250g), sodium triacetoxyborohydride (0.25g), and propylene carbonate (2500g) are mixed and dissolved to form a first material, and triethylamine (200g) is dissolved in diethyl carbonate (2000g) to form a second material. The first material and the second material are continuously pumped into the microchannel reactor by a plunger pump, wherein the flow rate of the first material is 20 g / min, the flow rate of the second material is 13.4 g / min, the reaction temperature is 60°C, and the residence time of the reaction is 5 minutes. The product generated by the reaction is quantitatively detected by an Agilent 6890GC gas chromatograph, and the product concentration is quantitatively measured by peak area. After analysis, the selectivity of the reaction is 92%, and the yield is 89%.

[0074] Example 4

[0075] This embodiment adopts Figure 1The microchannel reactor shown in the figure is reacted. Vinyl chloride (250g), sodium cyanoborohydride (0.25g), and propylene carbonate (1250g) are mixed and dissolved to form a first material, and triethylamine (200g) is dissolved in diethyl carbonate (200g) to form a second material. The first material and the second material are continuously pumped into the microchannel reactor by a plunger pump, wherein the flow rate of the first material is 50 g / min, the flow rate of the second material is 26.8 g / min, the reaction temperature is 90°C, and the residence time of the reaction is 3.5 minutes. The product generated by the reaction is quantitatively detected by an Agilent 6890GC gas chromatograph, and the product concentration is quantitatively measured by peak area. After analysis, the selectivity of the reaction is 95%, and the yield is 94%.

[0076] Example 5

[0077] This embodiment adopts Figure 1 The microchannel reactor shown in the figure is reacted. Vinyl chloride (250g), sodium cyanoborohydride (0.25g), and propylene carbonate (1250g) are mixed and dissolved to form a first material, and triethylamine (200g) is dissolved in diethyl carbonate (200g) to form a second material. The first material and the second material are continuously pumped into the microchannel reactor by a plunger pump, wherein the flow rate of the first material is 50 g / min, the flow rate of the second material is 53.6 g / min, the reaction temperature is 160°C, and the residence time of the reaction is 0.5 minute. The product generated by the reaction is quantitatively detected by an Agilent 6890GC gas chromatograph, and the product concentration is quantitatively measured by peak area. After analysis, the selectivity of the reaction is 93%, and the yield is 90%.

[0078] Example 6

[0079] This embodiment adopts Figure 2 The reactor combination of the microchannel reactor+tubular reactor shown in the figure reacts. After ethylene chlorocarbonate (1000g) and sodium borohydride (10g) are dissolved in propylene carbonate (3000g), the first material is formed, and triethylamine (1000g) is dissolved in diethyl carbonate (9kg) to form the second material. The first material and the second material are continuously pumped into the microchannel reactor by a plunger pump, wherein the flow velocity of the first material is 40 grams per minute, and the flow velocity of the second material is 15 grams per minute, and the reaction temperature in the microchannel reactor is 150°C. After the reactant flows out from the outlet of the microchannel reactor, it flows into the tubular reactor subsequently to react, and the reaction temperature in the tubular reactor is 150°C, and the total residence time of the reaction in the two reactors is 2.5min. The product generated by the reaction is quantitatively detected by an Agilent 6890GC gas chromatograph, with the peak area quantitative product concentration. After analysis, the selectivity of the reaction is 95%, and the yield is 93%.

[0080] Example 7

[0081] This embodiment adopts Figure 3 The Corning G5-SiC microchannel reactor shown in the figure is used for reaction. Ethylene chlorocarbonate (1000g) and sodium borohydride (10g) are dissolved in propylene carbonate (3000g) to form a first material, and triethylamine (1000g) is dissolved in diethyl carbonate (5kg) to form a second material. The first material and the second material are continuously pumped into the microchannel reactor by a plunger pump, wherein the flow rate of the first material is 400 g / min, the flow rate of the second material is 150 g / min, the reaction temperature in the reactor is 150°C, and the residence time of the reaction is 2.5min. The product generated by the reaction is quantitatively detected by an Agilent 6890GC gas chromatograph, and the product concentration is quantitatively measured by peak area. After analysis, the selectivity of the reaction is 95%, and the yield is 93%.

[0082] Comparative Example 1

[0083] Vinyl chloride (300 g) and dimethyl carbonate (900 g) were added to a tank reactor, mixed and dissolved, and heated. When the reaction temperature reached 60° C., triethylamine (401.5 g) was added to the tank reactor, and the temperature was subsequently raised to maintain the reaction temperature at about 67° C. The reaction was maintained at this temperature for 5 hours. After the reaction was completed, the reaction product was filtered with a Buchner funnel after cooling to room temperature, and the filtrate was washed with 500 g of dimethyl carbonate. After quantitative analysis of the vinylene carbonate in the product, it was calculated that the selectivity of the reaction was 85%, and the yield was 60%.

[0084] Comparative Example 2

[0085] This embodiment adopts Figure 1 The microchannel reactor shown in the figure is used for reaction. Vinyl chloride (250g), sodium cyanoborohydride (0.25g), and propylene carbonate (2500g) are mixed and dissolved to form a first material, and triethylamine (200g) is dissolved in diethyl carbonate (2000g) to form a second material. The first material and the second material are continuously pumped into the microchannel reactor by a plunger pump, wherein the flow rate of the first material is 20 g / min, the flow rate of the second material is 13.4 g / min, the reaction temperature is 160°C, and the residence time of the reaction is 5 minutes. The product generated by the reaction is quantitatively detected by an Agilent 6890GC gas chromatograph, and the product concentration is quantitatively measured by peak area. After analysis, the selectivity of the reaction is 80%, and the yield is 55%.

Claims

1. A method for preparing vinylene carbonate, the method comprising: (1) providing a first material, wherein the first material comprises ethylene chlorocarbonate, borohydride, and a solvent S1 capable of dissolving ethylene chlorocarbonate and the borohydride; (2) providing a second material, wherein the second material comprises triethylamine; (3) feeding the first material and the second material into a reaction zone of a reactor to react and form vinylene carbonate; Wherein, the borohydride is selected from one or more of sodium borohydride, sodium cyanoborohydride, sodium tri(1,1,1,3,3,3-hexafluoroisopropoxy)borohydride, sodium tri-sec-butylborohydride, sodium triacetoxyborohydride, sodium trimethoxyborohydride and sodium triethylborohydride.

2. The method according to claim 1, characterized in that The reaction temperature in the reaction zone of the reactor was set at 60-160°C.

3. The method according to claim 1, characterized in that: The mass ratio of ethylene chlorocarbonate to borohydride in the first material is (4-1000):

1.

4. The method according to claim 1, characterized in that: The mass ratio of ethylene chlorocarbonate to borohydride in the first material is (50-100):

1.

5. The method according to claim 1, characterized in that The solvent S1 is selected from one or more of tetrahydrofuran, chloroform, N,N-dimethylformamide, propylene carbonate, dimethyl carbonate, diethyl carbonate, and 2-methyltetrahydrofuran; the mass concentration of chloroethylene carbonate in the first material is in the range of 10-30%.

6. The method according to claim 1, characterized in that The second material comprises a solvent S2 capable of dissolving triethylamine.

7. The method according to claim 6, characterized in that The solvent S2 is selected from one or more of tetrahydrofuran, chloroform, N,N-dimethylformamide, propylene carbonate, dimethyl carbonate, diethyl carbonate, and 2-methyltetrahydrofuran; and the mass concentration of triethylamine in the second material is in the range of 10-50%.

8. The method according to claim 1, characterized in that The molar ratio of ethylene chlorocarbonate in the first material to triethylamine in the second material is 1:(1-4).

9. The method according to any one of claims 1 to 8, characterized in that: The residence time of the reaction in the reactor is 1-300 minutes.

10. The method according to any one of claims 1 to 8, characterized in that: The reaction is carried out in a continuous reaction mode, and the flow rate of the first material entering the reaction zone is 10-400 g / min, and the flow rate of the second material entering the reaction zone is 10-400 g / min.

11. The method according to any one of claims 1 to 8, wherein the reactor is selected from a tank reactor, a tubular reactor, a microchannel reactor, a high-throughput reactor, and a flow reactor.

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