- PREPARATION OF ISOCYANATOSILANES
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There is provided herein a method and an apparatus for producing an isocyanatoorganosilane which method includes feeding a carbamatoorganosilane to a cracking device where it is thermally dissociated into a reaction product mixture comprising isocyanatoorganosilane, alcohol, and heavies, followed by separating the mixture in a distillation column of two parts and collecting the isocyanatoorganosilane from the distillation column via a side stream having a predetermined location between the top and bottom parts of the column; and wherein the distillation column is configured to have a ratio of the length of the bottom part of the distillation column to the length of the top part of the distillation column which is effective to provide a side stream having a high purity and high weight percent of isocyanatoorganosilane.
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Paragraph 0051-0052
(2020/02/06)
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- The isocyanate group-containing alkoxysilane method (by machine translation)
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[Problem] an isocyanate group-containing alkoxysilane isocyanate group-containing alkoxysilane having high purity can be efficiently produced. [Solution] The amino group-containing alkoxysilane is reacted with dialkyl carbonate, carbamate alcohol mixture is obtained. Then, the mixture was heated to obtain an isocyanate group-containing alkoxysilanes. In this case, alcohol-containing fractions of 1 second, isocyanate group-containing alkoxysilane containing 2 fractions of a second, annular byproducts including 3 a fraction is obtained. The, the first fraction of the heated mixture before mixing 3, annular reaction byproduct alcohol, cyclic carbamate returned products. Figure 1 [drawing] (by machine translation)
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Paragraph 0102; 0107-0112
(2020/10/03)
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- Method for preparing 3-isocyanatopropyltrimethoxysilane
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The invention relates to a method for preparing 3-isocyanatopropyltrimethoxysilane. The method is characterized in that [3-(trimethoxysilane)propyl]methyl carbamate is used as a raw material to reactwith methyl trichlorosilane, and thus 3-isocyanatopropyltrimethoxysilane is synthesized by one step. The preparation method provided by the invention is simple, the production process is safe, the reaction temperature is easy to control, production equipment is simple, and thus the method is suitable for industrial production.
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Paragraph 0032-0039
(2019/02/06)
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- PROCESS FOR PREPARING ISOCYANATES CONTAINING ALKOXYSILANE GROUPS
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The invention relates to a process for preparing isocyanate containing alkoxysilane groups, in which, in the sequence of steps A) to D), A) alkoxysilano(cyclo)alkylamine is reacted with dialkyl carbonate in the presence of a basic catalyst to give alkoxysilano(cyclo)alkylurethane,B) simultaneously or successively, the catalyst is deactivated, and low boilers, solids, salt burdens and/or high boilers are removed,C) alkoxysilano(cyclo)alkylurethane obtained after B) is thermally cleaved to release isocyanate containing alkoxysilane groups and by-product, leaving bottoms material, andD) isocyanate containing alkoxysilane groups and by-product are separated from one another and from bottoms material and collected, pa wherein the process regime at least of steps C) to D) is continuous.
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Paragraph 0087; 0088; 0089; 0090; 0091; 0092; 0093
(2019/10/17)
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- PROCESS FOR PREPARING ISOCYANATES CONTAINING ALKOXYSILANE GROUPS
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The invention relates to a process for preparing isocyanate containing alkoxysilane groups, in which, in the sequence of steps A) to D), A) haloalkylalkoxysilane is reacted with metal cyanate and alcohol to give alkoxysilanoalkylurethane, B) alkoxysilanoalkylurethane is freed of low boilers, solids, salt burdens and/or high boilers and optionally purified, C) alkoxysilanoalkylurethane obtained after B) is thermally cleaved to release isocyanate containing alkoxysilane groups and by-product, leaving bottoms material, and D) isocyanate containing alkoxysilane groups and by-product are separated from one another and from cleavage bottoms material and collected, wherein the process regime at least of steps C) to D) is continuous.
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Paragraph 0068-0071
(2019/10/17)
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- PROCESS FOR PREPARING ISOCYANATES CONTAINING ALKOXYSILANE GROUPS
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The invention relates to a process for preparing isocyanate containing alkoxysilane groups, in which, in the sequence of steps A) to D), A) alkoxysilano(cyclo)alkylamine is reacted with dialkyl carbonate in the presence of a basic catalyst to give alkoxysilano(cyclo)alkylurethane,B) simultaneously or successively, the catalyst is removed and/or deactivated, and low boilers, solids, salt burdens and/or high boilers are removed,C) alkoxysilano(cyclo)alkylurethane obtained after B) is thermally cleaved to release isocyanate containing alkoxysilane groups and by-product, leaving bottoms material, andD) isocyanate containing alkoxysilane groups and by-product are separated from one another and from bottoms material and collected, wherein the basic catalyst is a guanidine base.
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Paragraph 0099-0103
(2019/10/23)
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- PROCESS FOR PREPARING ISOCYANATES CONTAINING ALKOXYSILANE GROUPS
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The present invention relates to a process for preparing isocyanate containing alkoxysilane groups, in which, in the sequence of steps A) to D), A) alkoxysilanoalkylamine is reacted with urea in the presence of an alcohol, optionally in the presence of at least one catalyst, to give alkoxysilanoalkylurethane, B) simultaneously or successively, if used, the catalyst is removed and/or deactivated, and low boilers, medium boilers and/or high boilers are removed, C) purified alkoxysilanoalkylurethane is thermally cleaved to release isocyanate containing alkoxysilane groups and by-product, leaving bottoms material, and D) isocyanate containing alkoxysilane groups and by-product are separated from one another and from bottoms material and collected, in which, in step C), i) the bottoms material is wholly or partly discharged from the cleavage apparatus,ii) subjected to thermal treatment and/or purification and/or an aftertreatment in the presence of alcohol andiii) the material removed, after thermal treatment and/or purification and/or aftertreatment in step B) or C), is fed in again.
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Paragraph 0086-0088
(2019/10/23)
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- Method for preparing isocyanate-based silane by hydrosilylation reaction
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The invention relates to a synthetic method of an isocyanate-based silane coupling agent and belongs to the field of synthesis of silane coupling agents. The preparation method comprises the followingsteps: taking allyl urea and sodium nitrite as main raw materials, taking toluene as a solvent, and taking tetra-n-butyl ammonium bromide as a catalyst to synthesize allyl isocyanate; then, under theaction of a noble metal catalyst such as platinum or rhodium, carrying out hydrosilylation with silicon-hydrogen bond containing hydrogenalkoxysilanes such as trimethoxy silane, triethoxy silane andthe like for carrying out a reaction to generate an isocyanate-based silane coupling agent crude product; and then carrying out reduced pressure distillation treatment to obtain the isocyanate-based silane coupling agent product. The method has the advantages of simple operation, high reaction conversion rate, high yield, stable quality, safe environment-friendly energy-saving efficient productionprocess, and the like, and industrial production is easy to realize.
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Paragraph 0020; 0021
(2019/10/01)
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- Preparation method of 3-isocyanatopropyltrialkoxysilane
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A preparation method of 3-isocyanatopropyltrialkoxysilane comprises the steps of (1) mixing 3-chloropropyltrialkoxysilane, urea and ammonium salt, heating to 120-130 DEG C, stirring to allow reactingfor 2-3 hours, cooling, and removing solid by centrifuging or filtering; (2) adding the separated liquid into a manganese or cobalt carboxylate catalyst, heating to 150-200 DEG C under nitrogen protection, and stirring to allow reacting for 1-2 hours; (3) sampling the reaction product, rectifying under reduced pressure after qualification is confirmed by detection, and separating the target product. The preparation method has the advantage of evidently reduced production cost.
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Paragraph 0017; 0019
(2019/03/25)
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- Preparation methods of carbamate alkoxyl silane and isocyanate alkoxyl silane
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The invention relates to a preparation method of carbamate alkoxyl silane and a preparation method of isocyanate alkoxyl silane. Particularly, firstly, environment-friendly nontoxic raw materials carbamate and chloropropyl alkoxyl silane are used for synthesizing carbamate alkoxyl silane, then carbamate alkoxyl silane is split under the mild condition, and isocyanate alkoxyl silane is obtained. The preparation methods have the advantages that the synthesis process is simple in route and belongs to green and clean production modes. The raw material carbamate is a nontoxic organic compound, andis easy to transport and store and free of leakage. The reaction condition is mild, no corrosion is caused to equipment in the reaction process, and the environment is not polluted. No solids or otherwastes are generated in the splitting process, and operation is easy.
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Paragraph 0051; 0052; 0054; 0055
(2018/10/19)
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- PREPARATION OF ISOCYANATOSILANES
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There is provided herein a method of preparing an isocyanatosilane including reacting an olefinic isocyanate with a hydridosilane in the presence of a dinuclear rhodium complex under hydro silylation conditions.
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Paragraph 0041-0054
(2019/01/05)
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- PRODUCTION OF ISOCYANATE FUNCTIONAL ORGANOSILANES
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Isocyanate-functional silanes are prepared in high yield by pyrolysis of an O-carbamate prepared by reaction of a dialkylcarbonate with an aminoalkyl-functional silane in the presence of a basic catalyst, where the catalyst is neutralized by an acid which has a pKa of all protolysis stages of not more than 4. The neutralized or partially neutralized catalyst need not be removed prior to pyrolysis. The isocyanato-functional silanes exhibit higher storage stability as compared to those prepared from O-carbamates where catalyst neutralization is effected by weak acids.
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Paragraph 0080-0085
(2017/11/30)
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- PROCESS FOR PRODUCING LOW-COLOR AND COLOR-STABLE ISOCYANATOORGANOSILANES AND PRODUCTS DERIVED THEREFROM
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The invention herein is directed to a process for producing isocyanatoorganosilanes having low color and improved color stability over known isocyanatosilanes involving a neutralizing step in which a carbamatoorganosilane intermediate is neutralized with acid to a pH equal to or greater than 6.0, to the isocyanatosilane produced by said process and to coatings and numerous other industrial applications which are useful in numerous industries containing the isocyanatoorganosilane produced by the process.
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Paragraph 0075
(2016/02/03)
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- Preparation method of 3-isocyanatopropyltrimethoxysilane
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The invention relates to a preparation method of 3-isocyanatopropyltrimethoxysilane and belongs to the technical field of organic chemistry. According to the preparation method, 3-aminopropyltrimethoxysilane and urea are taken as raw materials, dimethyl sulfoxide is taken as a solvent, a small amount of trimethyl orthoacetate is added for mixing, the mixture is stirred and heated and has a reaction in a vacuum condition, and a mixture containing (ureido)propyl silane is obtained; then a catalyst is added, reaction is performed continuously with diluted sulfuric acid, and isocyanate and sulfate are generated through deamination; filtering and rectification separation are performed, and a 3-isocyanatopropyltrimethoxysilane product is obtained. The preparation method has the advantages that the production raw materials are simple and available, potential risks in a production process are low, reaction conditions are mild, production equipment is simple, and the method is applicable to industrial production.
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Paragraph 0014
(2016/11/24)
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- Synthesis and properties of functionalized alkylalkoxysilanes
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A method of chloroalkylalkoxysilanes synthesis scalable to pilot production has been proposed. Morpholinotrialkoxysilanes have been prepared and studied as vulcanizing agents for low-molecular silicone rubbers. The reaction of N-morpholinomethyltrialkoxysilanes with triethanolamine has afforded N-[(silatranyl)-methyl]morpholine; it has been studied by X-ray analysis.
- Lebedev,Minas’yan,Abramkin,Sheludyakov,Kuzmina,Lebedeva,Surikov,Rybakov
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p. 1859 - 1863
(2016/10/04)
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- COMPOSITIONS COMPRISING ALKOXYSILANE-CONTAINING ISOCYANATES AND ACID STABILISERS
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The present invention relates to a composition comprising (A) an isocyanate of formula (I) OCN-A-SiR1R2R3 (I), wherein A is straight-chain, branched, substituted and/or unsubstituted aliphatic hydrocarbyl of 1 to 12 carbon atoms or substituted or unsubstituted cycloaliphatic hydrocarbyl of 4 to 18 carbon atoms, wherein R1 is selected from the group comprising —O—Ralk, wherein R2 and R3 are each independently selected from the group of substituents comprising —Ralk and —O—Ralk, and wherein —Ralk is hydrocarbyl of 1 to 6 carbon atoms, and B) a Bronstedt or Lewis acid or a compound which releases a Bronstedt or Lewis acid at room temperature; and also to a process for producing a stabilized alkoxysilane-containing isocyanate comprising the step of adding a Lewis or Bronstedt acid or a compound which releases a Bronstedt or Lewis acid at room temperature to an alkoxysilane-containing isocyanate.
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Paragraph 0110-0112
(2015/12/12)
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- PREPARATION OF ISOCYANATO SILANES
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A process for the preparation of alkoxysilyl group-containing isocyanate compounds which includes the step of reacting carbonyl chloride CIC(=0)CI with an alkoxysilyl group-containing amine in the presence of a high boiling point base, and optionally in the presence of an inert organic solvent, in order to minimize by product production and to simplify product purification, is disclosed.
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Page/Page column 25-26
(2014/01/07)
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- Method for producing isocyanate-organosilanes
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The invention describes a process for preparing isocyanatoorganosilanes by thermolysis of carbamatoorganosilanes in the presence of fluidized solid particles.
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Page/Page column 5-6
(2008/06/13)
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- Process for the production of isocyanatosilane and silylisocyanurate
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A process is provided for the production of isocyanatosilane from silylorganocarbamate in a cracking zone with a predetermined portion of purged reaction medium undergoing conversion in a trimerization zone to silylisocyanurate.
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Page/Page column 4
(2008/06/13)
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- Method for production of isocyanatosilanes
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A process is provided for the production of isocyanatosilane from silylorganocarbamate by neutralizing the basic catalyst with an acid to provide an inert metal halide salt, and subjecting the reaction mixture to cracking reaction conditions to obtain isocyanatosilane.
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Page/Page column 8
(2008/06/13)
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- METHOD FOR THE PRODUCTION OF ISOCYANATOORGANOSILANES
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The invention relates to a method for the production of isocyanatoorganosilanes by thermolysis of carbamatoorganosilanes with the aid of microwave radiation using homogeneous or heterogeneous catalysis.
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Page/Page column 12-13
(2008/06/13)
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- Process for preparing isocyanate group containing organosilicon compounds
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Organosilicon compounds with silicon-carbon linked or silicon-oxygen-carbon linked isocyanate groups are obtained by heating corresponding carbamate compounds with a low halide content. A method for the production of isocyanate group-containing organosilicon compounds (A) consisting of units of formula (Ia) involves heating organosilicon compounds (B) consisting of units of formula (Ib), with the proviso that (A) contain at least one group X while (B) contain at least one group Y and show a halide content of not more than 10000 ppm by weight; Ra(R1>O)bXcSiO(4-a-b-c)/2 (Ia); Ra(R1>O)bYcSiO(4-a-b-c-)/2 (Ib); X : a SiC- or SiOC-linked residue of formula -(O)g-Z-NCO (IIa); Y : a SiC- or SiOC-linked residue of formula -(O)g-Z-NH-COOR2> (IIb); g : 0 or 1; Z : an optionally substituted divalent hydrocarbon group, optionally with in-chain O, S, N or P; R, R1>, R2>SiC-linked, optionally substituted hydrocarbyl, optionally with in-chain O, S, N or P; a, b : 0, 1, 2 or 3; c : 0, 1, 2, 3 or 4; (a+b+c) : 4 or less.
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Page/Page column 4
(2008/06/13)
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- Hot oil process for producing isocyanato organosilanes
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Disclosed is a process for making isocyanatoorganosilane by adding a carbamatoorganosilane of the general formula to an inert liquid medium and holding the mixture thus formed at a temperature and pressure effective to convert said carbamatoorganosilane to isocyanatoorganosilane.
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