Green synthesis method of ethylene carbonate based on ionic liquid catalyst

Abstract

The invention relates to the technical field of ethylene carbonate, in particular to an ethylene carbonate green synthesis method based on an ionic liquid catalyst, which comprises the following steps: S1, preparing raw materials including ethylene oxide, carbon dioxide and a catalyst according to a mass ratio of 1: (1.2-1.4): (0.006-0.008), the catalyst is prepared by mixing ionic liquid, modified chitosan and powder, and the mass ratio of the ionic liquid to the modified chitosan to the powder is 1: (0.2-0.4): (0.1-0.3). According to the invention, the kaolin can be used as a carrier to enhance the dispersibility and prevent the agglomeration of the catalyst, and the addition of the multi-component substance can reduce the ring-opening activation energy of ethylene oxide and significantly improve the reaction efficiency, thereby enhancing the purity and yield of the synthesized substance.

Description

Technical Field

[0001] The invention relates to the technical field of ethylene carbonate, in particular to a green synthesis method of ethylene carbonate based on an ionic liquid catalyst. Background Art

[0002] Ethylene carbonate is an important organic compound. It is a colorless, transparent liquid at room temperature with a slight ethereal odor. It has a high dielectric constant and good chemical stability, and is widely used in various fields. In the lithium battery industry, it is often used as an electrolyte solvent.

[0003] In the prior art, the catalysts used in the synthesis and preparation of ethylene carbonate are insufficiently selective for the production of ethylene carbonate, resulting in the generation of various byproducts that affect the purity of the ethylene carbonate. In response to this, the present invention provides a green synthesis method for ethylene carbonate using an ionic liquid catalyst. Summary of the Invention

[0004] The purpose of the present invention is to provide a green synthesis method of ethylene carbonate based on an ionic liquid catalyst. The ethylene carbonate prepared by the present invention has not only good purity performance, but also excellent yield performance.

[0005] To achieve the above object, the present invention provides the following technical solution: a green synthesis method of ethylene carbonate based on an ionic liquid catalyst, comprising the following steps:

[0006] S1: Raw material preparation, the raw materials include ethylene oxide, carbon dioxide, and a catalyst, the mass ratio of ethylene oxide, carbon dioxide, and catalyst is 1: (1.2-1.4): (0.006-0.008), the catalyst is prepared by mixing ionic liquid, modified chitosan, and powder, the mass ratio of ionic liquid, modified chitosan, and powder is 1: (0.2-0.4): (0.1-0.3);

[0007] S2: Reaction preparation: ethylene oxide, carbon dioxide and a catalyst are reacted to prepare ethylene carbonate.

[0008] Furthermore, the ionic liquid is prepared by the following method: choline chloride, lactic acid, oxalic acid, and formic acid are added to a flask and heated in a water bath, the water bath temperature is set to 60-70°C, and after stirring, the reaction is carried out at a constant temperature for 20-30 minutes. The obtained product is washed and filtered, and then added to a flask, alkali lignin and anhydrous ethanol are added to the flask, and the water bath is heated to 65-75°C. After stirring, the reaction is carried out at a constant temperature for 10-20 minutes. The obtained product is filtered to obtain a solid, distilled water is added to the solid, and the reaction is allowed to stand for 10-20 hours. The obtained product is added to a centrifuge, and the centrifuge is set to 2000-3000 r / min and centrifuged for 4-6 minutes. A precipitate is taken from the obtained product, and the precipitate is mixed with the solution to prepare an ionic liquid.

[0009] Furthermore, the mass ratio of choline chloride, lactic acid, oxalic acid and formic acid is 1:(0.4-0.6):(0.2-0.4):(0.1-0.3).

[0010] Furthermore, the mass of alkali lignin is 40-60% of the mass of choline chloride, the mass of anhydrous ethanol is 20-40% of the mass of choline chloride, and the mass of distilled water is 2-3 times the mass of the solid matter.

[0011] Furthermore, the mass of the solution is 60-80% of the mass of the precipitate.

[0012] Furthermore, the solution is prepared by the following method: L-lysine and deionized water are added to a beaker and mixed evenly, acetic acid is added dropwise to the beaker, the pH value of the mixture of L-lysine and deionized water in the beaker is adjusted to 7, and then allowed to react for 10 to 20 minutes to prepare a solution, wherein the mass ratio of L-lysine to deionized water is 1:(4 to 6).

[0013] Furthermore, the modified chitosan is prepared by the following method: chitosan and acetic acid aqueous solution are added to a beaker and mixed, and a magnetic stirrer is set at 120-160 r / min and stirred for 30-40 minutes, tea polyphenols and deionized water are added to the beaker, and the magnetic stirrer is set at 200-300 r / min and stirred for 20-30 minutes, the obtained product is ultrasonically treated for 6-10 minutes, and then a sodium hydroxide solution is added to adjust the pH value to 9-10, and the obtained product is added to a centrifuge, and the centrifuge is set at 3000-5000 r / min and centrifuged for 4-6 minutes to obtain a precipitate, the precipitate is washed with deionized water, and then added to an oven, and the oven is set at 50-60°C and dried for 10-20 minutes to obtain the modified chitosan.

[0014] Furthermore, the mass ratio of chitosan to acetic acid aqueous solution is 1:(8-10), the mass concentration of acetic acid aqueous solution is 2-4%, the mass of tea polyphenols is 1.5 times the mass of chitosan, and the mass of deionized water is 2-4 times the mass of tea polyphenols.

[0015] Furthermore, the powder is kaolin with a particle size of 4 to 10 μm.

[0016] Furthermore, the reaction preparation method is: ethylene oxide, carbon dioxide, and a catalyst are added to a reactor, the reactor is set to a pressure of 2 to 4 MPa, a temperature of 160 to 180° C., and a reaction time of 14 to 22 minutes, and the obtained product is the base material.

[0017] Compared with the prior art, the present invention has the following beneficial effects:

[0018] 1. In the present invention, during the preparation process of ethylene carbonate, ionic liquid and modified chitosan are added to the catalyst, wherein, after the initial reaction with choline chloride, alkali lignin and anhydrous ethanol are introduced to enhance stability, and then mixed with L-lysine solution to form a catalytic center with high activity and low by-products. After the chitosan is cross-linked with tea polyphenols, a cross-linked porous structure is formed to enhance the adsorption capacity of reactants. The addition of kaolin can serve as a carrier to enhance dispersibility and prevent catalyst agglomeration. The addition of multi-component substances can reduce the ring-opening activation energy of ethylene oxide, significantly improve the reaction efficiency, and thereby improve the purity and yield of the synthesized substance.

[0019] 2. In the present invention, modified chitosan and powder are added during the preparation process. Chitosan and kaolin used as raw materials are both natural materials, which are relatively natural and environmentally friendly. After ethylene carbonate is synthesized, its waste has less pollution to the environment, which meets the requirements of green environmental protection. DETAILED DESCRIPTION

[0020] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0021] It should be noted that the raw materials used in the following examples are all commercially available raw materials.

[0022] Example 1:

[0023] A green synthesis method for ethylene carbonate based on an ionic liquid catalyst comprises the following steps:

[0024] S1: Raw material preparation, the raw materials include ethylene oxide, carbon dioxide, and a catalyst, the mass ratio of ethylene oxide, carbon dioxide, and catalyst is 1:(1.2):(0.006), the catalyst is prepared by mixing ionic liquid, modified chitosan, and powder, the mass ratio of ionic liquid, modified chitosan, and powder is 1:(0.2):(0.1);

[0025] S2: Reaction preparation: ethylene oxide, carbon dioxide and a catalyst are reacted to prepare ethylene carbonate.

[0026] The ionic liquid is prepared by the following method: choline chloride, lactic acid, oxalic acid, and formic acid are added to a flask and heated in a water bath, the water bath temperature is set to 60°C, stirred evenly, and reacted at a constant temperature for 20 minutes, the obtained product is washed and filtered, and then added to a flask, alkali lignin and anhydrous ethanol are added to the flask, heated to 65°C in a water bath, stirred evenly, and reacted at a constant temperature for 10 minutes, the obtained product is filtered to obtain a solid, distilled water is added to the solid, and the reaction is allowed to stand for 10 hours, the obtained product is added to a centrifuge, the centrifuge is set to 2000 r / min and centrifuged for 4 minutes, a precipitate is taken from the obtained product, and the precipitate is mixed with the solution to prepare the ionic liquid.

[0027] The mass ratio of choline chloride, lactic acid, oxalic acid and formic acid is 1:(0.4):(0.2):(0.1).

[0028] The mass of alkali lignin is 40% of the mass of choline chloride, the mass of anhydrous ethanol is 20% of the mass of choline chloride, and the mass of distilled water is twice the mass of the solid matter.

[0029] The mass of the solution is 60% of the mass of the precipitate.

[0030] The solution was prepared by the following method: L-lysine and deionized water were added to a beaker and mixed, acetic acid was added dropwise to the beaker, the pH value of the mixture of L-lysine and deionized water in the beaker was adjusted to 7, and then allowed to react for 10 minutes to prepare a solution, wherein the mass ratio of L-lysine to deionized water was 1:(4).

[0031] Modified chitosan was prepared by the following method: chitosan and acetic acid aqueous solution were added to a beaker and mixed, and stirred for 30 minutes using a magnetic stirrer set at 120 r / min, tea polyphenols and deionized water were added to the beaker, and stirred for 20 minutes using a magnetic stirrer set at 200 r / min, the resulting product was ultrasonically treated for 6 minutes, and then sodium hydroxide solution was added to adjust the pH value to 9, the resulting product was added to a centrifuge, and the centrifuge was set at 3000 r / min for 4 minutes to obtain a precipitate, the precipitate was washed with deionized water, and then added to an oven, and the oven was set at 50°C for drying for 10 minutes to obtain modified chitosan.

[0032] The mass ratio of chitosan to acetic acid aqueous solution is 1:(8), the mass concentration of acetic acid aqueous solution is 2%, the mass of tea polyphenols is 1.5 times the mass of chitosan, and the mass of deionized water is 2 times the mass of tea polyphenols.

[0033] The powder is kaolin with a particle size of 4 μm.

[0034] The reaction preparation method is as follows: ethylene oxide, carbon dioxide, and a catalyst are added to a reactor, the reactor is set to a pressure of 2 MPa, a temperature of 160° C., and a reaction time of 14 minutes, and the obtained product is the base material.

[0035] Example 2:

[0036] A green synthesis method for ethylene carbonate based on an ionic liquid catalyst comprises the following steps:

[0037] S1: Raw material preparation, the raw materials include ethylene oxide, carbon dioxide, and a catalyst, the mass ratio of ethylene oxide, carbon dioxide, and catalyst is 1:(1.3):(0.007), the catalyst is prepared by mixing ionic liquid, modified chitosan, and powder, the mass ratio of ionic liquid, modified chitosan, and powder is 1:(0.3):(0.2);

[0038] S2: Reaction preparation: ethylene oxide, carbon dioxide and a catalyst are reacted to prepare ethylene carbonate.

[0039] The ionic liquid is prepared by the following method: choline chloride, lactic acid, oxalic acid, and formic acid are added to a flask and heated in a water bath, the water bath temperature is set to 65°C, stirred evenly, and reacted at a constant temperature for 25 minutes, the obtained product is washed and filtered, and then added to a flask, alkali lignin and anhydrous ethanol are added to the flask, heated to 70°C in a water bath, stirred evenly, and reacted at a constant temperature for 15 minutes, the obtained product is filtered to obtain a solid, distilled water is added to the solid, and the reaction is allowed to stand for 15 hours, the obtained product is added to a centrifuge, the centrifuge is set to 2500r / min and centrifuged for 5 minutes, a precipitate is taken from the obtained product, and the precipitate is mixed with the solution to prepare the ionic liquid.

[0040] The mass ratio of choline chloride, lactic acid, oxalic acid and formic acid is 1:(0.5):(0.3):(0.2).

[0041] The mass of alkali lignin is 50% of the mass of choline chloride, the mass of anhydrous ethanol is 30% of the mass of choline chloride, and the mass of distilled water is 2.5 times the mass of the solid matter.

[0042] The mass of the solution is 70% of the mass of the precipitate.

[0043] The solution was prepared by the following method: L-lysine and deionized water were added to a beaker and mixed, acetic acid was added dropwise to the beaker, the pH value of the mixture of L-lysine and deionized water in the beaker was adjusted to 7, and then allowed to react for 15 minutes to prepare a solution, wherein the mass ratio of L-lysine to deionized water was 1:(5).

[0044] Modified chitosan was prepared by the following method: chitosan and acetic acid aqueous solution were added to a beaker and mixed, and stirred for 35 minutes using a magnetic stirrer set at 140 r / min, tea polyphenols and deionized water were added to the beaker, and stirred for 25 minutes using a magnetic stirrer set at 250 r / min, the resulting product was ultrasonically treated for 8 minutes, and then sodium hydroxide solution was added to adjust the pH value to 9.5, the resulting product was added to a centrifuge, and the centrifuge was set at 4000 r / min for 5 minutes to obtain a precipitate, the precipitate was washed with deionized water, and then added to an oven, and the oven was set at 55°C for drying for 15 minutes to obtain modified chitosan.

[0045] The mass ratio of chitosan to acetic acid aqueous solution is 1:(9), the mass concentration of acetic acid aqueous solution is 3%, the mass of tea polyphenols is 1.5 times the mass of chitosan, and the mass of deionized water is 3 times the mass of tea polyphenols.

[0046] The powder is kaolin with a particle size of 7 μm.

[0047] The reaction preparation method is as follows: ethylene oxide, carbon dioxide, and a catalyst are added to a reactor, the reactor is set to a pressure of 3 MPa, a temperature of 170° C., and a reaction time of 18 minutes, and the obtained product is the base material.

[0048] Example 3:

[0049] A green synthesis method for ethylene carbonate based on an ionic liquid catalyst comprises the following steps:

[0050] S1: Raw material preparation, the raw materials include ethylene oxide, carbon dioxide, and a catalyst, the mass ratio of ethylene oxide, carbon dioxide, and catalyst is 1:(1.4):(0.008), the catalyst is prepared by mixing ionic liquid, modified chitosan, and powder, the mass ratio of ionic liquid, modified chitosan, and powder is 1:(0.4):(0.3);

[0051] S2: Reaction preparation: ethylene oxide, carbon dioxide and a catalyst are reacted to prepare ethylene carbonate.

[0052] The ionic liquid is prepared by the following method: choline chloride, lactic acid, oxalic acid, and formic acid are added to a flask and heated in a water bath, the water bath temperature is set to 70°C, stirred evenly, and reacted at a constant temperature for 30 minutes, the obtained product is washed and filtered, and then added to a flask, alkali lignin and anhydrous ethanol are added to the flask, heated to 75°C in a water bath, stirred evenly, and reacted at a constant temperature for 20 minutes, the obtained product is filtered to obtain a solid, distilled water is added to the solid, and the reaction is allowed to stand for 20 hours, the obtained product is added to a centrifuge, the centrifuge is set to 3000 r / min and centrifuged for 6 minutes, a precipitate is taken from the obtained product, and the precipitate is mixed with the solution to prepare the ionic liquid.

[0053] The mass ratio of choline chloride, lactic acid, oxalic acid and formic acid is 1:(0.6):(0.4):(0.3).

[0054] The mass of alkali lignin is 60% of the mass of choline chloride, the mass of anhydrous ethanol is 40% of the mass of choline chloride, and the mass of distilled water is 3 times the mass of the solid matter.

[0055] The mass of the solution is 80% of the mass of the precipitate.

[0056] The solution was prepared by the following method: L-lysine and deionized water were added to a beaker and mixed, acetic acid was added dropwise to the beaker, the pH value of the mixture of L-lysine and deionized water in the beaker was adjusted to 7, and then allowed to react for 20 minutes to prepare a solution, wherein the mass ratio of L-lysine to deionized water was 1:(6).

[0057] Modified chitosan was prepared by the following method: chitosan and acetic acid aqueous solution were added to a beaker and mixed, and stirred for 40 minutes using a magnetic stirrer set at 160 r / min, tea polyphenols and deionized water were added to the beaker, and stirred for 30 minutes using a magnetic stirrer set at 300 r / min, the resulting product was ultrasonically treated for 10 minutes, and then sodium hydroxide solution was added to adjust the pH value to 10, the resulting product was added to a centrifuge, and the centrifuge was set at 5000 r / min for 6 minutes to obtain a precipitate, the precipitate was washed with deionized water, and then added to an oven, and the oven was set at 60°C for drying for 20 minutes to obtain modified chitosan.

[0058] The mass ratio of chitosan to acetic acid aqueous solution is 1:(10), the mass concentration of acetic acid aqueous solution is 4%, the mass of tea polyphenols is 1.5 times the mass of chitosan, and the mass of deionized water is 4 times the mass of tea polyphenols.

[0059] The powder is kaolin with a particle size of 10 μm.

[0060] The reaction preparation method is as follows: ethylene oxide, carbon dioxide, and a catalyst are added to a reactor, the reactor is set at a pressure of 4 MPa, a temperature of 180° C., and a reaction time of 22 minutes, and the obtained product is the base material.

[0061] Comparative Example 1: This comparative example differs from Example 1 in that this comparative example does not contain an ionic liquid.

[0062] Comparative Example 2: This comparative example differs from Example 1 in that choline chloride is not contained in this comparative example.

[0063] Comparative Example 3: The difference between this comparative example and Example 1 is that in this comparative example, an equal amount of chitosan is used to replace the modified chitosan.

[0064] Comparative Example 4: This comparative example differs from Example 1 in that the present comparative example does not contain powder.

[0065] Performance test: The performance test was performed on the ethylene carbonate prepared in Example 1, Example 2, Example 3, Comparative Example 1, Comparative Example 2, Comparative Example 3 and Comparative Example 4. The test data are recorded in the following table:

[0066]

[0067] It can be seen that the purity performance and yield performance of ethylene carbonate prepared in Comparative Examples 1, 2, 3 and 4 are lower than those in Examples 1, 2 and 3; this shows that: in the preparation process of ethylene carbonate, by adding ionic liquid and modified chitosan to the catalyst, wherein, after the preliminary reaction with choline chloride, alkali lignin and anhydrous ethanol are introduced, the stability can be enhanced, and then mixed with L-lysine solution to form a catalytic center with high activity and low by-products, chitosan can form a cross-linked porous structure after cross-linking treatment with tea polyphenols, thereby improving the adsorption capacity of reactants, the addition of kaolin can serve as a carrier to enhance dispersibility and prevent catalyst agglomeration, and the addition of multi-component substances can reduce the ring-opening activation energy of ethylene oxide, significantly improve the reaction efficiency, and thus improve the purity and yield of the synthesized substance;

[0068] By adding modified chitosan and powder during the preparation process, the chitosan and kaolin used as raw materials are both natural materials, which are relatively natural and environmentally friendly. After the ethylene carbonate is synthesized, its waste has less pollution to the environment, which meets the needs of green environmental protection.

[0069] By comparing and analyzing the relevant data in the table, it can be seen that the ethylene carbonate prepared by the present invention not only has good purity performance, but also has excellent yield performance. This shows that the green synthesis method of ethylene carbonate based on ionic liquid catalyst provided by the present invention has a broader market prospect and is more suitable for promotion.

[0070] Throughout this specification, references to terms such as "one embodiment," "example," or "specific example" indicate that the specific features, structures, materials, or characteristics described in conjunction with that embodiment or example are included in at least one embodiment or example of the present invention. In this specification, schematic representations of these terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

[0071] The preferred embodiments of the present invention disclosed above are intended only to help illustrate the present invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the present invention to the specific embodiments described. Obviously, many modifications and variations are possible based on the content of this specification. These embodiments are selected and described in detail in this specification to better explain the principles and practical applications of the present invention, thereby enabling those skilled in the art to better understand and utilize the present invention. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A green synthesis method for ethylene carbonate based on an ionic liquid catalyst, characterized in that: The following steps are involved: S1: Raw material preparation, the raw materials include ethylene oxide, carbon dioxide, and a catalyst, the mass ratio of ethylene oxide, carbon dioxide, and catalyst is 1: (1.2-1.4): (0.006-0.008), the catalyst is prepared by mixing ionic liquid, modified chitosan, and powder, the mass ratio of ionic liquid, modified chitosan, and powder is 1: (0.2-0.4): (0.1-0.3); S2: Reaction preparation: ethylene oxide, carbon dioxide and a catalyst are reacted to prepare ethylene carbonate.

2. The green synthesis method of ethylene carbonate based on ionic liquid catalyst according to claim 1, characterized in that: The ionic liquid is prepared by the following method: choline chloride, lactic acid, oxalic acid, and formic acid are added to a flask and heated in a water bath, the water bath temperature is set to 60-70°C, the mixture is stirred evenly, the mixture is reacted at a constant temperature for 20-30 minutes, the obtained product is washed and filtered, and then added to a flask, alkali lignin and anhydrous ethanol are added to the flask, the mixture is heated in a water bath to 65-75°C, the mixture is stirred evenly, the mixture is reacted at a constant temperature for 10-20 minutes, the obtained product is filtered to obtain a solid, distilled water is added to the solid, the mixture is allowed to react for 10-20 hours, the obtained product is added to a centrifuge, the centrifuge is set to 2000-3000 r / min, and the centrifuge is centrifuged for 4-6 minutes, a precipitate is collected from the obtained product, and the precipitate is mixed with the solution to prepare the ionic liquid.

3. The green synthesis method of ethylene carbonate based on ionic liquid catalyst according to claim 2, characterized in that: The mass ratio of choline chloride, lactic acid, oxalic acid and formic acid is 1:(0.4-0.6):(0.2-0.4):(0.1-0.3).

4. The green synthesis method of ethylene carbonate based on ionic liquid catalyst according to claim 2, characterized in that: The mass of alkali lignin is 40-60% of the mass of choline chloride, the mass of anhydrous ethanol is 20-40% of the mass of choline chloride, and the mass of distilled water is 2-3 times of the mass of the solid matter.

5. The green synthesis method of ethylene carbonate based on ionic liquid catalyst according to claim 1, characterized in that: The mass of the solution is 60-80% of the mass of the precipitate.

6. The green synthesis method of ethylene carbonate based on ionic liquid catalyst according to claim 2, characterized in that: The solution is prepared by the following method: L-lysine and deionized water are added to a beaker and mixed evenly, acetic acid is added dropwise to the beaker, the pH value of the mixture of L-lysine and deionized water in the beaker is adjusted to 7, and then the mixture is allowed to react for 10 to 20 minutes to prepare the solution, wherein the mass ratio of L-lysine to deionized water is 1:(4 to 6).

7. The green synthesis method of ethylene carbonate based on ionic liquid catalyst according to claim 1, characterized in that: The modified chitosan is prepared by the following method: chitosan and acetic acid aqueous solution are added to a beaker and mixed, and a magnetic stirrer is set at 120-160 r / min and stirred for 30-40 minutes, tea polyphenols and deionized water are added to the beaker, and the magnetic stirrer is set at 200-300 r / min and stirred for 20-30 minutes, the obtained product is ultrasonically treated for 6-10 minutes, and then a sodium hydroxide solution is added to adjust the pH value to 9-10, and the obtained product is added to a centrifuge, and the centrifuge is set at 3000-5000 r / min and centrifuged for 4-6 minutes to obtain a precipitate, and the precipitate is washed with deionized water, and then added to an oven, and the oven is set at 50-60°C and dried for 10-20 minutes to prepare the modified chitosan.

8. The green synthesis method of ethylene carbonate based on ionic liquid catalyst according to claim 7, characterized in that: The mass ratio of chitosan to acetic acid aqueous solution is 1:(8-10), the mass concentration of acetic acid aqueous solution is 2-4%, the mass of tea polyphenols is 1.5 times that of chitosan, and the mass of deionized water is 2-4 times that of tea polyphenols.

9. The green synthesis method of ethylene carbonate based on ionic liquid catalyst according to claim 1, characterized in that: The powder is kaolin with a particle size of 4 to 10 μm.

10. The green synthesis method of ethylene carbonate based on ionic liquid catalyst according to claim 1, characterized in that: The reaction preparation method is as follows: ethylene oxide, carbon dioxide and a catalyst are added into a reactor, the reactor is set at a pressure of 2-4 MPa, a temperature of 160-180° C., and a reaction time of 14-22 minutes, and the obtained product is the base material.

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