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Method for preparing amino siloxane

A technology of aminosiloxane and siloxane, which is applied in the field of preparation of aminosiloxane, can solve problems such as unsatisfactory catalytic effect, and achieve good catalytic effect, high reaction selectivity, and high reaction yield

Active Publication Date: 2015-05-13
济南市中未来产业发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, follow-up studies showed that PtO 2 Although it has a good catalytic effect on the addition of small molecule hydrogen-containing siloxane and unsaturated amine, it has a good catalytic effect on 1,1,3,3 tetramethyl-1,3-disiloxane, hydrogen-containing D4, etc. The catalytic effect of the hydrosilylation of organosiloxane with silicon-hydrogen bond and allylamine is not ideal

Method used

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  • Method for preparing amino siloxane
  • Method for preparing amino siloxane
  • Method for preparing amino siloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] in N 2 In the replaced kontes' tube, add allylamine (150mmol) and tetramethyldihydrodisiloxane (50mmol), simethicone 0.1g, PtO 2 0.0028g, seal the reaction vessel, stir and heat at 85°C, keep the temperature for 24 hours, the infrared test shows that the silicon-hydrogen bond disappears, let it stand and cool at room temperature, filter to remove PtO 2 , remove unreacted allylamine under reduced pressure, and distill under reduced pressure to obtain product 11g, 1 H-NMR shows that the content of γ-addition products is about 95%, and the product spectrum is shown in figure 1 .

Embodiment 2

[0030] in N 2 In the replaced kontes' tube, add allylamine (150mmol) and heptamethylcyclotetrasiloxane (50mmol), simethicone 0.15g, PtO 2 0.0028g, seal the reaction vessel, stir and heat at 85°C, keep the temperature for 24 hours, the infrared test shows that the silicon-hydrogen bond disappears, let it stand and cool at room temperature, filter to remove PtO 2 , remove unreacted allylamine under reduced pressure, distill under reduced pressure, obtain product 15.8g, 1 H-NMR showed that the content of γ-addition product was about 95%.

Embodiment 3

[0032] in N 2 Replaced in the kontes' tube, adding allylamine (150mmol) and a viscosity of 50,000 centipoise, 14.75g of methyl hydrogen silicone oil with a hydrogen content of 25%, PtO 2 0.0028g, airtight reaction vessel, stir and heat at 85°C, keep the temperature for 30 hours, the silicon-hydrogen bond disappears according to the infrared test, let it cool down at room temperature, filter to remove PtO 2 , remove unreacted allylamine under reduced pressure to obtain 17.6 g of product, 1 H-NMR showed that the content of γ-addition product was about 95%.

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Abstract

The invention relates to a method for preparing amino siloxane. The method comprises the following steps of: adding an unsaturated amine compound, siloxane containing silicon and hydrogen and platinum dioxide into a reactor in a mass ratio of (1-10): 1: (0.001-0.05); adding polysiloxane in an amount which is 0.1 to 1 percent of the total reaction substance quantity, wherein the molecular weight of polysiloxane is 5000 to 150000; introducing inert gas into the reactor to displace air, and sealing; and heating reactants to the temperature of between 40 and 150 DEG C, and reacting for 1 to 72 hours under stirring. The method is high in catalytic efficiency; the selectivity of a gamma-addition product is improved; PtO2 is a heterogenous catalyst and is easily separated from a system; and when the consumption of PtO2 is high, PtO2 can be recycled, so the yield is high.

Description

technical field [0001] The invention relates to a method for preparing aminosiloxane, which belongs to the field of organic silicon chemistry. Background technique [0002] Amino-containing siloxane is an important class of functional materials, widely used in the fields of fabric finishing, printing and dyeing, such as 1,3-dipropylamino-1,1,3,3-tetramethyldisiloxane Alkanes, aminopropyl polysiloxane, etc., are generally prepared by co-hydrolysis of corresponding aminosilane monomers in industry. The corresponding amino monomers are prepared by hydrosilylation. The hydrosilylation reaction is one of the important means to prepare silicone coupling agents, crosslinking agents and functionalized silicone polymers. Pd, Pt, Rh and other transition metal complexes have certain catalytic effects on the hydrosilylation reaction. activity, among which platinum-based catalysts are the most widely used. Commonly used platinum catalysts include chloroplatinic acid-isopropanol soluti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18
Inventor 周传健郑亚森陈国文张晨
Owner 济南市中未来产业发展有限公司
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