15396-00-6Relevant academic research and scientific papers
PREPARATION OF ISOCYANATOSILANES
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Paragraph 0051-0052, (2020/02/06)
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.
The isocyanate group-containing alkoxysilane method (by machine translation)
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Paragraph 0102; 0107-0112, (2020/10/03)
[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)
Preparation method of 3-isocyanatopropyltrialkoxysilane
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Paragraph 0017; 0019, (2019/03/25)
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.
Method for preparing isocyanate-based silane by hydrosilylation reaction
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Paragraph 0020; 0021, (2019/10/01)
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.
Method for preparing 3-isocyanatopropyltrimethoxysilane
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Paragraph 0032-0039, (2019/02/06)
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.
PROCESS FOR PREPARING ISOCYANATES CONTAINING ALKOXYSILANE GROUPS
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Paragraph 0087; 0088; 0089; 0090; 0091; 0092; 0093, (2019/10/17)
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.
PROCESS FOR PREPARING ISOCYANATES CONTAINING ALKOXYSILANE GROUPS
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Paragraph 0068-0071, (2019/10/17)
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.
PROCESS FOR PREPARING ISOCYANATES CONTAINING ALKOXYSILANE GROUPS
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Paragraph 0099-0103, (2019/10/23)
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.
PROCESS FOR PREPARING ISOCYANATES CONTAINING ALKOXYSILANE GROUPS
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Paragraph 0086-0088, (2019/10/23)
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.
PREPARATION OF ISOCYANATOSILANES
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Paragraph 0041-0054, (2019/01/05)
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.
