- 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 0102-0106
(2020/10/03)
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- Preparation method of methyl 3-trimethoxysilane carbamate
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The invention discloses a preparation method of methyl 3-trimethoxysilane carbamate. The preparation method comprises the following steps: S1, reaction process; sequentially adding raw materials including aminosilane, dimethyl carbonate (DMC) and a catalyst into a reactor, wherein the molar ratio of aminosilane to dimethyl carbonate is (2:1) - (4:1), introducing nitrogen into the reactor to replace and discharge air, heating the reaction system to 90-115 DEG C under a stirring condition, and reacting for 15-20 hours under a micro-vacuum or normal-pressure condition to obtain a crude product; and S2, a post-treatment process: adding a proper amount of acid into the reaction system for neutralization, vacuumizing the reactor after the neutralization is finished, heating the reactor to 80-100DEG C for removing residual methanol and unreacted dimethyl carbonate, continuously heating the reactor to 160-180 DEG C, and distilling the reaction product to obtain a methyl 3-trimethoxysilane carbamate product. The selected reaction raw materials are wide and easy to obtain, the quality is controllable, the raw materials are low-toxicity chemicals, and use of high-toxicity, highly-toxic, flammable and combustible chemicals is avoided.
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Paragraph 0009-0010; 0026-0044
(2020/10/14)
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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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- 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) 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 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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- 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 0067-0071
(2017/11/30)
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- MANUFACTURING METHOD OF CARBAMATE ALKYLSILANE
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PROBLEM TO BE SOLVED: To provide a manufacturing method capable of providing carbamate alkylsilane effectively from a reaction mixture obtained from a reaction of aminoalkylsilane and a carbonic ester compound at high purity and high yield. SOLUTION: There is provided a manufacturing method of carbamate alkylsilane of the formula (3) by distilling a reaction mixture obtained by reacting an organic silicate compound represented by the formula (1) and a carbonic ester compound represented by the formula (2) in a presence of a metal catalyst containing one or more kinds of metal selected from Mn and Zn. R1 is a substituted/unsubstituted bifunctional hydrocarbon group with 3 to 6 carbon atoms, R2 and R3 are each independently a substituted/unsubstituted C1 to 10 monovalent hydrocarbon group and n is an integer of 0 to 2. R4 is each independently a substituted/unsubstituted C1 to 10 monovalent hydrocarbon group. SELECTED DRAWING: None COPYRIGHT: (C)2018,JPOandINPIT
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Paragraph 0042
(2018/03/23)
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- METHOD FOR PRODUCING CARBAMATOORGANOSILANES
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Carbamatoorganosilanes are produced in exceptionally high yield with a high degree of purity, by reacting an aminoorganosilane with a dialkylcarbonate in the presence of a basic catalyst, wherein a first reaction period proceeds at a temperature in the range of 35-65° C., followed by a later reaction period at a temperature at least 10° C. higher. A low level of catalyst allows its removal by simple exit filtration, without a separate filtration step.
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Paragraph 0058; 0059; 0060; 0061; 0062; 0063
(2016/08/17)
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- Heterobimetallic dinuclear lanthanide alkoxide complexes as acid-base bifunctional catalysts for synthesis of carbamates under solvent-free conditions
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Heterobimetallic dinuclear lanthanide alkoxide complexes Ln2Na8(OCH2CH2NMe2)12(OH)2 [Ln: I (Nd), II (Sm), III (Yb) and IV (Y)] were used as efficient acid-base bifunctional catalysts for the synthesis of carbamates from dialkyl carbonates and amines as well as the N-Boc protection of amines. The cooperative catalysts showed high catalytic activity and a wide scope of substrates with good to excellent yields under solvent-free conditions. The systems have shown higher catalytic activities due to the noteworthy synergistic interactions of Lewis acid center-Br?nsted basic center. The comparison of catalytic efficiency between mono- and dinuclear heterobimetallic lanthanide alkoxide analogues was also investigated.
- Zeng, Ruijie,Bao, Linquan,Sheng, Hongting,Sun, Lili,Chen, Man,Feng, Yan,Zhu, Manzhou
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p. 78576 - 78584
(2016/09/09)
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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 0073; 0074
(2016/02/03)
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- PROCESS FOR PREPARING CARBAMATOORGANOSILANES
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The invention provides a process for preparing carbamatoorganosilanes (S) of the general formula (7) in which a haloorganosilane (S1) of the general formula (8) [in-line-formulae]X—R2—SiR3(3-x)(OR4)x ??(8)[/in-line-formulae] is reacted with a metal cyanate (MOCN) and an alcohol (A) of the general formula (9) [in-line-formulae]R1OH ??(9)[/in-line-formulae] in the presence of at least one aprotic solvent (L), where R1, R3 and R4 are each an unsubstituted or halogen-substituted hydrocarbyl radical having 1-10 carbon atoms,R2 is a divalent unsubstituted or halogen-substituted hydrocarbyl radical which has 1-10 carbon atoms and may be interrupted by nonadjacent oxygen atoms,X is a halogen atom, andx is a value of 0, 1, 2 or 3, where the removal of the solid metal halides formed as by-products and of any solid metal cyanate residues still present is preceded by distillative removal of at least 50% of the solvent (L).
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Page/Page column 4
(2012/06/01)
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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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- Process for the preparation of N-silylorganocarbamates
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A process is provided for preparing an N-silylorganocarbamate, which comprises: providing a mixture of aminoorganosilane and a catalytically effective amount of basic catalyst and; combining the mixture of aminoorganosilane and basic catalyst with an organocarbonate ester the mixture of aminoorganosilane and basic catalyst, the organocarbonate ester or both being at elevated temperature at the time of their being combined.
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Page column 6-9
(2008/06/13)
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