Preparation method of mannitol carbonate sulfate

Abstract

The invention provides a preparation method of mannitol carbonic acid sulfate, mannitol and dimethyl carbonate are used as starting raw materials to prepare mannitol carbonic acid sulfate, a target compound is obtained through ester exchange, cyclization and oxidation reaction, the raw materials are low in price and easy to obtain, the reaction operation is simple and convenient, the yield of the obtained product is 81% or above, the purity is 99.6% or above, and the method is suitable for industrial production. The method is suitable for industrial production.

Description

Technical Field

[0001] The present invention relates to the technical field of organic synthesis, in particular to a method for preparing mannitol carbonate sulfate. Background Art

[0002] The lithium-ion battery industry is developing towards higher voltage and energy density to meet the demands for longer battery life and higher performance in electric vehicles and energy storage. However, this also poses severe challenges to the stability, safety, and service life of electrolytes. Electrolyte additives play a crucial role in lithium-ion batteries, optimizing battery performance, improving safety, and extending battery life.

[0003] Carbonate compounds and cyclic sulfate compounds are widely used in lithium batteries or electrolyte additives. However, traditional carbonate compounds (such as EC and DMC) have limited antioxidant capacity, are prone to decomposition under high pressure or high temperature, and are prone to crystallization and precipitation at low temperatures, resulting in a decrease in the ionic conductivity of the electrolyte. These inherent disadvantages make it difficult to meet the requirements of high-voltage, high-energy-density batteries. Cyclic sulfates have outstanding performance in terms of interfacial stability and high-voltage compatibility. They can be preferentially oxidized and decomposed on the surface of high-voltage positive electrodes to form a dense cathode electrolyte interface (CEI) film, inhibiting the continued decomposition of the electrolyte and significantly improving the battery's cycling stability.

[0004] CN118652247A discloses a process for synthesizing bisulfate carbonate, which uses sorbitol and sulfonyl chloride as raw materials, reacts at low temperature under base catalysis to generate alcohol sulfate, which is then reacted with triphosgene to prepare bisulfate carbonate. This process is carried out entirely under low temperature conditions, and the raw materials contain highly toxic substances, making the operation dangerous and posing a significant hazard to operators and the environment. It does not conform to green chemistry, and the overall reaction yield is only 68-78%, which is a relatively low yield.

[0005] CN119192165A discloses a process for synthesizing cyclic carbonate-sulfate esters. The process uses mannitol, dimethyl carbonate, and N,N'-sulfonyldiimidazole as raw materials, reacts with an inorganic alkaline substance as a catalyst, and requires multiple organic solvent crystallization and purification steps to prepare the cyclic carbonate-sulfate ester. The process is complex to operate, the raw materials are expensive, and the product yield is low. The production cost is high and is not suitable for industrial production.

[0006] CN118307531B discloses a process for preparing mannitol carbonate sulfate using mannitol and dimethyl carbonate as raw materials, reacting under base catalysis and high pressure conditions, and then oxidizing with thionyl chloride and sodium hypochlorite. This process involves high-pressure reaction, dangerous operation, and high production costs, making it unsuitable for industrial production.

[0007] Therefore, developing a method for preparing mannitol carbonate sulfate with high yield, high purity and simple reaction operation is a technical problem to be solved urgently in this field. Summary of the Invention

[0008] In response to the shortcomings of the prior art, the present invention provides a method for preparing mannitol sulfate carbonate. The method uses inexpensive and readily available raw materials to obtain the target compound through transesterification, cyclization, and oxidation reactions. The method has the characteristics of high yield, high purity, and simple operation, making it suitable for industrial production.

[0009] To achieve this object, the present invention adopts the following technical solutions:

[0010] In a first aspect, the present invention provides a method for preparing mannitol sulfate carbonate, the method comprising the following steps:

[0011] (1) Mannitol is reacted with dimethyl carbonate to obtain compound 1, and the reaction formula is shown below:

[0012]

[0013] (2) Compound 1 is reacted with thionyl chloride to obtain compound 2. The reaction formula is as follows:

[0014]

[0015] (3) Compound 2 is reacted with an aqueous sodium hypochlorite solution to obtain compound 3, as shown in the following reaction formula:

[0016]

[0017] The invention uses mannitol and dimethyl carbonate as starting raw materials to prepare mannitol carbonate sulfate. The raw materials are cheap and easy to obtain, and the reaction operation is simple. The yield of the obtained product is above 81%, the purity is above 99.6%, and the product is suitable for industrial production.

[0018] The following are preferred technical solutions of the present invention, but are not intended to limit the technical solutions provided by the present invention. Through the following preferred technical solutions, the objectives and beneficial effects of the present invention can be better achieved and realized.

[0019] Preferably, in step (1), the reaction is carried out in a solvent.

[0020] Preferably, in step (1), the solvent includes a non-aqueous solvent.

[0021] Preferably, in step (1), the non-aqueous solvent comprises any one or a combination of at least two of acetonitrile, 1,2-dichloroethane, ethanol, carbon tetrachloride or benzene, more preferably acetonitrile.

[0022] Preferably, in step (1), the reaction is carried out in the presence of a catalyst.

[0023] Preferably, in step (1), the catalyst comprises an organic base catalyst.

[0024] Preferably, in step (1), the organic base catalyst comprises any one or a combination of at least two of 1,5,7-triazabicyclo[4.4.0]decene-5-ene, 1,8-diazabispiro[5.4.0]undec-7-ene, triethylamine, imidazole or 4-dimethylaminopyridine, and is further preferably 1,5,7-triazabicyclo[4.4.0]decene-5-ene or 1,8-diazabispiro[5.4.0]undec-7-ene.

[0025] Preferably, the molar ratio of mannitol to the organic base catalyst is 1:(0.01-0.04), for example, 1:0.01, 1:0.02, 1:0.03 or 1:0.04, and more preferably 1:(0.015-0.025).

[0026] Preferably, in step (1), the molar ratio of mannitol to dimethyl carbonate is 1:(1-1.15), for example, it can be 1:1, 1:1.05, 1:1.10 or 1:1.15, and more preferably 1:(1.05-1.10).

[0027] Preferably, in step (1), the reaction temperature is 65-80°C, for example, 65°C, 68°C, 71°C, 74°C, 77°C or 80°C, and more preferably 70-75°C.

[0028] Preferably, in step (1), the reaction time is 8 to 12 hours, for example, 8 hours, 9 hours, 10 hours, 11 hours or 12 hours, and more preferably 10 to 11 hours.

[0029] Preferably, in step (2), the reaction is carried out in a solvent.

[0030] Preferably, in step (2), the solvent includes a non-aqueous solvent.

[0031] Preferably, in step (2), the non-aqueous solvent comprises any one or a combination of at least two of 1,2-dichloroethane, acetonitrile, carbon tetrachloride, toluene or xylene, and more preferably 1,2-dichloroethane.

[0032] Preferably, the molar ratio of compound 1 to thionyl chloride is 1:(2-2.7), for example, 1:2, 1:2.2, 1:2.4, 1:2.6 or 1:2.7, and more preferably 1:(2-2.5).

[0033] Preferably, in step (2), the reaction temperature is 70-85°C, for example, 70°C, 73°C, 76°C, 79°C, 82°C or 85°C, and more preferably 75-80°C.

[0034] Preferably, in step (2), the reaction time is 2 to 4 hours, for example, 2 hours, 2.5 hours, 3 hours, 3.5 hours or 4 hours, and more preferably 2.5 to 3 hours.

[0035] Preferably, in step (3), the reaction is carried out in a solvent.

[0036] Preferably, in step (3), the solvent includes a non-aqueous solvent.

[0037] Preferably, in step (3), the non-aqueous solvent comprises any one or a combination of at least two of dichloromethane, 1,2-dichloroethane, acetonitrile, toluene, xylene or dimethyl carbonate, more preferably a combination of dichloromethane and acetonitrile.

[0038] Preferably, in step (3), the reaction is carried out in the presence of a catalyst.

[0039] Preferably, in step (3), the catalyst comprises an aqueous solution of ruthenium trichloride.

[0040] Preferably, in step (3), the mass fraction of the ruthenium trichloride aqueous solution is 1-5%, for example, it can be 1%, 2%, 3%, 4% or 5%.

[0041] Preferably, in step (3), the molar ratio of compound 2 to the catalyst is 1:(0.0001-0.005), for example, it can be 1:0.0001, 1:0.001, 1:0.002, 1:0.003, 1:0.004 or 1:0.005, and more preferably 1:(0.0015-0.003).

[0042] Preferably, the molar ratio of the compound 2 to the sodium hypochlorite aqueous solution is 1:(2-4), for example, it can be 1:2, 1:2.5, 1:3, 1:3.5 or 1:4, and more preferably 1:(2.5-3).

[0043] Preferably, the mass fraction of the sodium hypochlorite aqueous solution is 8-12%, for example, 8%, 9%, 10%, 11% or 12%.

[0044] Preferably, in step (3), the reaction temperature is 10-25°C, for example, 10°C, 13°C, 16°C, 19°C, 22°C or 25°C, and more preferably 15-20°C.

[0045] Preferably, the reaction time is 0.5 to 2 h, for example, 0.5 h, 1 h, 1.5 h or 2 h, and more preferably 1 to 1.5 h.

[0046] As a preferred technical solution of the present invention, the preparation method of mannitol carbonate sulfate specifically comprises:

[0047] (1) Mannitol and dimethyl carbonate are reacted in a solvent in the presence of a catalyst at 65-80° C. for 8-12 hours to obtain compound 1;

[0048] The catalyst includes an organic base catalyst;

[0049] The organic base catalyst includes any one or a combination of at least two of 1,5,7-triazabicyclo[4.4.0]decene-5-ene, 1,8-diazobispiro[5.4.0]undec-7-ene, triethylamine, imidazole or 4-dimethylaminopyridine;

[0050] The molar ratio of mannitol to organic base catalyst is 1:(0.01-0.04);

[0051] The molar ratio of mannitol to dimethyl carbonate is 1:(1-1.15);

[0052] (2) Compound 1 is reacted with thionyl chloride in a solvent at 70-85°C for 2-4 hours to obtain compound 2;

[0053] The molar ratio of compound 1 to thionyl chloride is 1:(2-2.7);

[0054] (3) Compound 2 is reacted with a sodium hypochlorite aqueous solution in a solvent and in the presence of a catalyst at 10-25° C. for 0.5-2 h to obtain compound 3;

[0055] The catalyst includes an aqueous solution of ruthenium trichloride;

[0056] The mass fraction of the ruthenium trichloride aqueous solution is 1-5%;

[0057] The molar ratio of the compound 2 to the catalyst is 1:(0.0001-0.005);

[0058] The molar ratio of compound 2 to sodium hypochlorite aqueous solution is 1:(2-4);

[0059] The mass fraction of the sodium hypochlorite aqueous solution is 8-12%.

[0060] Compared with the prior art, the present invention has the following beneficial effects:

[0061] The invention uses mannitol and dimethyl carbonate as starting raw materials to prepare mannitol carbonate sulfate, and obtains the target compound through ester exchange, cyclization and oxidation reactions. The raw materials are cheap and easy to obtain, and the reaction operation is simple. The yield of the obtained product is above 71%, the purity is above 99.6%, and the product is suitable for industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0062] Figure 1 The compound 3 prepared in Example 1 1 H NMR spectrum.

[0063] Figure 2 The compound 3 prepared in Example 1 13 C NMR spectrum.

[0064] Figure 3 This is the infrared spectrum of compound 3 prepared in Example 1. DETAILED DESCRIPTION

[0065] The technical solution of the present invention will be further described below with reference to the accompanying drawings and through specific embodiments. However, the following examples are merely simplified examples of the present invention and do not represent or limit the scope of protection of the present invention. The scope of protection of the present invention shall be subject to the claims.

[0066] Example 1

[0067] This embodiment provides mannitol sulfate carbonate and a preparation method thereof, wherein the preparation method comprises the following steps:

[0068] (1) In a 500 mL reaction apparatus equipped with a water separator, acetonitrile (227.7 g), mannitol (91.1 g, 0.5 mol), dimethyl carbonate (47.3 g, 0.525 mol), and 1,5,7-triazabicyclo[4.4.0]decene-5-ene (TBD) (1.0 g, 0.0075 mol) were added, mixed evenly, and reacted at 72°C for 10 hours. After the reaction was completed, the temperature was slowly lowered to 55°C, filtered, and the filtrate was concentrated, crystallized, and dried to obtain mannitol carbonate (Compound 1).

[0069] (2) Mannitol carbonate (104.1 g, 0.5 mol) in step (1) was added to a 1000 mL reaction flask, dichloroethane (520.4 g) was added, stirred evenly, heated to 55 ° C, and thionyl chloride (136.8 g, 1.15 mol) was slowly added dropwise. After the addition was completed, the temperature was raised to 75 ° C. and the reaction was kept warm for 2.5 hours. After the reaction was completed, the temperature was cooled to room temperature, filtered, and the filter cake was washed with water and methanol, respectively, and dried to obtain mannitol carbonate sulfite (Compound 2).

[0070] (3) Mannitol carbonate sulfite (150.1 g, 0.5 mol) obtained in step (2) was added to a 5000 mL reaction flask, acetonitrile (1201.0 g) and dichloromethane (900.8 g) were added, the temperature was controlled at 20° C., sodium hypochlorite aqueous solution (930.5 g, 1.25 mol, 10 wt%) was added, and ruthenium trichloride aqueous solution (15.6 g, 0.00075 mol, 1 wt%) was slowly added dropwise. After the addition was completed, the mixture was kept warm for 1 hour. After the reaction was completed, the liquid was separated, and the organic phase was concentrated to obtain a solid, which was washed with potassium carbonate aqueous solution (200 g, 5 wt%), then slurried with 200 mL of methanol, filtered, and dried to obtain mannitol carbonate sulfate (Compound 3).

[0071] Mannitol carbonate sulfate was characterized by H NMR spectroscopy. Figure 1 As shown, its NMR data are as follows:

[0072] 1 H NMR (500MHz, Chloroform-d) δ 5.41-5.27 (m, 2H), 5.13 (qd, J = 4.8, 1.9Hz, 2H), 4.73 (dd, J = 12.2, 4.9Hz, 2H), 4.48 (dd, J = 12.2, 4.9Hz, 2H).

[0073] Mannitol carbonate sulfate was characterized by NMR carbon spectroscopy. Figure 2 As shown, its NMR data are as follows:

[0074] 13 C NMR (125MHz, Chloroform-d) δ154.10,78.15,77.76,67.74.

[0075] Mannitol carbonate sulfate was tested with infrared spectroscopy. Figure 3 As shown, the infrared data are as follows:

[0076] FT-IR (KBr, cm -1 ):3207.86,1799.31,1474.37,1401.48,1044.71,999.26.

[0077] Example 2

[0078] This embodiment provides mannitol carbonate sulfate and a preparation method thereof. The only difference between the embodiment and the embodiment 1 is that TBD is replaced with an equimolar amount of 1,8-diazobispiro[5.4.0]undec-7-ene (DBU). The rest is the same as the embodiment 1.

[0079] Example 3

[0080] This embodiment provides a mannitol carbonate sulfate and a preparation method thereof, which differs from Example 1 in that the amount of dimethyl carbonate used in step (1) is (49.5 g, 0.55 mol) (the molar ratio of mannitol to dimethyl carbonate is 1:1.1), the amount of TBD used is (1.7 g, 0.0125 mol) (the molar ratio of mannitol to TBD is 1:0.025), and the amount of thionyl chloride used in step (2) is (148.7 g, 1.25 mol). ol) (the molar ratio of compound 1 to thionyl chloride is 1:2.5), the amount of sodium hypochlorite aqueous solution used in step (3) is (1116.6 g, 1.5 mol, 10 wt%), (the molar ratio of compound 2 to sodium hypochlorite aqueous solution is 1:3), the amount of ruthenium trichloride aqueous solution used is (31.1 g, 0.0015 mol, 1 wt%) (the molar ratio of compound 2 to ruthenium trichloride aqueous solution is 1:0.003), and the rest are the same as in Example 1.

[0081] Example 4

[0082] This embodiment provides mannitol carbonate sulfate and a preparation method thereof. The difference between the embodiment 1 and the embodiment 1 is that the mass of thionyl chloride is adjusted to (130.9 g, 1.1 mol) in step (2). The rest is the same as that in embodiment 1.

[0083] Example 5

[0084] This embodiment provides mannitol carbonate sulfate and a preparation method thereof. The difference between the embodiment 1 and the embodiment 1 is that the reaction temperature in step (1) is 75° C., the temperature for adding thionyl chloride dropwise in step (2) is 58° C., and the reaction temperature is 80° C.; the rest is the same as in embodiment 1.

[0085] Example 6

[0086] This embodiment provides mannitol carbonate sulfate and a preparation method thereof. The difference between this embodiment and embodiment 1 is that the reaction temperature of step (1) is 70°C, the filtration temperature is 50°C, and the reaction temperature of step (3) is 15°C. The rest is the same as in embodiment 1.

[0087] Example 7

[0088] This embodiment provides mannitol carbonate sulfate and a preparation method thereof. The difference between this embodiment and embodiment 1 is that the reaction time of step (2) is 3 hours, and the reaction time of step (3) is 1.5 hours. The rest is the same as embodiment 1.

[0089] Example 8

[0090] This embodiment provides mannitol carbonate sulfate and a preparation method thereof. The difference between this embodiment and embodiment 1 is that the reaction time of step (1) is 9 hours, and the rest is the same as embodiment 1.

[0091] Example 9

[0092] This embodiment provides a mannitol carbonate sulfate and a preparation method thereof, which differs from Example 1 in that the amount of dimethyl carbonate used in step (1) is (51.8 g, 0.575 mol) (the molar ratio of mannitol to dimethyl carbonate is 1:1.15), the amount of TBD used is (2.8 g, 0.02 mol) (the molar ratio of mannitol to TBD is 1:0.04), and the amount of thionyl chloride used in step (2) is (160.6 g, 1.35 mol). ol) (the molar ratio of compound 1 to thionyl chloride is 1:2.7), the amount of sodium hypochlorite aqueous solution used in step (3) is (1488.8 g, 2.0 mol, 10 wt%) (the molar ratio of compound 2 to sodium hypochlorite aqueous solution is 1:4), the amount of ruthenium trichloride aqueous solution used is (51.9 g, 0.0025 mol, 1 wt%) (the molar ratio of compound 2 to ruthenium trichloride aqueous solution is 1:0.005), and the rest are the same as in Example 1.

[0093] Example 10

[0094] This embodiment provides a mannitol carbonate sulfate and a preparation method thereof, which differs from Example 1 in that the amount of dimethyl carbonate used in step (1) is (45.0 g, 0.5 mol) (the molar ratio of mannitol to dimethyl carbonate is 1:1.0), the amount of TBD used is (0.7 g, 0.005 mol) (the molar ratio of mannitol to TBD is 1:0.01), and the amount of thionyl chloride used in step (2) is (119.0 g, 1.0 mol). )(the molar ratio of compound 1 to thionyl chloride is 1:2.0), the amount of sodium hypochlorite aqueous solution used in step (3) is (744.4 g, 1.0 mol, 10 wt%) (the molar ratio of compound 2 to sodium hypochlorite aqueous solution is 1:2), the amount of ruthenium trichloride aqueous solution used is (1.037 g, 0.00005 mol, 1 wt%) (the molar ratio of compound 2 to ruthenium trichloride aqueous solution is 1:0.0001), and the rest are the same as in Example 1.

[0095] Example 11

[0096] This embodiment provides mannitol carbonate sulfate and a preparation method thereof. The difference between the embodiment 1 and the embodiment 1 is that the reaction temperature in step (1) is 80°C, the filtration temperature is 65°C, the temperature for dropwise addition of thionyl chloride in step (2) is 60°C, the reaction temperature is 85°C, and the reaction temperature in step (3) is 25°C. The rest is the same as in embodiment 1.

[0097] Example 12

[0098] This embodiment provides mannitol carbonate sulfate and a preparation method thereof. The difference between the embodiment 1 and the embodiment 1 is that the reaction temperature in step (1) is 65°C, the filtration temperature is 40°C, the temperature for dropwise addition of thionyl chloride in step (2) is 50°C, the reaction temperature is 70°C, and the reaction temperature in step (3) is 10°C. The rest is the same as in embodiment 1.

[0099] Example 13

[0100] This embodiment provides mannitol carbonate sulfate and a preparation method thereof. The difference between this embodiment and embodiment 1 is that the reaction time of step (1) is 12 hours, the reaction time of step (2) is 4 hours, and the reaction time of step (3) is 2 hours. The rest is the same as embodiment 1.

[0101] Example 14

[0102] This embodiment provides mannitol carbonate sulfate and a preparation method thereof. The difference between this embodiment and embodiment 1 is that the reaction time of step (1) is 8 hours, the reaction time of step (2) is 2 hours, and the reaction time of step (3) is 0.5 hours. The rest is the same as embodiment 1.

[0103] The yield and purity of mannitol sulfate carbonate prepared in the above example are shown in Table 1:

[0104] Table 1

[0105]

[0106]

[0107] As can be seen from the data in Table 1, the purity of mannitol sulfate carbonate obtained by the preparation method of the present invention is above 99.6%, the yield is above 71%, and the yield of the preferred solution reaches above 86%.

[0108] From the comparison between Example 1 and Example 9, it can be seen that the molar ratio of mannitol to dimethyl carbonate is preferably 1:(1.05-1.10), while in Example 9, the molar ratio of mannitol to dimethyl carbonate is 1:1.15, and the amounts of TBD, thionyl chloride, sodium hypochlorite aqueous solution and ruthenium trichloride aqueous solution are not within the preferred range of the present invention, resulting in the ester exchange reaction in step (1) producing more by-products. In step (3), the product undergoes a certain degree of hydrolysis under alkaline conditions, and the use of a large amount of sodium hypochlorite aqueous solution will aggravate the hydrolysis of the product, resulting in a decrease in the total yield.

[0109] From the comparison of Example 1 and Example 10, it can be seen that the molar ratio of mannitol to dimethyl carbonate is preferably 1:(1.05-1.10), while in Example 10, the molar ratio of mannitol to dimethyl carbonate is 1:1.0, and the amounts of TBD, thionyl chloride, sodium hypochlorite aqueous solution and ruthenium trichloride aqueous solution are not within the preferred range of the present invention, resulting in insufficient transesterification, cyclization and oxidation reactions, and the overall yield of the target product is low.

[0110] From the comparison between Example 1 and Example 11, it can be seen that the temperatures of the three-step reaction are all within the upper limit specified in the present invention. As the temperature increases, the raw materials in step (1) will continue to evaporate during the reaction, resulting in incomplete reaction. At the same time, the higher temperature in step (3) also aggravates the hydrolysis of the product, thereby reducing the total yield of the product.

[0111] From the comparison between Example 1 and Example 12, it can be seen that the temperatures of the three-step reaction are all within the lower limit specified in the present invention. The by-product methanol in step (1) evaporates slowly, which reduces the reaction rate. At the same time, steps (2) and (3) react slowly at lower temperatures, resulting in a decrease in the total yield of the product.

[0112] From the comparison between Example 1 and Example 13, it can be seen that the reaction times of the three steps are all within the upper limit defined by the present invention. Even if the reaction time is extended, the reaction yield will not be improved.

[0113] From the comparison between Example 1 and Example 14, it can be seen that the time of the three-step reaction is within the lower limit specified in the present invention. Under this condition, the three-step reaction cannot fully react, resulting in a decrease in the yield of the target product.

[0114] The applicant declares that the above is only a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention fall within the scope of protection and disclosure of the present invention.

Claims

1. A method for preparing mannitol carbonate sulfate, characterized in that: The preparation method of the mannitol carbonate sulfate comprises the following steps: (1) Mannitol is reacted with dimethyl carbonate to obtain compound 1, and the reaction formula is shown below: (2) Compound 1 is reacted with thionyl chloride to obtain compound 2. The reaction formula is as follows: (3) Compound 2 is reacted with an aqueous sodium hypochlorite solution to obtain compound 3, as shown in the following reaction formula:

2. The method for preparing mannitol sulfate carbonate according to claim 1, wherein In step (1), the reaction is carried out in a solvent; Preferably, in step (1), the solvent comprises a non-aqueous solvent; Preferably, in step (1), the non-aqueous solvent comprises any one or a combination of at least two of acetonitrile, 1,2-dichloroethane, ethanol, carbon tetrachloride or benzene, more preferably acetonitrile; Preferably, in step (1), the reaction is carried out in the presence of a catalyst; Preferably, in step (1), the catalyst comprises an organic base catalyst; Preferably, in step (1), the organic base catalyst comprises any one or a combination of at least two of 1,5,7-triazabicyclo[4.4.0]decene-5-ene, 1,8-diazabispiro[5.4.0]undec-7-ene, triethylamine, imidazole or 4-dimethylaminopyridine, and is further preferably 1,5,7-triazabicyclo[4.4.0]decene-5-ene or 1,8-diazabispiro[5.4.0]undec-7-ene; Preferably, the molar ratio of mannitol to the organic base catalyst is 1:(0.01-0.04), more preferably 1:(0.015-0.025).

3. The preparation method of mannitol sulfate carbonate according to claim 1 or 2, wherein In step (1), the molar ratio of mannitol to dimethyl carbonate is 1:(1-1.15), preferably 1:(1.05-1.10).

4. The method for preparing mannitol sulfate carbonate according to any one of claims 1 to 3, wherein In step (1), the reaction temperature is 65-80°C, preferably 70-75°C; Preferably, in step (1), the reaction time is 8 to 12 hours, more preferably 10 to 11 hours.

5. The method for preparing mannitol sulfate carbonate according to any one of claims 1 to 4, wherein: In step (2), the reaction is carried out in a solvent; Preferably, in step (2), the solvent comprises a non-aqueous solvent; Preferably, in step (2), the non-aqueous solvent comprises any one or a combination of at least two of 1,2-dichloroethane, acetonitrile, carbon tetrachloride, toluene or xylene, more preferably 1,2-dichloroethane; Preferably, the molar ratio of the compound 1 to thionyl chloride is 1:(2-2.7), more preferably 1:(2-2.5).

6. The method for preparing mannitol sulfate carbonate according to any one of claims 1 to 5, wherein: In step (2), the reaction temperature is 70-85°C, preferably 75-80°C; Preferably, in step (2), the reaction time is 2 to 4 hours, more preferably 2.5 to 3 hours.

7. The method for preparing mannitol sulfate carbonate according to any one of claims 1 to 6, wherein: In step (3), the reaction is carried out in a solvent; Preferably, in step (3), the solvent comprises a non-aqueous solvent; Preferably, in step (3), the non-aqueous solvent comprises any one or a combination of at least two of dichloromethane, 1,2-dichloroethane, acetonitrile, toluene, xylene or dimethyl carbonate, more preferably a combination of dichloromethane and acetonitrile.

8. The method for preparing mannitol sulfate carbonate according to any one of claims 1 to 7, wherein: In step (3), the reaction is carried out in the presence of a catalyst; Preferably, in step (3), the catalyst comprises an aqueous solution of ruthenium trichloride; Preferably, in step (3), the mass fraction of the ruthenium trichloride aqueous solution is 1-5%; Preferably, in step (3), the molar ratio of the compound 2 to the catalyst is 1:(0.0001-0.005), more preferably 1:(0.0015-0.003).

9. The method for preparing mannitol sulfate carbonate according to any one of claims 1 to 8, wherein: The molar ratio of the compound 2 to the sodium hypochlorite aqueous solution is 1:(2-4), preferably 1:(2.5-3); Preferably, the mass fraction of the sodium hypochlorite aqueous solution is 8-12%; Preferably, in step (3), the reaction temperature is 10 to 25°C, preferably 15 to 20°C; Preferably, the reaction time is 0.5 to 2 hours, more preferably 1 to 1.5 hours.

10. The method for preparing mannitol sulfate carbonate according to any one of claims 1 to 9, characterized in that: The preparation method of the mannitol carbonate sulfate specifically comprises: (1) Mannitol and dimethyl carbonate are reacted in a solvent in the presence of a catalyst at 65-80° C. for 8-12 hours to obtain compound 1; The catalyst includes an organic base catalyst; The organic base catalyst includes any one or a combination of at least two of 1,5,7-triazabicyclo[4.4.0]decene-5-ene, 1,8-diazobispiro[5.4.0]undec-7-ene, triethylamine, imidazole or 4-dimethylaminopyridine; The molar ratio of mannitol to organic base catalyst is 1:(0.01-0.04); The molar ratio of mannitol to dimethyl carbonate is 1:(1-1.15); (2) Compound 1 is reacted with thionyl chloride in a solvent at 70-85°C for 2-4 hours to obtain compound 2; The molar ratio of compound 1 to thionyl chloride is 1:(2-2.7); (3) Compound 2 is reacted with a sodium hypochlorite aqueous solution in a solvent and in the presence of a catalyst at 10-25° C. for 0.5-2 h to obtain compound 3; The catalyst includes an aqueous solution of ruthenium trichloride; The mass fraction of the ruthenium trichloride aqueous solution is 1-5%; The molar ratio of the compound 2 to the catalyst is 1:(0.0001-0.005); The molar ratio of compound 2 to sodium hypochlorite aqueous solution is 1:(2-4); The mass fraction of the sodium hypochlorite aqueous solution is 8-12%.

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