Methyl diethoxysilane

Many standard proteins lacking sufficient aromatic amino acids and thiols on their surface as e.g. urease need reactive photo cross-linking. For that purpose the protein stock solutions 5% (w/v in distilled water) is mixed with a solution of 3% (w/v) 4,4 -diazidostilbene-2,2 disulfonic acid disodiumsalt tetrahydrate (DIAS) in a ratio of 10 1 (v / v). The mixture is spin-coated onto the mirror and activated with a monolayer l-(3-aminopropyl)-methyl-diethoxysilane. Amino-silane, an efficient adhesion promoter, is applied via vapor silanization as described above. Finally the spin-coated protein film is cross-linking via irradiation with UV-light for 30 seconds (350 nm, 60 W), The application of wavelength less than 350 nm will lead to considerable DIAS decomposition, therefore DNA cross-linker devices as used above are not recommended for this method. 

Mordenite Framework Inverted (MFI) zeolite membranes were synthesized on the inner surface of a-alumina tubes (Pall Corp.) from an aluminum-free precursor solution containing Si02, NaOH, H2O, and template tetrapropylammonium hydroxide (TPAOH) by in situ hydrothermal crystallization at 453 K for 20 h (Tang et al. 2009). The resultant zeolite membrane had a thickness of 2-3 xm. The membrane surface was modified by the in situ catalytic cracking deposition of methyl-diethoxysilane (MDBS) molecules at the sites of [(tSi-0")H ] whereas MDBS vapor was carried by an equimolar H2/CO2 mixture flowing over the membrane surface at a pressure of 1.5 bar and a temperature of 723 K. 

Methyl(phenylaminomethyl)diethoxysilane (AM-2) is prepared by the etherification of methyl(chloromethyl)dichlorosilane with anhydrous ethyl alcohol and subsequent amidation of the etherified product with aniline. 

The etherification stage entails only the substitution of chlorine atoms which are situated directly at the silicon atom, forming methyl(chloromethyl)diethoxysilane (the chlorine in the chloromethyl radical is not affected) ... 

At the stage of methyl(phenylaminomethyl)diethoxysilane amidation with aniline, the chlorine atoms in the chloromethyl radical are replaced with a phenylamine group, which forms... 

The production process of methyl(phenylaminomethyl)diethoxysilane (Fig. 27) comprises two main stages the etherification of... 

Methyl(chloromethyl)diethoxysilane is synthesised in etherificator /, which is an enameled steel apparatus with a removable cover, spherical bottom and jacket for heating (with a heat carrier or vapour). From batch box 2 the etherificator receives a necessary amount of anhydrous ethyl alcohol after that cooler 4 is filled with water. 

Fig. 27. Production diagram of methyl(phenylaminomethyl)diethoxysilane 1 -etherificator 2, 3, 5, 7, 8 - batch boxers 4, 9, 13 - coolers 6 - reactor 10, 16 -nutsch filters 11, 17- collector boxes 12- distillation tank 14, 15 - receptacles 18 - depository...

The obtained methyl(chloromethyl)diethoxysilane is sent by nitrogen flow into batch box 5, from where it is sent for amidation into reactor 6, which is an enameled cylindrical apparatus with a jacket and an agitator. First, the reactor is loaded with a necessary amount of methyl(chloromethyl)diethoxysilane from batch box 5 then cooler 9 is filled with water, the agitator is switched on and anilinee is introduced from batch box 8. 

We should note that the reactor receives an excess of aniline, so that the amidation of methyl(chloromethyl)diethoxysilane is accompanied by the binding of released hydrogen chloride. When introducing aniline, one should keep a close watch on the temperature in the reactor, since the process takes place with the liberation of heat. After aniline has been introduced, the reactive mixture is heated to 135-140 °C within 2-3 hours and agitated at this temperature for 8-8.5 hours. After that reactor 6 is... 

Then, the solution of methyl(phenylaminomethyl)diethoxysilane in the mixture of toluene and aniline is sent by nitrogen flow into distillation tank 12. There a residual pressure of 25-35 GPa is created, cooler 13 is filled with water, the agitator is switched on and the tank is slowly heated. The distilled toluene enters receptacle 14 through run-down box 4 the distillation continues up to 100°C. The toluene in the receptacle is sampled to determine the density (at the density of 0.854-0.870 g/cm3 the distillation is considered complete). The distilled toluene from receptacle 14 is sent in vacuum into batch box 7 and used for another process of amidation. 

After the distillation of toluene begins the distillation of aniline. The distillation of aniline is conducted up to 160-165°C in the tank (under a residual pressure of 30 GPa) and collected in receptacle 15. From there aniline is sent in vacuum into batch box 8 and used for another process of amidation. The target product which remains in tank 12, methyl(phenylaminomethyl)diethoxysilane, is cooled down to 30-50 °C, filtered in nutsch filter 16 and collected in box 17. After 2-3 days of standing, methyl(phenylaminomethyl)diethoxysilane is sent from box 17 into depository 18. 

Methyl(phenylaminomethyl)diethoxysilane is a trasparent liquid ranging in colour from light yellow to light brown (the boiling point is 152-153 °C at 20 GPa). It can be easily dissolved in organic solvents is hydrolysed in the presence of water. 

Technical methyl(phenylaminomethyl)diethoxysilane should meet the following requirements ... 

Methyl(phenylaminomethyl)diethoxysilane is used as a modifying agent for some polymethylphenylsiloxane varnishes and polyolefines, as well as to obtain binding agents for fiberglass plastics. 

Similarly to methyl(phenylaminomethyl)diethoxysilane and diethylami-nomethyltriethoxysilane, one can also obtain other substituted ethers of orthosilicon acid with an aminogroup in the organic radical, e.g. a-aminomethyltrialkoxysilanes, as well as 1-aminohexamethylene-6-aminomethyltriethoxysilane. 

The etherification of chloromethyltrichlorosilane with anhydrous ethyl alcohol is carried out in an etherificator by the technique described for obtaining methyl(phenylaminomethyl)diethoxysilane and according to the diagram described in Fig. 27. 

Structure II polymers are relatively elastic when polymethylphenylsiloxanes are obtained by the hydrolytic cocondensation only of trifunctional monomers (e.g., methyl- and phenyltrichlorosilanes), there are polymers with low elasticity. Polydimethyl- and polymethylphenylsiloxanes can be modified with organic polymers (polyester, epoxy) or silicone substances, e.g. methyl(phenylaminomethyl)diethoxysilane. The modification of polydimethyl- and polymethylphenylsiloxanes improves some properties of these polymers and varnishes based on them in particular, it considerably increases adhesion and mechanical durability of varnish films. 

The R1 values obtained for such phenylethynyl substituted siloxanes are higher then that reported for traditional aromatic-based systems [9] or the phenol modified ones (1.50-1.53) [10]. The synthesis of high refractive index (methyl)(diphenyle thenyl)-dichlorosilane via hydrosilylation was also described [1]. Such monomer was later hydrolyzed and condensed into silicone fluid. Similar process was also presented, applying silylative coupling process in the synthesis of an analogous (methyl)(phenylethenyl)diethoxysilane [11], so the two reactions shall be discussed in the following section. 

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