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Preparation method of long-chain alkane and epoxy co-modified amino-terminated silicone oil

A technology of long-chain alkane and amino silicone oil, applied in the field of preparation of amino silicone oil, can solve various problems such as unsatisfactory properties, affecting physical properties, color change, etc., to improve the degree of yellowing, increase the waxy feeling and fluffy sense of effect

Inactive Publication Date: 2013-06-26
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the existence of amino groups in silicone oil, it will cause yellowing and discoloration during long-term storage, which will seriously affect its physical properties. In addition, the silicone oil with pure amino groups cannot be satisfactory in various properties, so in recent years Modified amino silicone oil has become a research hotspot, effectively promoting the emergence of new varieties

Method used

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  • Preparation method of long-chain alkane and epoxy co-modified amino-terminated silicone oil
  • Preparation method of long-chain alkane and epoxy co-modified amino-terminated silicone oil
  • Preparation method of long-chain alkane and epoxy co-modified amino-terminated silicone oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In a 1000ml four-necked flask equipped with a mechanical stirrer, condenser, thermometer, and nitrogen tube, add 300g octamethylcyclotetrasiloxane and 2.1g 1,3-bis(3-aminopropyl)-1, 1',3,3'-Tetramethyldisiloxane, stir and mix evenly, heat up to 60°C, add 12g of tetramethylammonium hydroxide alkali gum with a mass fraction of 1%, and stir for 0.5 hours, then heat up To 100°C, heat preservation reaction for 8 hours. Rapidly raise the temperature to 150°C to decompose the catalyst for 0.5 hours, then lower the temperature to 80°C, react at a vacuum of 0 MPa for 0.5 hours, and cool down to room temperature to obtain a colorless and transparent long-chain alkane-modified double-ended amino silicone oil.

[0032] 100 g of the obtained long-chain alkane-modified amino silicone oil was dissolved in 70 ml of toluene, and the temperature was raised to 65° C., under nitrogen protection, 1.6 g of epichlorohydrin was added, and the reaction was stirred for 6 hours. Afterwards, the ...

Embodiment 2

[0034] In a 1000ml four-necked flask equipped with a mechanical stirrer, a condenser, a thermometer, and a nitrogen tube, add 300g of octamethylcyclotetrasiloxane, 1g of octaalkylmethyldimethoxysiloxane and 4.5g of 1 , 3-bis(3-aminopropyl)-1,1',3,3'-tetramethyldisiloxane, stir and mix evenly, heat up to 80°C, add potassium hydroxide containing 1% mass fraction 15g of alkali glue was stirred and reacted for 1 hour, then the temperature was raised to 130°C, and the reaction was kept for 6 hours. React for 0.5 hour at a vacuum degree of 0 MPa, and cool down to room temperature to obtain a colorless and transparent long-chain alkane-modified double-ended amino silicone oil.

[0035] 100 g of the obtained long-chain alkane-modified amino-terminated silicone oil was dissolved in 100 ml of xylene, and the temperature was raised to 70° C., under nitrogen protection, 3.4 g of epichlorohydrin was added, and the reaction was stirred for 4 hours. Afterwards, the solvent was evaporated un...

Embodiment 3

[0037] In a 1000ml four-necked flask equipped with a mechanical stirrer, a condenser, a thermometer, and a nitrogen tube, add 300g of octamethylcyclotetrasiloxane, 2.1g of hexadecylmethyldimethoxysiloxane and 6g of 1,3-bis(3-aminopropyl)-1,1′,3,3′-tetramethyldisiloxane, stir and mix evenly, heat up to 70°C, add tetramethyldisiloxane containing 1% mass fraction 18 g of base ammonium hydroxide alkali gel and stirred for 0.5 hours, then heated up to 110° C., and kept for 7 hours. Rapidly raise the temperature to 150°C to decompose the catalyst for 0.5 hours, then lower the temperature to 80°C, react for 1.5 hours under a vacuum of 0 MPa, and cool down to room temperature to obtain a colorless and transparent long-chain alkane-modified double-ended amino silicone oil.

[0038] 100 g of the obtained long-chain alkane-modified amino silicone oil was dissolved in 60 ml of petroleum ether, and the temperature was raised to 80° C., under nitrogen protection, 4.5 g of epichlorohydrin wa...

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Abstract

The invention relates to a preparation method of long-chain alkane and epoxy co-modified amino-terminated silicone oil. The structural formula of the long-chain alkane and epoxy co-modified amino-terminated silicone oil is represented by figure 1 in the specification. The preparation method of the modified silicone oil comprises the following steps: adding octamethylcyclotetrasiloxane, a long-chain alkane coupling agent and an amino-terminated silane end capping agent according to certain proportions, uniformly stirring, heating to 60-80DEG C, adding an alkaline catalyst, reacting under stirring for 0.5-1.5h, controlling the reaction temperature in a range of 90-140DEG C, carrying out a temperature maintenance reaction for a period of time, carrying out reduced pressure distillation to obtain a low-boiling-point substance which is modified silicone oil, dissolving the modified silicone oil in a solvent, reacting with epichlorohydrin at 50-100DEG C for 2-7h, and carrying out reduced pressure evaporation to remove the solvent in order to obtain the long-chain alkane and epoxy co-modified amino-terminated silicone oil. The long-chain alkane and epoxy co-modified amino-terminated silicone oil is mixed with an emulsifier and an acid, are added with deionized water in batch, and undergoes pH adjustment by the acid to about 7 in order to obtain an emulsion of the long-chain alkane and epoxy co-modified amino-terminated silicone oil. The long-chain alkane and epoxy co-modified amino-terminated silicone oil prepared in the invention overcomes the yellow disadvantage of amino silicone oil, and has the advantages of good lubrication property, good hydrophobicity and good fluffy feeling when the long-chain alkane and epoxy co-modified amino-terminated silicone oil is used for texture finishing.

Description

technical field [0001] The invention relates to a preparation method of amino silicone oil, in particular to a preparation method of long-chain alkane and epoxy co-modified double-end amino silicone oil. Background technique [0002] In recent years, various countries have carried out extensive and in-depth development and research on the auxiliary amino silicone oil used in the textile industry. It is currently the most widely used silicone auxiliary in the domestic and foreign markets for fabric finishing. It can give cotton, hemp, All kinds of fabrics such as nylon and silk have soft, smooth and plump feel. At the same time, amino silicone oil is also a conditioner for cosmetics or hair, and is widely used in products such as shampoo and hair conditioner. Since amino silicone oil is easy to interact with the negative charge on the hair, it can be firmly adsorbed on the surface of the hair, giving the hair good suppleness and luster, and at the same time antistatic and dr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/388
Inventor 郑昌戈张鹏李萍
Owner JIANGNAN UNIV
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