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A kind of secondary aminosilane coupling agent and preparation method thereof

The technology of a secondary amino silane coupling agent and a terminal primary amino silane coupling agent is applied in the field of organic synthesis and can solve the problems of yellowing of silane-modified polyether/polyurethane polymers, difficult control of the reaction process and high activity of primary hydrogen atoms. , to achieve the effect of easy process control, simple and easy preparation method, and easy availability of raw materials

Active Publication Date: 2021-05-11
SHANGHAI DONGDA CHEM
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Problems solved by technology

The present application overcomes that in the prior art, when the primary ammonia silane is used as a capping agent to cap and modify the isocyanato polyether / polyurethane prepolymer, due to the high activity of its primary hydrogen atom, the reaction process is difficult to control and easy to Gel phenomenon occurs, and it is easy to cause yellowing of silane-modified polyether / polyurethane polymers, and a secondary aminosilane coupling agent and its preparation method and application are provided

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  • A kind of secondary aminosilane coupling agent and preparation method thereof

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[0029] In a specific embodiment, the present invention provides a method for preparing a secondary aminosilane coupling agent, comprising the steps of:

[0030] Carrying out the Michael addition reaction of the pretreated allyl-terminated polyether and the terminal primary aminosilane coupling agent under a nitrogen atmosphere to obtain the secondary aminosilane coupling agent;

[0031] The allyl-terminated polyether is monofunctional and has a number average molecular weight of 300-3000;

[0032] The pretreatment method of the allyl polyether is: add 0.05-5% antioxidant to the allyl polyether, react at 60-100°C for 0.5-3h under the protection of nitrogen, and then -0.085--0.095 MPa pressure, vacuum dehydration at 90-120°C for 0.5-2h, then cool down to 40-60°C;

[0033] The terminal primary aminosilane coupling agent is γ-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, γ-aminopropylmethyldimethoxysilane, γ-aminopropyl One or two mixtures of methyldiethoxysilane; ...

Embodiment 1

[0043] In a four-necked flask equipped with a stirrer, a constant pressure dropping funnel, and an air duct, 100 parts of pretreated allyl-terminated polyether (S1010, Shanghai Dongda Chemical Co., Ltd.) with a number average molecular weight of 1000 were added successively, Introduce nitrogen and start stirring, drop γ-aminopropyltrimethoxysilane at 40°C, the molar ratio of terminal allyl polyether to γ-aminopropyltrimethoxysilane is 1:1, drop within 30 minutes After the addition is completed, the temperature is raised to 60° C. and reacted for 10 hours to obtain the secondary aminosilane coupling agent.

Embodiment 2

[0045] In a four-necked flask equipped with a stirrer, a constant pressure dropping funnel, and an air duct, 100 parts of pretreated allyl-terminated polyether (S1010, Shanghai Dongda Chemical Co., Ltd.) with a number average molecular weight of 1000 were added successively, Infuse nitrogen and start stirring, drop γ-aminopropyltriethoxysilane at 40°C, the molar ratio of terminal allyl polyether to γ-aminopropyltriethoxysilane is 1:1, 30 minutes After the internal dropwise addition was completed, the temperature was raised to 90° C. and reacted for 4 hours to obtain the secondary aminosilane coupling agent.

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Abstract

The present application relates to a preparation method of a secondary aminosilane coupling agent, which comprises, under an inert atmosphere, performing a Michael addition reaction on a pre-treated allyl-terminated polyether and a primary aminosilane coupling agent to obtain the described Secondary aminosilane coupling agent; the pretreatment method of the allyl polyether is: add 0.05-5% antioxidant to the allyl polyether, under the protection of inert gas and at 60-100°C Reaction at a temperature of 0.5-3h, and then under the pressure of -0.085 to -0.095MPa and vacuum dehydration at a temperature of 90-120°C for 0.5-2h, and then lower the temperature to 40-60°C. The present application also relates to the secondary aminosilane coupling agent prepared by the above method, the isocyanate-based polyether polymer modified by it, the polyurethane polymer modified by it and its preparation method. The preparation method of the invention is simple, and the process of capping and modifying the polyurethane prepolymer by the prepared secondary aminosilane is easy to control without gel phenomenon.

Description

technical field [0001] The present application relates to the technical field of organic synthesis, in particular to a secondary aminosilane coupling agent and a preparation method thereof. Background technique [0002] Silane coupling agent is a kind of organosilicon compound containing two kinds of different chemical properties groups in the molecule at the same time, and its classic product can be used with the general formula YSiX 3 In the formula, Y is a non-hydrolyzable group, including alkenyl (mainly vinyl), and the end has Cl, NH 2 , SH, N 3 , (meth)acryloyloxy, isocyanate and other functional groups of hydrocarbon groups, that is, carbon functional groups; X is a hydrolyzable group. Due to this special structure, there are reactive groups in its molecule that can chemically bond with inorganic materials (such as glass, silica sand, metal, etc.) and chemically bond with organic materials (synthetic resins, etc.). For surface treatment, it can also be used as an a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/336C08G18/48C08G18/28
CPCC08G18/289C08G18/48C08G65/336
Inventor 何志强梅生富黄斌李欣怡
Owner SHANGHAI DONGDA CHEM
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