Perfluoropolyether silane compound and preparation method thereof

By using metal catalysts and ligands to perform hydrosilication reaction in perfluoropolyether silane synthesis, the problem of narrow application scope and uncontrollable selectivity in the prior art is solved, and the full application and selectivity controllability are achieved. The synthesis of fluoropolyether silanes obtains branched products, expanding the application range of materials.

CN119119104AInactive Publication Date: 2024-12-13CHINA UNIV OF MINING & TECH
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Patent Information

Application Number
CN202411241557.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-05
Publication Date
2024-12-13
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

The existing perfluoropolyether silane synthesis method has a narrow scope of application, and branched perfluoropolyether silane products cannot be obtained, and the selectivity is uncontrollable.

Method used

The hydrogenation reaction of metal catalysts and ligands is carried out under specific temperatures and conditions. By regulating the reaction conditions and catalyst selection, the synthesis of selectively controllable perfluoropolyether silane is achieved.

Benefits of technology

The synthesis of perfluoropolyether silanes with wide applicability and selectivity controllability can be achieved, and perfluoropolyether silanes with different polymerization degrees and structures can be obtained, including branched products, and the scope of application of the material is expanded.

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Abstract

The invention discloses a perfluoropolyether silane compound and a preparation method thereof. The perfluoropolyether silane compound is selected from any one of compounds with a structural formula as shown in a formula 5 '. According to the invention, commercially available perfluoropolyether alcohol and organosilane are used as raw materials, and the perfluoropolyether silane is synthesized through a two-step reaction. The method has the advantages of simple step operation, controllable selectivity and wide application range. # imgabs0 #
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Description

Technical Field

[0001] The invention relates to the technical field of fluorine chemical industry, and in particular to a perfluoropolyether silane compound and a preparation method thereof. Background Art

[0002] Perfluoropolyether silanes contain perfluoropolyether segments and silane functional groups. Perfluoropolyether segments are generally composed of multiple repeated fluorinated ether units, such as -CF2O-, -CF2CF2O-, etc., which make the molecule have excellent chemical inertness, thermal stability and low surface energy. Common structures of silane functional groups such as -Si(OR)3 (where R is usually methyl, ethyl, etc.) can undergo condensation reactions with hydroxyl groups on the surface of the substrate, thereby achieving good adhesion and modification.

[0003] Perfluoropolyether silanes can easily achieve a better balance of performance by adjusting the combination of appropriate perfluoropolyether segments and silane functional groups, such as improving adhesion to the substrate, weather resistance and chemical corrosion resistance while maintaining good hydrophobic and oleophobic properties. Therefore, perfluoropolyether silane materials have a wide range of uses in various fields of daily production and life. For example, in surface treatment, it can give materials excellent waterproof, oil-proof and anti-fouling properties, and is often used in the treatment of textiles, leather and paper to improve their stain resistance and easy-to-clean properties. In the electronics field, it can be used to improve the moisture and corrosion resistance of electronic components and enhance their reliability and service life. In the optical field, it helps to improve the surface properties of optical lenses and displays, reduce reflections, improve clarity and wear resistance. In industrial lubrication, it can be used as a high-performance lubricant and play an excellent lubricating role under high temperature, high pressure and harsh environments. In paints and coatings, it can enhance the adhesion, weather resistance and chemical corrosion resistance of coatings.

[0004] Existing methods for synthesizing perfluoropolyether silane materials are all based on a hydrosilylation reaction of perfluoropolyether and silane, which has a narrow scope of application and mostly produces linear perfluoropolyether silanes, and cannot produce branched perfluoropolyether silane products. Therefore, it is of great significance to develop a universal and selectively controllable method for synthesizing perfluoropolyether silanes. Summary of the invention

[0005] One of the objects of the present invention is to provide a perfluoropolyether silane.

[0006] The second object of the present invention is to provide a method for preparing the above-mentioned perfluoropolyether silane, which has simple steps and operation, controllable selectivity and a wide range of applications.

[0007] To achieve the above purpose, the technical solution adopted by the present invention is as follows:

[0008] In a first aspect, the present invention provides a perfluoropolyether silane compound, wherein the perfluoropolyether silane is selected from any one of the compounds having the structural formula shown in Formula 5':

[0009]

[0010] In formula 5', R 1 , R 2 , R 3 independently selected from hydrogen, C1-C 10 Alkyl, C1-C 10 Alkoxy, C6-C 10 Aryl, substituted C1-C 10 Alkyl I, substituted C6-C 10 Any one of the aryl I and the substituents shown in formula II;

[0011]

[0012] In Formula II, y is an integer selected from 0 to 100;

[0013] R 4 Selected from hydrogen, C1-C 10 Alkyl, substituted C1-C 10 Any one of the alkyl groups II;

[0014] R 5 , R 6 Independently selected from C1-C 10 The alkyl group;

[0015] R f A substituent selected from the group consisting of those shown in formula III;

[0016]

[0017] In formula III, t is selected from an integer from 0 to 20, and n is selected from an integer from 1 to 4;

[0018] When t is 0, m is selected from an integer from 1 to 4, and q is selected from an integer from 0 to 4;

[0019] When t is selected from an integer from 1 to 20, m and q are independently selected from an integer from 1 to 4;

[0020] Z is selected from an integer ranging from 0 to 100.

[0021] Preferably, the substituted C1-C 10 The substituents in the alkyl group I are selected from C6-C 10 Aryl, substituted C6-C 10 Any one of the aryl groups I;

[0022] The substituted C6-C 10The substituent in the aryl group I is any one of C1-C8 alkyl, fluorine, chlorine, bromine, trifluoromethyl, nitro, C1-C8 alkoxy, phenoxy, methyl ester, ethyl ester, tert-butyl ester and n-butyl ester.

[0023] Preferably, the substituted C1-C 10 The substituents in the alkyl group II are selected from the substituents shown in formula IV;

[0024]

[0025] In Formula IV, R 7 , R 8 , R 9 Independently selected from C1-C 10 Alkyl, C6-C 10 Aryl, substituted C1-C 10 Any one of the alkyl groups III.

[0026] Preferably, the substituted C1-C 10 The substituent in the alkyl group III is selected from C6-C 10 The aromatic group.

[0027] In a second aspect, the present invention provides a method for preparing the above-mentioned perfluoropolyether silane compound, the method at least comprising:

[0028] The material I containing the compound 3 and the compound 4 is subjected to a hydrosilation reaction at 25 to 160° C. for 0.5 to 36 hours in the presence of a metal catalyst and a ligand to obtain the compound 5′;

[0029] The compound 3 is selected from any one of the compounds having the structural formula shown in Formula 3:

[0030]

[0031] The compound 4 is selected from any one of the compounds having the structural formula shown in Formula 4:

[0032]

[0033] The molar ratio of the ligand to the compound 3 is 0.005% to 20%; the molar ratio of the compound 3 to the compound 4 is 0.8 to 10; and the molar ratio of the metal catalyst to the compound 3 is 0.005% to 20%.

[0034] Optionally, the metal catalyst is selected from transition metal catalysts;

[0035] The transition metal catalyst is selected from at least one of FeCl2, FeCl3, FeBr2, FeBr3, FeI2, Fe(OAc)2, Fe(acac)2, CoCl2, CoBr2, CoI2, Co(acac)3, Co2(CO)8, CoCl(PPh3)3, RhCl3, RhCl(PPh)3, [Rh(cod)Cl]2, Rh(cod)2BF4, [Rh(cod)(OMe)]2, [Rh(C2H4)2Cl]2, RhCl(PPh3)3, Rh(acac)(CO)2, Rh(acac)(C2H4)2, PtCl2, H2PtCl6, Castel catalyst, and PtCl2(NH3)2.

[0036] The ligand is selected from tricyclohexylphosphine (PCy3), tri-tert-butylphosphine (P t Bu3), 2-dicyclohexylphosphino-2',4',6'-triisopropylbiphenyl (Xphos), bis(diphenylphosphino)ethane (dppe), bis(diphenylphosphino)propane (dppp), bis(diphenylphosphino)butane (dppb), 1,2-bis(dicyclohexylphosphino)ethane (dcype), 1,1'-bis(diphenylphosphino)ferrocene (dppf), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (Xantphos), 1,2-bis(diphenylphosphino)benzene (dppBz), bis(2-diphenylphosphinophenyl)ether (DPEphos), 2,2'- At least one of bis(diphenylphosphine)-1,1'-binaphthyl (BINAP), 5,5'-bis(diphenylphosphine)-4,4'-di-1,3-benzodioxole (Segphos), 5,5'-bis[di(3,5-di-tert-butyl-4-methoxyphenyl)phosphine]-4,4'-di-1,3-benzodioxole (DTBM-Segphos), 2,2'-bis(diphenylphosphine)-6,6'-dimethoxy-1,1'-biphenyl (OMe-BIPHEP), o-phenanthroline (phen), bipyridine, pyridine imine, pyridone imine, pyridine diimine, and bisoxazoline.

[0037] Optionally, the material I further includes an organic solvent, which is selected from at least one of ether, tetrahydrofuran (THF), 2-methyltetrahydrofuran (2-MeTHF), N,N-dimethylformamide (DMF), N,N-dimethylacetamide, dichloromethane (DCM), dichloroethane, acetonitrile, cyclohexane, toluene, xylene, and chlorobenzene; the concentration of the compound 3 in the material I is 0.10 to 5.0 mol / L.

[0038] Optionally, the material I further includes an additive; the additive is selected from at least one of sodium triethylborohydride, lithium triethylborohydride, potassium triethylborohydride, diethylzinc, diphenylzinc, trimethylaluminum, aluminum trichloride, triethylboron, triphenylboron, methylmagnesium chloride, ethylmagnesium chloride, isopropylmagnesium chloride, and trimethylsilylmethylmagnesium chloride; the molar ratio of the additive to compound 3 is 0.01 to 2.0.

[0039] Optionally, the obtaining of the compound 3 comprises at least the following steps:

[0040] Allylating material II containing compound 1 and compound 2 in the presence of a promoter at 25 to 120° C. for 1 to 36 hours to obtain compound 3; the molar ratio of compound 1 to compound 2 is 0.8 to 10;

[0041] The compound 1 is selected from any one of the compounds having the structural formula shown in Formula 1:

[0042]

[0043] The compound 2 is selected from any one of the compounds having the structural formula shown in Formula 2:

[0044]

[0045] In formula 2, X is selected from halogen, hydroxyl, C1-C 10 Any one of the alkoxy groups and the substituents represented by formula V;

[0046]

[0047] In Formula V, R 10 Selected from C1-C 10 Alkyl, C1-C 10 Any of the alkoxy groups.

[0048] Optionally, in the material II, the concentration of the compound 1 in the material II is 0.10 to 5.0 mol / L.

[0049] Optionally, the promoter is selected from acid compounds; in Formula 2, X is selected from hydroxyl, C1-C 10 Any one of the alkoxy groups and the substituents represented by formula V;

[0050] The acid compound is selected from at least one of camphorsulfonic acid, p-toluenesulfonic acid, benzenesulfonic acid, trifluoroacetic acid, trifluoromethanesulfonic acid, diphenyl phosphate, dibenzyl phosphate, triethylboron, diethylzinc, trimethylaluminum, dimethylaluminum chloride, aluminum chloride, ferric chloride, indium chloride, tri(pentafluorophenyl)boron, boron trifluoride etherate, aluminum trifluoromethanesulfonate (Al(OTf)3), copper trifluoromethanesulfonate, scandium trifluoromethanesulfonate, zinc trifluoromethanesulfonate, iron trifluoromethanesulfonate (Fe(OTf)3), ytterbium trifluoromethanesulfonate, lanthanum trifluoromethanesulfonate (La(OTf)3), and indium trifluoromethanesulfonate (In(OTf)3);

[0051] The molar ratio of the acid compound to compound 1 is 0.02-2.

[0052] Optionally, the promoter is selected from alkaline compounds; in Formula 2, X is selected from halogens;

[0053] The alkaline compound is selected from at least one of sodium hydroxide, potassium hydroxide, sodium hydride, calcium hydride, calcium oxide, magnesium aluminum hydrotalcite, triethylamine, 1,8-diazabicycloundec-7-ene (DBU), and 1,4-diazabicyclo[2.2.2]octane (DABCO);

[0054] The molar ratio of the base compound to compound 1 is 0.05-10.

[0055] Specifically, the present application provides a method for preparing a synthetic compound 5'.

[0056] (1) using perfluoropolyether alcohol 1 and allyl reagent 2 as raw materials, carrying out an allylation reaction at 25 to 60°C for 12 to 24 hours in the presence of an acid or a base to obtain the compound 3;

[0057] (2) Compound 3 and organosilane 4 are used as raw materials, and a hydrosilylation reaction is carried out at 60-100° C. for 24-36 hours in the presence of a metal catalyst, a ligand and an additive NaBEt3H to obtain the compound 5′.

[0058]

[0059] Compared with the prior art, the present invention has the following beneficial effects:

[0060] 1. The preparation method of the compound provided by the present invention has wide universality, and perfluoropolyether alcohols with different polymerization degrees and various organosilanes can react to prepare perfluoropolyether silanes, and the selectivity of hydrosilylation can be changed by regulating metal catalysts and ligands. Therefore, the present invention has potential application prospects in the rapid and selective synthesis of perfluoropolyether silanes.

[0061] 2. The present invention can obtain branched perfluoropolyether silane products, which have a wide range of applications. DETAILED DESCRIPTION

[0062] The present invention is further described in detail below with reference to specific embodiments.

[0063] Unless otherwise specified, the raw materials and catalysts in the examples of this application were purchased through commercial channels.

[0064] The analysis method in the examples of the present application is as follows: NMR was detected on a Bruker AVANCE III 400 MHz.

[0065] Example 1-31

[0066] 1. Base-promoted allylation reaction of polyether alcohol

[0067] In a 50 mL Schlenk reaction bottle, perfluoropolyether alcohol 1a (10.0 mmol) was dissolved in 30 mL solvent, and then a base (12.0 mmol) or an acid catalyst (1.0 mmol) was added. The mixture was stirred for 30 min at room temperature, and then allyl precursor 2 (12.0 mmol) was slowly added dropwise. The reaction was continued for 12 h. After the reaction, mesitylene trimethoxybenzene was added as an internal standard, and the product yield was detected by H NMR spectrum.

[0068]

[0069] Table 1. Effects of allyl precursors, bases, and solvents on the reaction

[0070]

[0071]

[0072] From the results in Table 1, it can be seen that when the allyl precursor X is a halogen, NaH is the best base, and the reaction effects are comparable in 2-methyltetrahydrofuran, tetrahydrofuran and N,N-dimethylformamide solvents (No. 1, 4, 6). However, since 2-methyltetrahydrofuran can be obtained from biomass, green 2-methyltetrahydrofuran is selected as the best solvent. Allyl bromide is used as the raw material, and the yield of the target product is the highest (No. 7).

[0073] When allyl alcohol is used as a precursor, an acid catalyst can promote the reaction. La(OTf)3 is the best catalyst, and the yield is high in DCE solvent (No. 13). Through temperature screening, 60°C was found to be the best temperature, with a yield of 72% (No. 19). Other allyl precursors can also participate in the reaction, for example, allyl acetate can achieve comparable reaction results (No. 20).

[0074] 2. Hydrosilylation of polyallyl ether

[0075] In a 10mL Schlenk reaction bottle, polyallyl ether 3a (2.0mmol) was dissolved in 2mL solvent, and metal catalyst (0.2mmol), ligand (0.2mmol), additive (0.2mmol), and silane 4a (2.2mmol) were added in sequence. The mixture was stirred for 24h at a certain temperature. After stirring, trimethoxybenzene was added as an internal standard, and the product yield was detected by H NMR spectrum.

[0076]

[0077] Table 2. Effect of catalytic system on the selectivity of hydrosilylation reaction

[0078]

[0079]

[0080] As can be seen from Table 2, for the iron catalytic system, the commonly used diphosphine ligands and o-phenanthroline (Examples 1-5) can promote the reaction, but the selectivity is low; when the bidentate pyridone imine L4 is the ligand, the branched chain hydrosilylation is the main product (Example 9); when the tridentate pyridone diimine L8 is the ligand, the selectivity becomes a linear hydrosilylation product (Example 13). When FeI2 is the catalyst precursor, the selectivity and yield of the product decrease (Example 15). Temperature and solvent screening found that 100oC is the optimal temperature and THF is the best solvent (Example 17).

[0081] For the cobalt catalytic system, by optimizing the common phosphine ligand, it was found that when DPEphos was the ligand, the reaction effect was the best (Examples 20-24); the additive was TMSCH2MgCl, the yield and selectivity could be improved, and 80oC was the optimal temperature (Example 27). Precious metal rhodium and platinum catalysts can also promote the reaction, with linear hydrosilylation as the main path, among which the Custer catalyst had the highest activity (Example 31).

[0082] H NMR data:

[0083] Compound 5a: 1 H NMR (400MHz, Chloroform-d) δ3.56–3.45(m,4H),1.54–1.38(m,2H),0.38–0.26(m,2H),0.07(s,18H),0.06(s,3H).

[0084] Compound 5a': 1H NMR (400MHz, Chloroform-d) δ3.51–3.42(m,4H),1.53–1.36(m,3H),0.84(d,J=7.3Hz,3H),0.08(s,18H),0.07(s,3H).

[0085] Embodiment 32

[0086] In a 10 mL Schlenk reaction bottle, polyallyl ether 3a (2.0 mmol) was dissolved in 2 mL tetrahydrofuran (THF), and FeCl2 (0.2 mmol), ligand L4 (0.2 mmol), NaBEt3H (0.2 mmol), and triphenylsilane 4b (2.2 mmol) were added in sequence. The mixture was stirred at 80 °C for 24 h. Afterwards, trimethoxybenzene was added as an internal standard, and the yields of products 5b and 5b' were detected by H NMR.

[0087]

[0088] Compound 5b: 1 H NMR(400MHz,Chloroform-d)δ7.14–7.46(m,15H),3.67–3.35(m,4H),1.45–1.40(m,4H).

[0089] Compound 5b': 1 H NMR (400MHz, Chloroform-d) δ7.09–7.40 (m, 15H), 3.50–3.37 (m, 4H), 1.45–1.30 (m, 1H), 0.88 (d, J = 7.1Hz, 3H).

[0090] Embodiment 33

[0091] In a 10 mL Schlenk reaction bottle, polyallyl ether 3a (2.0 mmol) was dissolved in 2 mL tetrahydrofuran (THF), and FeCl2 (0.2 mmol), ligand L4 (0.2 mmol), NaBEt3H (0.2 mmol), and trimethylsilane 4c (2.2 mmol) were added in sequence. The mixture was stirred at 80 °C for 24 h. Afterwards, mesitylene trimethoxybenzene was added as an internal standard, and the yields of products 5c and 5c' were detected by H NMR.

[0092]

[0093] Compound 5c: 1H NMR (400MHz, Chloroform-d) δ3.67–3.35(m,4H),1.43–1.42(m,2H),0.70–0.68(m,2H),0.05(s,9H).

[0094] Compound 5c': 1 H NMR (400MHz, Chloroform-d) δ3.53–3.29 (m, 4H), 1.39–1.28 (m, 1H), 0.81 (d, J = 6.9Hz, 3H), 0.06 (s, 9H).

[0095] The compound 5' and any one of the compounds 5' prepared according to the method are both oil-soluble and water-soluble and easy to adjust. It has various excellent properties of traditional siloxanes, such as high and low temperature resistance, electrical insulation, low surface tension, etc., and also has special properties such as lubrication, softening effect, good spreadability and emulsification stability provided by polyether, and is used in the fields of electronics and electrical, textiles, light industry, construction, cosmetics, medical and food.

[0096] The above description is only a specific implementation mode of the present invention, but the protection scope of the present invention is not limited thereto. Any modifications, equivalent substitutions and improvements made by any technician familiar with the technical field within the technical scope disclosed by the present invention and within the spirit and principle of the present invention should be covered by the protection scope of the present invention.

Claims

1. A perfluoropolyether silane compound, characterized in that The perfluoropolyether silane is selected from any one of the compounds having the structural formula shown in Formula 5': In formula 5', R 1 , R 2 , R 3 independently selected from hydrogen, C1-C 10 Alkyl, C1-C 10 Alkoxy, C6-C 10 Aryl, substituted C1-C 10 Alkyl I, substituted C6-C 10 Any one of the aryl I and the substituents shown in formula II; In Formula II, y is an integer selected from 0 to 100; R 4 Selected from hydrogen, C1-C 10 Alkyl, substituted C1-C 10 Any one of the alkyl groups II; R 5 , R 6 Independently selected from C1-C 10 The alkyl group; R f A substituent selected from the group consisting of those shown in formula III; In formula III, t is selected from an integer from 0 to 20, and n is selected from an integer from 1 to 4; When t is 0, m is selected from an integer from 1 to 4, and q is selected from an integer from 0 to 4; When t is selected from an integer from 1 to 20, m and q are independently selected from an integer from 1 to 4; Z is selected from an integer ranging from 0 to 100.

2. A perfluoropolyether silane compound according to claim 1, characterized in that: The substituted C1-C 10 The substituents in the alkyl group I are selected from C6-C 10 Aryl, substituted C6-C 10 Any one of the aryl groups I; The substituted C6-C 10 The substituent in the aryl group I is any one of C1-C8 alkyl, fluorine, chlorine, bromine, trifluoromethyl, nitro, C1-C8 alkoxy, phenoxy, methyl ester, ethyl ester, tert-butyl ester and n-butyl ester.

3. A perfluoropolyether silane compound according to claim 1, characterized in that: The substituted C1-C 10 The substituents in the alkyl group II are selected from the substituents shown in formula IV; In Formula IV, R 7 , R 8 , R 9 Independently selected from C1-C 10 Alkyl, C6-C 10 Aryl, substituted C1-C 10 Any of the alkyl groups III; The substituted C1-C 10 The substituent in the alkyl group III is selected from C6-C 10 The aromatic group.

4. A method for preparing the perfluoropolyether silane compound according to any one of claims 1 to 3, characterized in that: The method at least comprises: The material I containing the compound 3 and the compound 4 is subjected to a hydrosilation reaction at 25 to 160° C. for 0.5 to 36 hours in the presence of a metal catalyst and a ligand to obtain the compound 5′; The compound 3 is selected from any one of the compounds having the structural formula shown in Formula 3: The compound 4 is selected from any one of the compounds having the structural formula shown in Formula 4: The molar ratio of the ligand to compound 3 is 0.005% to 20%; the molar ratio of compound 3 to compound 4 is 0.8 to 10; the molar ratio of the metal catalyst to compound 3 is 0.005% to 20%; The metal catalyst is selected from a transition metal catalyst; the transition metal catalyst is selected from at least one of FeCl2, FeCl3, FeBr2, FeBr3, FeI2, Fe(OAc)2, Fe(acac)2, CoCl2, CoBr2, CoI2, Co(acac)3, Co2(CO)8, CoCl(PPh3)3, RhCl3, RhCl(PPh)3, [Rh(cod)Cl]2, Rh(cod)2BF4, [Rh(cod)(OMe)]2, [Rh(C2H4)2Cl]2, RhCl(PPh3)3, Rh(acac)(CO)2, Rh(acac)(C2H4)2, PtCl2, H2PtCl6, Custer catalyst, and PtCl2(NH3)2; The ligand is selected from tricyclohexylphosphine, tri-tert-butylphosphine, 2-dicyclohexylphosphine-2',4',6'-triisopropylbiphenyl, bis(diphenylphosphine)ethane, bis(diphenylphosphine)propane, bis(diphenylphosphine)butane, 1,2-bis(dicyclohexylphosphine)ethane, 1,1'-bis(diphenylphosphine)ferrocene, 4,5-bis(diphenylphosphine)-9,9-dimethylxanthene, 1,2-bis(diphenylphosphine)benzene, bis(2-diphenylphosphinephenyl)ether, 2,2'-bis( At least one of diphenylphosphine)-1,1'-binaphthyl, 5,5'-bis(diphenylphosphine)-4,4'-di-1,3-benzodioxole, 5,5'-bis[di(3,5-di-tert-butyl-4-methoxyphenyl)phosphine]-4,4'-di-1,3-benzodioxole, 2,2'-bis(diphenylphosphine)-6,6'-dimethoxy-1,1'-biphenyl, o-phenanthroline, bipyridine, pyridinealdehyde imine, pyridone imine, pyridine diimine, and bisoxazoline.

5. The method for preparing a perfluoropolyether silane compound according to claim 4, characterized in that: The material I also includes an organic solvent, which is selected from at least one of ether, tetrahydrofuran, 2-methyltetrahydrofuran, N,N-dimethylformamide, N,N-dimethylacetamide, dichloromethane, dichloroethane, acetonitrile, cyclohexane, toluene, xylene, and chlorobenzene; the concentration of the compound 3 in the material I is 0.10-5.0 mol / L.

6. The method for preparing a perfluoropolyether silane compound according to claim 5, characterized in that: The material I also includes an additive; the additive is selected from at least one of sodium triethylborohydride, lithium triethylborohydride, potassium triethylborohydride, diethylzinc, diphenylzinc, trimethylaluminum, aluminum trichloride, triethylboron, triphenylboron, methylmagnesium chloride, ethylmagnesium chloride, isopropylmagnesium chloride, and trimethylsilylmethylmagnesium chloride; the molar ratio of the additive to compound 3 is 0.01 to 2.

0.

7. The method for preparing a perfluoropolyether silane compound according to claim 4, characterized in that: The obtaining of the compound 3 comprises at least the following steps: Allylating material II containing compound 1 and compound 2 in the presence of a promoter at 25 to 120° C. for 1 to 36 hours to obtain compound 3; the molar ratio of compound 1 to compound 2 is 0.8 to 10; The compound 1 is selected from any one of the compounds having the structural formula shown in Formula 1: The compound 2 is selected from any one of the compounds having the structural formula shown in Formula 2: In formula 2, X is selected from halogen, hydroxyl, C1-C 10 Any one of the alkoxy groups and the substituents represented by formula V; In Formula V, R 10 Selected from C1-C 10 Alkyl, C1-C 10 Any of the alkoxy groups.

8. The method for preparing a perfluoropolyether silane compound according to claim 7, characterized in that: In the material II, the concentration of the compound 1 in the material II is 0.10 to 5.0 mol / L.

9. The method for preparing a perfluoropolyether silane compound according to claim 8, characterized in that: The promoter is selected from acid compounds; in Formula 2, X is selected from hydroxyl, C1-C 10 Any one of the alkoxy groups and the substituents represented by formula V; The acid compound is selected from at least one of camphorsulfonic acid, p-toluenesulfonic acid, benzenesulfonic acid, trifluoroacetic acid, trifluoromethanesulfonic acid, diphenyl phosphate, dibenzyl phosphate, triethylboron, diethylzinc, trimethylaluminum, dimethylaluminum chloride, aluminum chloride, ferric chloride, indium chloride, tri(pentafluorophenyl)boron, boron trifluoride ethyl ether, aluminum trifluoromethanesulfonate, copper trifluoromethanesulfonate, scandium trifluoromethanesulfonate, zinc trifluoromethanesulfonate, iron trifluoromethanesulfonate, ytterbium trifluoromethanesulfonate, lanthanum trifluoromethanesulfonate, and indium trifluoromethanesulfonate; The molar ratio of the acid compound to compound 1 is 0.02-2.

10. The method for preparing a perfluoropolyether silane compound according to claim 8, characterized in that: The promoter is selected from alkaline compounds; in Formula 2, X is selected from halogens; The alkaline compound is selected from at least one of sodium hydroxide, potassium hydroxide, sodium hydride, calcium hydride, calcium oxide, magnesium aluminum hydrotalcite, triethylamine, 1,8-diazabicycloundec-7-ene, and 1,4-diazabicyclo[2.2.2]octane; The molar ratio of the base compound to compound 1 is 0.05-10.

11. The method for preparing a perfluoropolyether silane compound according to claim 4, characterized in that: (1) using perfluoropolyether alcohol 1 and allyl reagent 2 as raw materials, carrying out an allylation reaction at 25 to 60°C for 12 to 24 hours in the presence of an acid or a base to obtain the compound 3; (2) Compound 3 and organosilane 4 are used as raw materials, and a hydrosilylation reaction is carried out at 60-100° C. for 24-36 hours in the presence of a metal catalyst, a ligand and an additive NaBEt3H to obtain the compound 5′.

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