Preparation method of diisopropylamine silane

Abstract

The invention relates to a preparation method of diisopropylamine silane, and belongs to the technical field of synthesis of organosilicon compounds. The method comprises the following steps: under the protection of argon, adding a solvent into a reactor, slowly dropwise adding a lithium diisopropylamide solution, and controlling the dropwise adding speed to control the reaction temperature at-5 to 0 DEG C; under the condition of continuous stirring, slowly dropwise adding iodosilane; after dropwise adding, heating the reaction system, and continuously stirring for reaction; and after the reaction is completed, adding aminocarboxylic acid-MOF composite chelating resin, stirring, filtering to remove insoluble substances, carrying out reduced pressure distillation to remove the solvent, and finally, carrying out rectification purification to obtain high-purity diisopropylamine silane. The amino carboxylic acid-MOF composite chelating resin is prepared from chloromethylated resin, zirconium aminobenzenedicarboxylate (MOF), dichloroethane, disodium iminodiacetate, 2-amino-1, 3, 5-triazine and sodium hydroxide, and the amino carboxylic acid-MOF composite chelating resin is prepared from the chloromethylated resin, zirconium aminobenzenedicarboxylate (MOF), dichloroethane, disodium iminodiacetate, 2-amino-1, 3 The purity of the prepared diisopropylamine silane reaches 99% or above, and the purity grade of metal ions reaches 6N grade.

Description

Technical Field

[0001] The invention relates to the technical field of organosilicon compound synthesis, in particular to a method for preparing diisopropylamine silane. Background Art

[0002] Diisopropylamine silane is an organosilicon compound primarily used in the semiconductor industry for high-k dielectric films, passivation and spacer layers, DRAM capacitor dielectrics, and 3D NAND memories. Its advantages include low-temperature deposition, high step coverage, low carbon contamination, and high purity adaptability. It is an indispensable precursor in advanced semiconductor manufacturing processes, particularly in the fabrication of high-k dielectrics and 3D structures.

[0003] CN104876957B provides a method for synthesizing organoaminosilanes, and describes a method for preparing organoaminosilane compounds or other compounds such as organoaminodisilanes and organoaminocarbosilanes by catalytic hydrosilylation of a silicon source containing hydrosilane with imine.

[0004] CN115260223A discloses a method for preparing diisopropylamine silane using a chlorine-free catalyst. The method utilizes the inexpensive chlorine-free compounds calcium bis(hexamethyldisilazide) and / or strontium bis(hexamethyldisilazide) as a novel catalyst to efficiently catalyze the dehydrogenative coupling reaction of monosilane and diisopropylamine, resulting in a one-step synthesis of diisopropylamine silane with a yield of 40-65%.

[0005] CN118184688A provides a method for preparing diisopropylamine silane, comprising the steps of reacting diisopropylamine silane with pinacol borane in the presence of a first catalyst to form diisopropylamine silane and pinacol phenylboronic acid ester, wherein the first catalyst is borane or a solution thereof. The method for preparing diisopropylamine silane provided by this method facilitates separation and purification, and also exhibits high selectivity, significantly reducing the generation of by-products.

[0006] CN117737705A provides a method for forming a silicon oxide film. The method uses a ruthenium-supported molecular sieve catalyst to catalyze the reaction of diisopropylamine and phenylsilane, followed by distillation purification, to obtain high-purity diisopropylamine silane with a vapor phase purity of 98.7-99.6%. This is then used as a silicon source to form a silicon oxide film via plasma chemical vapor deposition.

[0007] CN117143139A The present invention relates to a method for synthesizing diisopropylaminosilane and its application. The method comprises the following steps: filling a tubular reactor with a solid-phase catalyst, then introducing monosilane and diisopropylamine into the reactor for reaction, and separating and purifying the resulting reaction solution to obtain the diisopropylaminosilane; the solid-phase catalyst comprises a CuH active component and a resin carrier. The present invention utilizes a solid-phase catalyst composed of the active component CuH and the resin carrier to achieve continuous or semi-continuous preparation of diisopropylaminosilane.

[0008] CN117510533A provides a preparation process and system for diisopropylamine silane, which uses dichloromethane and metallic sodium instead of ether, and uses monochlorosilane and diisopropylamine as raw materials to prepare diisopropylamine silane, thereby avoiding the explosion caused by oxidation of ether during the preparation process.

[0009] The prior art of the aforementioned patent suffers from low reaction yields, the use of monochlorosilane and diisopropylamine as raw materials easily produces a large amount of hydrochloride as a byproduct, and the catalyst used can also introduce metallic impurities. With the advancement of semiconductor technology nodes, the purity requirements for precursor materials are becoming increasingly stringent, and the chlorine content of silicon-based precursors is required to be below 1 ppm. Therefore, to overcome these issues, the present invention provides a novel method for preparing diisopropylamine silane. Summary of the Invention

[0010] In order to solve the above problems, the present invention provides a method for preparing diisopropylamine silane, the operating steps of which are as follows, calculated by weight:

[0011] S1 Raw material mixing: Under the protection of argon, add 200-400 parts of solvent to the reactor, slowly add 110-135 parts of lithium diisopropylamide solution dropwise, and control the dropwise addition rate to keep the reaction temperature at -5 to 0°C; under continuous stirring, slowly add 45-55 parts of iodosilane dropwise, and maintain the reaction temperature;

[0012] S2 temperature rise reaction: after the dropwise addition is completed, the reaction system is heated to a high temperature and the reaction is continued with stirring;

[0013] S3 post-treatment: After the reaction is completed, add 10-20 parts of aminocarboxylic acid-MOF composite chelating resin, stir for 100-180 minutes, filter to remove insoluble matter, remove the solvent by reduced pressure distillation, and finally purify by distillation to obtain high-purity diisopropylamine silane.

[0014] As a preferred embodiment of the present invention, the solvent in S1 is n-hexane or carbon tetrachloride.

[0015] As a preferred embodiment of the present invention, the stirring rate of S1 is 300-500 rpm.

[0016] As a preferred embodiment of the present invention, the reaction temperature of S2 is 20-40° C. and the reaction time is 1-4 hours.

[0017] As a preferred embodiment of the present invention, the pressure of the reduced pressure distillation in S3 is 50-70 mmHg and the temperature is 60-70°C.

[0018] As a preferred embodiment of the present invention, the distillation in S3 adopts a high-efficiency fractionating tower with a top pressure of 80-100 mmHg, a top temperature of 80-90°C, a bottom temperature of 105-115°C, and a reflux ratio of 4-8:1.

[0019] As a preferred embodiment of the present invention, the preparation method of the aminocarboxylic acid-MOF composite chelating resin is as follows, calculated by weight:

[0020] H1: Disperse 100-150 parts of chloromethylated resin and 2-5 parts of zirconium aminophthalate MOF in 1000-1200 parts of dichloroethane and stir to swell for 1-4 hours;

[0021] H2: Add 5-10 parts of disodium iminodiacetate, 1-3 parts of 2-amino-1,3,5-triazine, and 3-7 parts of sodium hydroxide to the H1 system, stir and react at 70-80°C for 5-8h, and vacuum dry at 60-70°C to obtain an aminocarboxylic acid-MOF composite chelating resin.

[0022] Reaction mechanism:

[0023] In a low-temperature environment protected by argon, the amino anion of lithium diisopropylamide ((i-Pr)2N-) acts as a nucleophile to attack the silicon atom of iodosilane, and the nucleophilic substitution reaction (S n (Mechanism 2) The intermediate product, lithium diisopropylaminosilane, is formed, with the iodide ion acting as a leaving group. The low temperature effectively inhibits the self-polymerization of the amino anion and the decomposition of the silane, laying the foundation for subsequent reactions.

[0024] Upon heating, the intermediate product undergoes further substitution reactions and molecular rearrangement, fully bonding the diisopropylamine groups to the silicon atoms and forming the target product's skeleton. In the post-processing stage, the aminocarboxylic acid-MOF composite chelating resin forms a stable chelate with lithium ions via the aminocarboxylic acid groups. The porous structure of the MOF enhances adsorption capacity, and combined with the boiling point separation of distillation, a high-purity product is ultimately achieved.

[0025] Technical effects:

[0026] The present invention provides a method for preparing diisopropylamine silane. Compared with the prior art, the present invention has the following significant effects:

[0027] 1. The present invention can significantly reduce the occurrence of side reactions through the synergistic effect of low-temperature dropwise addition and specific chelating resin. Combined with efficient distillation, the product purity can reach more than 99%, meeting the purity requirements of high-end materials.

[0028] 2. The process design takes into account both efficiency and economy: the stirring rate and the high solubility of n-hexane / carbon tetrachloride improve the mass transfer efficiency, which can increase the utilization rate of raw materials and shorten the reaction time; the solvent and chelating resin are recyclable and reusable, which significantly reduces the production cost. At the same time, the wide range of operating parameters (such as temperature and pressure) enhances the controllability and equipment compatibility of industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 This is a simplified diagram of the process flow.

[0030] Figure 2 This is the NMR spectrum of diisopropylaminesilane.

[0031] Figure 3 This is the GC spectrum of diisopropylaminesilane. DETAILED DESCRIPTION

[0032] In order to further illustrate the technical means and effects adopted by the present invention to achieve the predetermined purpose of the invention, the specific implementation methods, structures, features and effects of the present invention are described in detail below in conjunction with the accompanying drawings and preferred embodiments.

[0033] 1. Metal ion impurity content: ICP-OES / MS is used for analysis and detection.

[0034] 2. Purity of diisopropylaminesilane: GC is used for analysis and detection.

[0035] Example 1

[0036] A preparation method of diisopropylamine silane, the operating steps are:

[0037] S1: Mixing raw materials: Under the protection of argon, add 200g of solvent to the reactor, slowly add 110g of lithium diisopropylamide solution dropwise, and control the dropwise addition rate to keep the reaction temperature at -5°C; under continuous stirring, slowly add 45g of iodosilane dropwise to maintain the reaction temperature;

[0038] S2 temperature rise reaction: after the dropwise addition is completed, the reaction system is heated to a high temperature and the reaction is continued with stirring;

[0039] S3 post-treatment: After the reaction is completed, 10 g of aminocarboxylic acid-MOF composite chelating resin is added, stirred for 100 minutes, insoluble matter is removed by filtration, the solvent is removed by reduced pressure distillation, and finally purified by distillation to obtain high-purity diisopropylamine silane.

[0040] The solvent in S1 is n-hexane.

[0041] The stirring rate of S1 is 300 rpm.

[0042] The reaction temperature of S2 is 20°C and the reaction time is 1 hour.

[0043] The pressure of the reduced pressure distillation in S3 is 50 mmHg and the temperature is 60°C.

[0044] The distillation in S3 adopts a high-efficiency fractionating tower with a top pressure of 80 mmHg, a top temperature of 80° C., a bottom temperature of 105° C., and a reflux ratio of 4:1.

[0045] The preparation method of the aminocarboxylic acid-MOF composite chelating resin is as follows:

[0046] H1: Disperse 100 g of chloromethylated resin and 2 g of aminophthalate zirconium MOF (CAS: 1260119-00-3) in 1000 g of dichloroethane and stir to swell for 1 h;

[0047] H2: Add 5 g of disodium iminodiacetate, 1 g of 2-amino-1,3,5-triazine, and 3 g of sodium hydroxide to the H1 system, stir and react at 70°C for 5 h, and vacuum dry at 60°C to obtain an aminocarboxylic acid-MOF composite chelating resin.

[0048] Example 2

[0049] A preparation method of diisopropylamine silane, the operating steps are:

[0050] S1 Raw material mixing: Under the protection of argon, add 250g of solvent to the reactor, slowly add 118g of lithium diisopropylamide solution dropwise, and control the dropwise addition rate to keep the reaction temperature at -5°C; under continuous stirring, slowly add 48g of iodosilane dropwise, and maintain the reaction temperature;

[0051] S2 temperature rise reaction: after the dropwise addition is completed, the reaction system is heated to a high temperature and the reaction is continued with stirring;

[0052] S3 post-treatment: After the reaction is completed, 13 g of aminocarboxylic acid-MOF composite chelating resin is added, stirred for 120 minutes, insoluble matter is removed by filtration, the solvent is removed by reduced pressure distillation, and finally purified by distillation to obtain high-purity diisopropylamine silane.

[0053] The solvent in S1 is n-hexane.

[0054] The stirring rate of S1 is 400 rpm.

[0055] The reaction temperature of S2 is 25°C and the reaction time is 2 hours.

[0056] The pressure of the reduced pressure distillation in S3 is 60 mmHg and the temperature is 65°C.

[0057] The distillation in S3 adopts a high-efficiency fractionating tower with a top pressure of 90 mmHg, a top temperature of 85° C., a bottom temperature of 110° C., and a reflux ratio of 5:1.

[0058] The preparation method of the aminocarboxylic acid-MOF composite chelating resin is as follows:

[0059] H1: Disperse 110 g of chloromethylated resin and 3 g of aminophthalate zirconium MOF (CAS: 1260119-00-3) in 1050 g of dichloroethane and stir to swell for 2 h;

[0060] H2: Add 6 g of disodium iminodiacetate, 2 g of 2-amino-1,3,5-triazine, and 4 g of sodium hydroxide to the H1 system, stir and react at 75°C for 6 h, and vacuum dry at 65°C to obtain an aminocarboxylic acid-MOF composite chelating resin.

[0061] Example 3

[0062] A preparation method of diisopropylamine silane, the operating steps are:

[0063] S1 Raw material mixing: Under the protection of argon, add 350g of solvent to the reactor, slowly add 130g of lithium diisopropylamide solution dropwise, and control the dropwise addition rate to keep the reaction temperature at 0°C; under continuous stirring, slowly add 53g of iodosilane dropwise, and maintain the reaction temperature;

[0064] S2 temperature rise reaction: after the dropwise addition is completed, the reaction system is heated to a high temperature and the reaction is continued with stirring;

[0065] S3 post-treatment: After the reaction is completed, 18 g of aminocarboxylic acid-MOF composite chelating resin is added, stirred for 160 minutes, insoluble matter is removed by filtration, the solvent is removed by reduced pressure distillation, and finally purified by distillation to obtain high-purity diisopropylamine silane.

[0066] The solvent in the S1 is carbon tetrachloride.

[0067] The stirring rate of S1 is 400 rpm.

[0068] The reaction temperature of S2 is 35° C. and the reaction time is 3 hours.

[0069] The pressure of the reduced pressure distillation in S3 is 60 mmHg and the temperature is 65°C.

[0070] The distillation in S3 adopts a high-efficiency fractionating tower with a top pressure of 90 mmHg, a top temperature of 85° C., a bottom temperature of 110° C., and a reflux ratio of 7:1.

[0071] The preparation method of the aminocarboxylic acid-MOF composite chelating resin is as follows:

[0072] H1: Disperse 140 g of chloromethylated resin and 4 g of aminophthalate zirconium MOF (CAS: 1260119-00-3) in 1150 g of dichloroethane and stir to swell for 3 h;

[0073] H2: Add 8 g of disodium iminodiacetate, 2 g of 2-amino-1,3,5-triazine, and 6 g of sodium hydroxide to the H1 system, stir and react at 75°C for 7 h, and vacuum dry at 65°C to obtain an aminocarboxylic acid-MOF composite chelating resin.

[0074] Example 4

[0075] A preparation method of diisopropylamine silane, the operating steps are:

[0076] S1 Raw material mixing: Under the protection of argon, add 400g of solvent to the reactor, slowly add 135g of lithium diisopropylamide solution dropwise, and control the dropwise addition rate to keep the reaction temperature at 0°C; under continuous stirring, slowly add 55g of iodosilane dropwise, and maintain the reaction temperature;

[0077] S2 temperature rise reaction: after the dropwise addition is completed, the reaction system is heated to a high temperature and the reaction is continued with stirring;

[0078] S3 post-treatment: After the reaction is completed, 20 g of aminocarboxylic acid-MOF composite chelating resin is added, stirred for 180 minutes, insoluble matter is removed by filtration, the solvent is removed by reduced pressure distillation, and finally purified by distillation to obtain high-purity diisopropylamine silane.

[0079] The solvent in the S1 is carbon tetrachloride.

[0080] The stirring rate of S1 is 500 rpm.

[0081] The reaction temperature of S2 is 40° C. and the reaction time is 4 hours.

[0082] The pressure of the reduced pressure distillation in S3 is 70 mmHg and the temperature is 70°C.

[0083] The distillation in S3 adopts a high-efficiency fractionating tower with a top pressure of 100 mmHg, a top temperature of 90° C., a bottom temperature of 115° C., and a reflux ratio of 8:1.

[0084] The preparation method of the aminocarboxylic acid-MOF composite chelating resin is as follows:

[0085] H1: Disperse 150 g of chloromethylated resin and 5 g of aminophthalate zirconium MOF (CAS: 1260119-00-3) in 1200 g of dichloroethane and stir to swell for 4 h;

[0086] H2: Add 10 g of disodium iminodiacetate, 3 g of 2-amino-1,3,5-triazine, and 7 g of sodium hydroxide to the H1 system, stir and react at 80°C for 8 h, and vacuum dry at 70°C to obtain an aminocarboxylic acid-MOF composite chelating resin.

[0087] Comparative Example 1

[0088] A preparation method of diisopropylamine silane, the operating steps are:

[0089] S1: Mixing raw materials: Under the protection of argon, add 200g of solvent to the reactor, slowly add 110g of lithium diisopropylamide solution dropwise, and control the dropwise addition rate to keep the reaction temperature at -5°C; under continuous stirring, slowly add 45g of iodosilane dropwise to maintain the reaction temperature;

[0090] S2 temperature rise reaction: after the dropwise addition is completed, the reaction system is heated to a high temperature and the reaction is continued with stirring;

[0091] S3 post-treatment: After the reaction is completed, the insoluble matter is removed by filtration, the solvent is removed by distillation under reduced pressure, and finally purified by distillation to obtain high-purity diisopropylamine silane.

[0092] The solvent in S1 is n-hexane.

[0093] The stirring rate of S1 is 300 rpm.

[0094] The reaction temperature of S2 is 20°C and the reaction time is 1 hour.

[0095] The pressure of the reduced pressure distillation in S3 is 50 mmHg and the temperature is 60°C.

[0096] The distillation in S3 adopts a high-efficiency fractionating tower with a top pressure of 80 mmHg, a top temperature of 80° C., a bottom temperature of 105° C., and a reflux ratio of 4:1.

[0097] Comparative Example 2

[0098] A preparation method of diisopropylamine silane, the operating steps are:

[0099] S1: Mixing raw materials: Under the protection of argon, add 200g of solvent to the reactor, slowly add 110g of lithium diisopropylamide solution dropwise, and control the dropwise addition rate to keep the reaction temperature at -5°C; under continuous stirring, slowly add 45g of iodosilane dropwise to maintain the reaction temperature;

[0100] S2 temperature rise reaction: after the dropwise addition is completed, the reaction system is heated to a high temperature and the reaction is continued with stirring;

[0101] S3 post-treatment: After the reaction is completed, 10 g of aminocarboxylic acid-MOF composite chelating resin is added, stirred for 100 minutes, insoluble matter is removed by filtration, the solvent is removed by reduced pressure distillation, and finally purified by distillation to obtain high-purity diisopropylamine silane.

[0102] The solvent in S1 is n-hexane.

[0103] The stirring rate of S1 is 300 rpm.

[0104] The reaction temperature of S2 is 20°C and the reaction time is 1 hour.

[0105] The pressure of the reduced pressure distillation in S3 is 50 mmHg and the temperature is 60°C.

[0106] The distillation in S3 adopts a high-efficiency fractionating tower with a top pressure of 80 mmHg, a top temperature of 80° C., a bottom temperature of 105° C., and a reflux ratio of 4:1.

[0107] The preparation method of the aminocarboxylic acid-MOF composite chelating resin is as follows:

[0108] H1: Disperse 100 g of chloromethylated resin and 2 g of aminophthalate zirconium MOF (CAS: 1260119-00-3) in 1000 g of dichloroethane and stir to swell for 1 h;

[0109] H2: Add 1 g of 2-amino-1,3,5-triazine and 3 g of sodium hydroxide to the H1 system, stir and react at 70°C for 5 h, and vacuum dry at 60°C to obtain an aminocarboxylic acid-MOF composite chelating resin.

[0110] Comparative Example 3

[0111] A preparation method of diisopropylamine silane, the operating steps are:

[0112] S1: Mixing raw materials: Under the protection of argon, add 200g of solvent to the reactor, slowly add 110g of lithium diisopropylamide solution dropwise, and control the dropwise addition rate to keep the reaction temperature at -5°C; under continuous stirring, slowly add 45g of iodosilane dropwise to maintain the reaction temperature;

[0113] S2 temperature rise reaction: after the dropwise addition is completed, the reaction system is heated to a high temperature and the reaction is continued with stirring;

[0114] S3 post-treatment: After the reaction is completed, 10 g of aminocarboxylic acid-MOF composite chelating resin is added, stirred for 100 minutes, insoluble matter is removed by filtration, the solvent is removed by reduced pressure distillation, and finally purified by distillation to obtain high-purity diisopropylamine silane.

[0115] The solvent in S1 is n-hexane.

[0116] The stirring rate of S1 is 300 rpm.

[0117] The reaction temperature of S2 is 20°C and the reaction time is 1 hour.

[0118] The pressure of the reduced pressure distillation in S3 is 50 mmHg and the temperature is 60°C.

[0119] The distillation in S3 adopts a high-efficiency fractionating tower with a top pressure of 80 mmHg, a top temperature of 80° C., a bottom temperature of 105° C., and a reflux ratio of 4:1.

[0120] The preparation method of the aminocarboxylic acid-MOF composite chelating resin is as follows:

[0121] H1: Disperse 100 g of chloromethylated resin and 2 g of aminophthalate zirconium MOF (CAS: 1260119-00-3) in 1000 g of dichloroethane and stir to swell for 1 h;

[0122] H2: Add 5 g of disodium iminodiacetate and 3 g of sodium hydroxide to the H1 system, stir and react at 70°C for 5 h, and vacuum dry at 60°C to obtain an aminocarboxylic acid-MOF composite chelating resin.

[0123] Table 1 Test results of the embodiments and comparative examples

[0124] purity / % Yield / % Metal ion purity grade Example 1 99.49 86.8 6N Example 2 99.53 87.3 6N Example 3 99.62 87.8 6N Example 4 99.68 88.2 6N Comparative Example 1 80.64 65.5 3N Comparative Example 2 92.36 78.4 4N Comparative Example 3 94.91 80.7 5N

[0125] Through the data analysis of the above examples and comparative examples, the diisopropylamine silane prepared by the present invention has a purity of more than 99.49%, and the metal ion purity grade reaches 6N level.

[0126] The above description is merely a preferred embodiment of the present invention and does not constitute any form of limitation to the present invention. Although the present invention has been disclosed as above in terms of a preferred embodiment, it is not intended to limit the present invention. Any person skilled in the art can, without departing from the scope of the technical solution of the present invention, make some changes or modifications to equivalent embodiments using the technical contents disclosed above. However, any brief modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention are still within the scope of the technical solution of the present invention.

Claims

1. A method for preparing diisopropylamine silane, wherein the steps are as follows, calculated by weight: S1 Raw material mixing: Under the protection of argon, add 200-400 parts of solvent to the reactor, slowly add 110-135 parts of lithium diisopropylamide solution dropwise, and control the dropwise addition rate to keep the reaction temperature at -5 to 0°C; under continuous stirring, slowly add 45-55 parts of iodosilane dropwise, and maintain the reaction temperature; S2 temperature rise reaction: after the dropwise addition is completed, the reaction system is heated to a high temperature and the reaction is continued with stirring; S3 post-treatment: After the reaction is completed, add 10-20 parts of aminocarboxylic acid-MOF composite chelating resin, stir for 100-180 minutes, filter to remove insoluble matter, remove the solvent by reduced pressure distillation, and finally purify by distillation to obtain high-purity diisopropylamine silane; The aminocarboxylic acid-MOF composite chelating resin is prepared by reacting chloromethylated resin, aminophthalate zirconium MOF, disodium iminodiacetic acid, 2-amino-1,3,5-triazine and sodium hydroxide.

2. The method for preparing diisopropylamine silane according to claim 1, wherein: The solvent in S1 is n-hexane or carbon tetrachloride.

3. The method for preparing diisopropylamine silane according to claim 1, wherein: The stirring rate of S1 is 300-500 rpm.

4. The method for preparing diisopropylamine silane according to claim 1, wherein: The reaction temperature of S2 is 20-40° C. and the reaction time is 1-4 hours.

5. The method for preparing diisopropylamine silane according to claim 1, wherein: The pressure of the reduced pressure distillation in S3 is 50-70 mmHg and the temperature is 60-70°C.

6. The method for preparing diisopropylamine silane according to claim 1, wherein: The distillation in S3 adopts a high-efficiency fractionating tower with a top pressure of 80-100 mmHg, a top temperature of 80-90°C, a bottom temperature of 105-115°C, and a reflux ratio of 4-8:

1.

7. The method for preparing diisopropylamine silane according to claim 1, wherein: The preparation method of the aminocarboxylic acid-MOF composite chelating resin is as follows, calculated by weight: H1: Disperse 100-150 parts of chloromethylated resin and 2-5 parts of zirconium aminophthalate MOF in 1000-1200 parts of dichloroethane and stir to swell for 1-4 hours; H2: Add 5-10 parts of disodium iminodiacetate, 1-3 parts of 2-amino-1,3,5-triazine, and 3-7 parts of sodium hydroxide to the H1 system, stir and react at 70-80°C for 5-8h, and vacuum dry at 60-70°C to obtain an aminocarboxylic acid-MOF composite chelating resin.

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