Preparation method of diisopropylamine silane

Abstract

The invention relates to a preparation method of diisopropylamine silane, which comprises the following steps: (1) reacting dichlorosilane with diisopropylamine to obtain diisopropylamine chlorosilane; and (2) carrying out a reaction on the diisopropylamine chlorosilane obtained in the step (1) and lithium hydride to obtain the diisopropylamine silane. The preparation method of diisopropylamine silane in the prior art is optimized, a complex catalyst does not need to be prepared in advance, raw materials are simple and easy to obtain, reaction steps are simple, high-temperature and high-pressure reaction conditions are avoided, the reaction conditions are mild, the obtained target product has high yield and purity, and industrial large-scale production is facilitated.

Description

Technical Field

[0001] This invention relates to the field of organic synthesis technology, and in particular to a method for preparing diisopropylamine silane. Background Technology

[0002] Diisopropylamine silane is a liquid silicon-based precursor used in high-end semiconductor fields. It can be used to prepare SiO2, SiN, SiCN, and SiC through chemical vapor deposition or atomic layer deposition (ALD) techniques, and is therefore widely applied in memory, light-emitting materials, solar cells, capacitors, logic chips, and power semiconductors. Compared to other silicon-based precursors, diisopropylamine silane has several advantages: First, its structure contains no chlorine atoms, thus avoiding the formation of chlorides during use and preventing damage to the resulting film. Furthermore, the direct bond between silicon and amine atoms in its structure, due to the weak bond energy between silicon and nitrogen, makes bond breaking easier, resulting in higher reactivity during ALD. Low-temperature deposition can be achieved through plasma ALD, avoiding damage to heat-sensitive substrates. Its good volatility and low carbon and oxygen impurity residues make it an important candidate to replace traditional precursors such as chlorosilanes. In recent years, with increasingly stringent requirements for process technology and material performance in the semiconductor field, the market demand for diisopropylamine silane has been growing.

[0003] There are reports on the synthesis of diisopropylamine silane, but all have certain drawbacks. Patent CN108586514A reports a method that first prepares a carbon nanotube catalyst through complex steps, and then uses it as a catalyst to catalyze the reaction of monochlorosilane and diisopropylamine to obtain diisopropylamine silane. This method requires the initial preparation of carbon nanotubes using diethyl ether, heavy metal compounds, etc., resulting in complex synthesis steps and low efficiency. Patent CN115260223A also requires the initial preparation of bis(hexamethyldisilazon)calcium as a catalyst through a complex reaction, followed by the catalysis of silane and diisopropylamine under high pressure. In this method, silane readily spontaneously combusts, requiring precise operation, resulting in low product yield, and the generation of hydrogen gas during the reaction, which is unfavorable for scale-up production. Patent CN117820348A reports a method for synthesizing diisopropylamine silane using Al(NMe2)3 as a catalyst. This method requires the initial preparation of Al(NMe2)3 (commercially available LiNMe2 reacts with AlCl3, followed by filtration and concentration to obtain Al(NMe2)3), and the yield is at most 60%. Patent CN118184688A uses copper bromide as a catalyst to catalyze the reaction of diisopropylamine and phenylsilane, followed by vacuum distillation to obtain a phenylsilaneamine intermediate. The intermediate is then reduced using borane and pinacolborane to finally obtain diisopropylamine silane. This method not only uses expensive phenylsilane but also involves complex reaction steps and low yields.

[0004] It is evident that although there are currently several methods for synthesizing diisopropylamine silane, all of them suffer from unavoidable problems. Therefore, providing a convenient and efficient method for preparing diisopropylamine silane, avoiding the need for prior preparation of complex catalysts, high-temperature and high-pressure reaction environments, and hazardous reaction raw materials, while achieving high yield and high purity, is a pressing technical problem to be solved in this field. Summary of the Invention

[0005] To address the aforementioned technical problems, this invention provides a method for preparing diisopropylamine silane. This invention primarily optimizes existing methods for synthesizing diisopropylamine silane by preferentially reacting diisopropylamine and dichlorosilane, followed by reduction with lithium hydride to obtain diisopropylamine silane. This method not only eliminates the need for pre-preparation of a catalyst through complex steps but also utilizes mild reaction conditions, avoids the use of hazardous raw materials such as silane, and generates no hydrogen during the reaction, achieving both high yield and high purity.

[0006] To achieve this objective, the present invention adopts the following technical solution:

[0007] This invention provides a method for preparing diisopropylamine silane, the method comprising the following steps:

[0008] (1) Dichlorosilane reacts with diisopropylamine to give diisopropylaminechlorosilane;

[0009] (2) The diisopropylamine chlorosilane obtained in step (1) is reacted with lithium hydride to obtain the diisopropylamine silane;

[0010] The reaction formula for the preparation method is as follows:

[0011]

[0012] The method for preparing diisopropylamine silane provided by this invention does not require the preparation of a catalyst through complex steps in advance, and only uses raw materials such as dichlorosilane, diisopropylamine and lithium hydride, thus avoiding the use of dangerous and expensive raw materials. In addition, the reaction conditions are mild and the product yield and purity are high.

[0013] In this invention, the use of dichlorosilane avoids high-temperature and high-pressure reaction conditions and the generation of dangerous byproducts such as hydrogen; the use of lithium hydride reducing agent reduces the danger of the reaction and improves the convenience of the reaction; at the same time, all reaction steps do not require extremely low temperatures, and 0-25°C is sufficient to meet the requirements, thus reducing energy consumption.

[0014] Preferably, the molar ratio of dichlorosilane and diisopropylamine in step (1) is 1:(2 to 2.05), for example, it can be 1:2, 1:2.02, 1:2.04 or 1:2.05, etc.

[0015] In this invention, a specific molar ratio of dichlorosilane to diisopropylamine is beneficial for improving the yield of the target product. The best technical effect is achieved when the molar ratio is 1:(2-2.05). If the molar ratio is lower than 1:2, diisopropylamine cannot completely react with the generated hydrochloric acid to form diisopropylamine hydrochloride compound, resulting in an excessively high concentration of hydrochloric acid in the reaction system, which prevents the reaction from proceeding normally, reduces the product yield, and causes harm to the human body due to the volatilization of hydrochloric acid. If the molar ratio is higher than 1:2.05, excess diisopropylamine will react with the intermediate diisopropylaminechlorosilane to generate bis(diisopropylamine)silane, thereby affecting the reduction of the intermediate and reducing the product yield and purity.

[0016] Preferably, the reaction in step (1) is carried out in the presence of a solvent.

[0017] Preferably, the reaction specifically includes: mixing dichlorosilane and a solvent and cooling, adding diisopropylamine, and reacting to obtain diisopropylaminechlorosilane.

[0018] Preferably, the mixing is carried out under stirring.

[0019] Preferably, the cooling is to -20 to -10°C, for example, -20°C, -15°C, or -10°C. Preferably, the temperature change of the system is controlled to be less than 5°C during the addition of diisopropylamine.

[0020] Preferably, the dichlorosilane is added to the system by introducing gas from a gas cylinder.

[0021] Preferably, the diisopropylamine is added dropwise through a constant-pressure dropping funnel.

[0022] Preferably, the temperature of the reaction in step (1) is 0 to 25°C, for example, 0°C, 5°C, 10°C, 15°C, 20°C or 25°C, and the reaction time is 1 to 8 hours, for example, 1 hour, 2 hours, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours or 8 hours, preferably 3 to 5 hours.

[0023] The preparation method provided by the present invention has a wide reaction temperature range in step (1), which can be adjusted according to the actual production situation; at the same time, this specific temperature range indicates that the preparation method does not require extremely low temperature during the preparation process, and 25°C is sufficient to meet the requirements, thus reducing energy consumption.

[0024] Preferably, the solvent is a hydrocarbon solvent.

[0025] Preferably, the hydrocarbon solvent includes C5 to C64. 12 Alkanes (e.g., C5 alkanes, C6 alkanes, C7 alkanes, C8 alkanes, C9 alkanes, C4 alkanes, C5 alkanes, C6 alkanes, C7 alkanes, C8 alkanes, C9 ...9 alkanes, C9 alkanes, C9 alkanes, C9 alkanes, C9 alkan 10 Alkanes, C 11 Alkanes or C12 Alkanes), preferably any one or a combination of at least two of n-pentane, n-hexane or n-heptane, and more preferably n-hexane.

[0026] The hydrocarbon solvent used in this invention is preferably n-pentane, n-hexane, or n-heptane, which reduces reaction costs, is non-coordinated, and is non-toxic to humans.

[0027] Preferably, the molar ratio of the dichlorosilane in step (1) to the lithium hydride in step (2) is 1:(2 to 2.2), for example, it can be 1:2, 1:2.05, 1:2.1, 1:2.15 or 1:2.2, etc.

[0028] In this invention, a specific molar ratio of dichlorosilane to lithium hydride is beneficial to improving the yield of the target product. The best technical effect is achieved when the molar ratio is 1:(2 to 2.2). If the molar ratio is lower than 1:2, the reduction time of the diisopropylaminechlorosilane generated in the first stage is longer and it cannot be completely reduced, resulting in a decrease in product yield and purity. If the molar ratio is higher than 1:2.2, not only will the production cost increase, but the excess lithium hydride will also reduce the generated diisopropylaminesilane to silane, which will also cause a decrease in product yield and purity.

[0029] Preferably, the reaction in step (2) specifically includes: filtering the reaction system obtained in step (1) to obtain a reaction solution containing diisopropylamine chlorosilane; cooling the reaction solution and then adding lithium hydride to obtain the diisopropylamine silane through the reaction.

[0030] In this invention, the reaction system obtained in step (1) is filtered to remove the diisopropylamine hydrochloride compound, and a reaction solution containing diisopropylamine chlorosilane is obtained.

[0031] Preferably, the cooling is to a temperature of -20 to -10°C, for example, -20°C, -15°C, or -10°C.

[0032] Preferably, the lithium hydride is added in batches, preferably in 2 to 4 batches (e.g., 2, 3 or 4).

[0033] Preferably, the lithium hydride is added using a solid feeder.

[0034] In this invention, lithium hydride is added using a solid feeder in batches. This not only avoids the risk of byproducts caused by local heat accumulation (excessive local lithium hydride concentration will reduce diisopropylamine silane to silane), but also ensures that the raw materials are fully contacted and reacted, thereby improving the yield.

[0035] Preferably, the temperature change of the system is controlled to be less than 5°C during the addition of lithium hydride.

[0036] Preferably, the temperature of the reaction in step (2) is 0 to 25°C, for example, 0°C, 5°C, 10°C, 15°C, 20°C or 25°C, and the reaction time is 5 to 10 hours, for example, 5 hours, 6 hours, 7 hours, 8 hours, 9 hours or 10 hours, preferably 5 to 8 hours.

[0037] Preferably, both the reaction in step (1) and the reaction in step (2) are carried out under a protective gas atmosphere.

[0038] Preferably, the protective gas includes any one or a combination of at least two of nitrogen, argon, or helium.

[0039] Preferably, after the reaction in step (2), the reaction system is further filtered, and the filtrate is distilled under normal pressure and under reduced pressure to obtain the diisopropylamine silane.

[0040] In this invention, after the reaction in step (2), the reaction system is filtered to remove lithium chloride, and then the hydrocarbon solvent is removed by atmospheric distillation. The fraction at 50-52℃ / 100-105mmHg is collected by vacuum distillation to obtain diisopropylamine silane.

[0041] Compared with the prior art, the present invention has at least the following beneficial effects:

[0042] (1) The preparation method of diisopropylamine silane provided by the present invention does not require a catalyst prepared through complex steps, which simplifies the synthesis method; the raw materials are simple and readily available, and there is no need to use highly flammable raw materials such as silane and silane; the reaction conditions are mild, no high temperature and high pressure environment is required, and no high-risk by-products (such as hydrogen) are generated, which improves the safety and convenience of the reaction; the use of lithium hydride, a simple and readily available reducing agent, reduces the cost of raw materials and the danger.

[0043] (2) Through the synthesis method of the present invention, the product yield is greatly improved to 90.3% and the purity can reach 98.9%, which is conducive to large-scale industrial production. Attached Figure Description

[0044] Figure 1 It is the diisopropylamine silane prepared in Example 1. 1 Nuclear magnetic resonance (NMR) image of H NMR. Detailed Implementation

[0045] To facilitate understanding of the present invention, the following embodiments are provided. Those skilled in the art should understand that these embodiments are merely illustrative and should not be construed as limiting the scope of the invention.

[0046] Example 1

[0047] This embodiment provides a method for preparing diisopropylamine silane, the method comprising the following steps:

[0048] (1) Under N2 atmosphere, dichlorosilane gas (10g, 0.099mol) and 300mL of n-hexane were added to a 500mL three-necked reaction flask, cooled to -10℃, and diisopropylamine (20g, 0.198mol) was slowly added dropwise to the reaction flask at a rate of 0.35g / min. During this period, the temperature change of the system was kept not more than 5℃. After the gas was purged, the reaction was carried out at 25℃ for 3h.

[0049] (2) The generated diisopropylamine hydrochloride was removed by filtration, and the temperature was lowered to -10°C. Lithium hydride powder (1.57 g, 0.198 mol) was added to the reaction flask in three batches, and the temperature change of the reaction system was controlled to be less than 5°C. After the lithium hydride was added, the reaction was carried out at 25°C for 5 h under N2 atmosphere. After the reaction was completed, the reaction solution was filtered to remove the generated lithium chloride, and n-hexane was evaporated at 70°C. Then the apparatus was replaced with a vacuum distillation apparatus, and the fraction at 50°C / 100 mmHg was collected to obtain 11.61 g of colorless liquid diisopropylamine silane (yield: 89.3%).

[0050] The NMR characterization data of the obtained compound diisopropylamine silane are as follows (NMR test results are shown in the figure). Figure 1 As shown):

[0051] 1 H NMR (400MHz, C6D6): δ4.56 (s, 3H), 2.93 (m, 2H), 1.03 (d, J = 6.7Hz, 12H).

[0052] Example 2

[0053] This embodiment provides a method for preparing diisopropylamine silane, the method comprising the following steps:

[0054] (1) Under N2 atmosphere, dichlorosilane gas (10g, 0.099mol) and 300mL of n-hexane were added to a 500mL three-necked reaction flask, cooled to -10℃, and diisopropylamine (20.5g, 0.203mol) was slowly added dropwise to the reaction flask at a rate of 0.35g / min. During this period, the temperature change of the system was kept not more than 5℃. After the gas was purged, the reaction was carried out at 25℃ for 5h.

[0055] (2) The generated diisopropylamine hydrochloride was removed by filtration, and the temperature was lowered to -10°C. Lithium hydride powder (1.73 g, 0.218 mol) was added to the reaction flask in three batches, and the temperature change of the reaction system was controlled to be less than 5°C. After the lithium hydride was added, the reaction was carried out at 25°C for 7 h under N2 atmosphere. After the reaction was completed, the reaction solution was filtered to remove the generated lithium chloride, and n-hexane was evaporated at 70°C. Then the apparatus was replaced with a vacuum distillation apparatus, and the fraction at 51°C / 102 mmHg was collected to obtain 11.74 g of colorless liquid diisopropylamine silane (yield: 90.3%).

[0056] The NMR characterization data of the obtained compound, diisopropylamine silane, are as follows:

[0057] 1 H NMR (400MHz, C6D6): δ4.56 (s, 3H), 2.92 (m, 2H), 1.02 (d, J = 6.7Hz, 12H).

[0058] Example 3

[0059] This embodiment provides a method for preparing diisopropylamine silane, the method comprising the following steps:

[0060] (1) Under N2 atmosphere, dichlorosilane gas (10.5g, 0.104mol) and 300mL of n-hexane were added to a 500mL three-necked reaction flask, cooled to -10℃, and diisopropylamine (21g, 0.208mol) was slowly added dropwise to the reaction flask at a rate of 0.35g / min. During this period, the temperature change of the system was kept not more than 5℃. After the gas was purged, the reaction was carried out at 25℃ for 1h.

[0061] (2) The generated diisopropylamine hydrochloride was removed by filtration, and the temperature was lowered to -10°C. Lithium hydride powder (1.65 g, 0.208 mol) was added to the reaction flask in three batches, and the temperature change of the reaction system was controlled to be less than 5°C. After the lithium hydride was added, the reaction was carried out at 25°C for 5 h under N2 atmosphere. After the reaction was completed, the reaction solution was filtered to remove the generated lithium chloride, and n-hexane was evaporated at 70°C. Then the apparatus was replaced with a vacuum distillation apparatus, and the fraction at 52°C / 105 mmHg was collected to obtain 7.30 g of colorless liquid diisopropylamine silane (yield: 53.5%).

[0062] The NMR characterization data of the obtained compound, diisopropylamine silane, are as follows:

[0063] 1 H NMR (400MHz, C6D6): δ4.56 (s, 3H), 2.92 (m, 2H), 1.03 (d, J = 6.7Hz, 12H).

[0064] Example 4

[0065] This embodiment provides a method for preparing diisopropylamine silane, the method comprising the following steps:

[0066] (1) Under N2 atmosphere, dichlorosilane gas (12.5g, 0.124mol) and 300mL of n-hexane were added to a 500mL three-necked reaction flask, cooled to -10℃, and diisopropylamine (25g, 0.248mol) was slowly added dropwise to the reaction flask at a rate of 0.35g / min. During this period, the temperature change of the system was kept not more than 5℃. After the gas was purged, the reaction was carried out at 0℃ for 5h.

[0067] (2) The generated diisopropylamine hydrochloride was removed by filtration, and the temperature was lowered to -10°C. Lithium hydride powder (1.97 g, 0.248 mol) was added to the reaction flask in three batches, and the temperature change of the reaction system was controlled to be less than 5°C. After the lithium hydride was added, the reaction was carried out at 0°C under N2 atmosphere for 8 h. After the reaction was completed, the reaction solution was filtered to remove the generated lithium chloride, and n-hexane was evaporated at 70°C. Then the apparatus was replaced with a vacuum distillation apparatus, and the fraction at 50°C / 103 mmHg was collected to obtain 14.45 g of colorless liquid diisopropylamine silane (yield: 88.9%).

[0068] The NMR characterization data of the obtained compound, diisopropylamine silane, are as follows:

[0069] 1 H NMR (400MHz, C6D6): δ4.55 (s, 3H), 2.93 (m, 2H), 1.01 (d, J = 6.7Hz, 12H).

[0070] Example 5

[0071] This embodiment provides a method for preparing diisopropylamine silane. The only difference between this method and that of Example 1 is that in step (2), lithium hydride (1.57g, 0.198mol) is changed to lithium hydride (2.36g, 0.297mol). The other raw materials, contents and methods are the same as in Example 1, and 10.44g of colorless liquid diisopropylamine silane is obtained (yield: 80.3%).

[0072] The NMR characterization data of the obtained compound, diisopropylamine silane, are as follows:

[0073] 1 H NMR (400MHz, C6D6): δ4.57 (s, 3H), 2.92 (m, 2H), 1.03 (d, J = 6.7Hz, 12H).

[0074] Example 6

[0075] This embodiment provides a method for preparing diisopropylamine silane. The only difference between this method and Example 1 is that in step (2), lithium hydride (1.57g, 0.198mol) is changed to lithium hydride (1.18g, 0.149mol). Other raw materials, contents and methods are the same as in Example 1, and 8.76g of colorless liquid diisopropylamine silane is obtained (yield: 67.4%).

[0076] The NMR characterization data of the obtained compound, diisopropylamine silane, are as follows:

[0077] 1 H NMR (400MHz, C6D6): δ4.56 (s, 3H), 2.91 (m, 2H), 1.02 (d, J = 6.7Hz, 12H).

[0078] Example 7

[0079] This embodiment provides a method for preparing diisopropylamine silane. The only difference between this method and Example 1 is that in step (1), diisopropylamine (20g, 0.198mol) is adjusted to diisopropylamine (30g, 0.297mol). The other raw materials, contents and methods are the same as in Example 1, and 8.90g of colorless liquid diisopropylamine silane is obtained (yield: 68.5%).

[0080] The NMR characterization data of the obtained compound, diisopropylamine silane, are as follows:

[0081] 1 H NMR (400MHz, C6D6): δ4.55 (s, 3H), 2.92 (m, 2H), 1.01 (d, J = 6.7Hz, 12H).

[0082] Example 8

[0083] This embodiment provides a method for preparing diisopropylamine silane. The only difference between this method and Example 1 is that in step (1), diisopropylamine (20g, 0.198mol) is adjusted to diisopropylamine (18g, 0.178mol). The other raw materials, contents and methods are the same as in Example 1, and 11.13g of colorless liquid diisopropylamine silane is obtained (yield: 85.6%).

[0084] The NMR characterization data of the obtained compound, diisopropylamine silane, are as follows:

[0085] 1 H NMR (400MHz, C6D6): δ4.57 (s, 3H), 2.92 (m, 2H), 1.03 (d, J = 6.7Hz, 12H).

[0086] Comparative Example 1

[0087] This comparative example provides a method for preparing diisopropylamine silane. The only difference between this method and Example 1 is that in step (2), lithium hydride (1.57 g, 0.198 mol) is replaced with sodium hydride (4.75 g, 0.198 mol). The other raw materials, contents and methods are the same as in Example 1, and no product was obtained.

[0088] Comparative Example 2

[0089] This comparative example provides a method for preparing diisopropylamine silane. The only difference between this method and Example 1 is that in step (2), lithium hydride (1.57 g, 0.198 mol) is replaced with lithium aluminum hydride (7.51 g, 0.298 mol). The other raw materials, contents and methods are the same as in Example 1, and 4.60 g of colorless liquid diisopropylamine silane is obtained (yield: 35.4%).

[0090] Comparative Example 3

[0091] This comparative example provides a method for preparing diisopropylamine silane. The only difference between this method and Example 1 is that in step (2), lithium hydride (1.57 g, 0.198 mol) is replaced with diisobutylaluminum hydride (28.1 g, 0.198 mol). The other raw materials, contents and methods are the same as in Example 1, and 1.63 g of colorless liquid diisopropylamine silane is obtained (yield: 12.5%).

[0092] Comparative Example 4

[0093] This comparative example provides a method for preparing diisopropylamine silane. The only difference between this method and Example 1 is that in step (2), lithium hydride (1.57 g, 0.198 mol) is replaced with lithium borohydride (4.31 g, 0.198 mol). The other raw materials, contents and methods are the same as in Example 1, and 2.57 g of colorless liquid diisopropylamine silane is obtained (yield: 19.8%).

[0094] Comparative Example 5

[0095] This comparative example provides a method for preparing diisopropylamine silane. The only difference between this method and Example 1 is that in step (2), lithium hydride (1.57 g, 0.198 mol) is replaced with lithium borohydride (1.53 g, 0.07 mol). The other raw materials, contents and methods are the same as in Example 1, and 4.59 g of colorless liquid diisopropylamine silane is obtained (yield: 35.3%).

[0096] The yields and purities of the diisopropylamine silanes obtained in Examples 1-8 and Comparative Examples 1-5 are shown in Table 1.

[0097] Table 1

[0098]

[0099]

[0100] The test results show that:

[0101] (1) As can be seen from Examples 1-8, the method for preparing diisopropylamine silane provided by the present invention not only does not require the preparation of catalysts through complex steps in advance, but also does not require the use of silane and other high-risk raw materials such as silane. Furthermore, the reaction conditions are mild, no high-risk byproducts (such as hydrogen) are generated during the reaction, the reaction process is safe, and the product yield and purity are high, making it suitable for industrial scale-up production.

[0102] (2) A comparison between Example 1 and Example 3 shows that if the reaction time is too short, the yield and purity of the target product will decrease. A comparison between Example 1 and Examples 5-8 shows that when the amount of diisopropylamine and lithium hydride is too high or too low compared to dichlorosilane, the yield and purity of the target product will decrease.

[0103] (3) As can be seen from the comparison between Example 1 and Comparative Examples 1-5, the selection of lithium hydride as a specific reducing agent in the technical solution of the present invention can obtain the target product diisopropylamine silane with higher yield and purity.

[0104] In summary, this invention optimizes the existing method for preparing diisopropylamine silane, using readily available and simple raw materials, a simple reaction process and operation, mild reaction conditions, and a safe reaction process with no dangerous byproducts. Furthermore, the target product obtained has high yield and purity, which is beneficial for large-scale industrial production.

[0105] The applicant declares that the above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.

Claims

1. A method for preparing diisopropylamine silane, characterized in that, The preparation method includes the following steps: (1) Dichlorosilane reacts with diisopropylamine to give diisopropylaminechlorosilane; (2) The diisopropylamine chlorosilane obtained in step (1) is reacted with lithium hydride to obtain the diisopropylamine silane; The reaction formula for the preparation method is as follows:

2. The preparation method according to claim 1, characterized in that, The molar ratio of dichlorosilane and diisopropylamine in step (1) is 1:(2 to 2.05).

3. The preparation method according to claim 1 or 2, characterized in that, The reaction described in step (1) is carried out in the presence of a solvent; Preferably, the reaction specifically includes: mixing dichlorosilane and a solvent and cooling, adding diisopropylamine, and reacting to obtain diisopropylaminechlorosilane; Preferably, the cooling is to a temperature of -20 to -10°C; Preferably, the temperature change of the system is controlled to be less than 5°C during the addition of diisopropylamine; Preferably, the temperature of the reaction in step (1) is 0 to 25°C, and the reaction time is 1 to 8 hours, preferably 3 to 5 hours.

4. The preparation method according to claim 3, characterized in that, The solvent is a hydrocarbon solvent; Preferably, the hydrocarbon solvent includes C5 to C64. 12 Alkanes, preferably any one or a combination of at least two of n-pentane, n-hexane or n-heptane, more preferably n-hexane.

5. The preparation method according to any one of claims 1-4, characterized in that, The molar ratio of the dichlorosilane in step (1) to the lithium hydride in step (2) is 1:(2~2.2).

6. The preparation method according to any one of claims 1-5, characterized in that, The reaction in step (2) specifically includes: filtering the reaction system obtained in step (1) to obtain a reaction solution containing diisopropylamine chlorosilane; cooling the reaction solution and then adding lithium hydride to obtain the diisopropylamine silane through the reaction.

7. The preparation method according to claim 6, characterized in that, The cooling is to reduce the temperature to -20 to -10°C; Preferably, the lithium hydride is added in batches, preferably in 2 to 4 batches; Preferably, the temperature change of the system is controlled to be less than 5°C during the addition of lithium hydride.

8. The preparation method according to any one of claims 1-7, characterized in that, The reaction temperature in step (2) is 0 to 25°C, and the reaction time is 5 to 10 hours, preferably 5 to 8 hours.

9. The preparation method according to any one of claims 1-8, characterized in that, Both the reaction described in step (1) and the reaction described in step (2) are carried out under a protective gas atmosphere; Preferably, the protective gas includes any one or a combination of at least two of nitrogen, argon, or helium.

10. The preparation method according to any one of claims 1-9, characterized in that, Step (2) further includes filtering the reaction system, and distilling the filtrate under normal and reduced pressure to obtain the diisopropylamine silane.

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