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Preparation method of isocyanate modified polyether silicone oil nonionic emulsion and its products and applications

A polyether silicone oil and isocyanate technology, which is applied in textiles and papermaking, fiber treatment, carbon fiber, etc., can solve problems such as difficult realization of hydrosilicon addition reaction, hairiness, unstable storage of amino-modified silicone oil, etc.

Active Publication Date: 2021-09-14
吉林乾仁新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention is aimed at the deficiencies of the prior art, such as the preparation of polyether-modified silicone oil using the hydrosilylation reaction of hydrogen-containing silicone oil and allyl polyether is difficult to achieve; amino-modified silicone oil is stored in an aqueous phase system under weakly acidic conditions Poor stability, the oil prepared by compounding with epoxy-modified silicone oil also inherits the shortcoming of unstable storage of amino-modified silicone oil, and it is easy to cause the carbon fiber precursor to stick to the roller during the oiling process, resulting in problems such as hairiness and broken filaments

Method used

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  • Preparation method of isocyanate modified polyether silicone oil nonionic emulsion and its products and applications
  • Preparation method of isocyanate modified polyether silicone oil nonionic emulsion and its products and applications
  • Preparation method of isocyanate modified polyether silicone oil nonionic emulsion and its products and applications

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Add 172.48g of dried octamethylcyclotetrasiloxane and 26.70g of end-capping agent 1,1,3,3-tetramethyldisiloxane into a four-port open reaction kettle equipped with a thermometer and agitator and 3.00 g of concentrated sulfuric acid were reacted in an oil bath at 45° C. for 7 hours under the protection of nitrogen. Then add 10.20g of sodium bicarbonate to continue the reaction for 2 hours to neutralize the catalyst. After the reaction, carry out suction filtration, and place the filtrate in an oil bath at 120°C for vacuum rotary evaporation to remove unreacted substances. Terminal hydrogen silicone oil.

[0045] Dry the ethylene glycol monoallyl ether with anhydrous sodium sulfate for more than 7 hours, and then pour the ethylene glycol monoallyl ether into the reaction kettle. Put 1000 molecular weight double-ended hydrogen-containing silicone oil into another reaction kettle, pass nitrogen gas into the oil bath at 120°C to remove water for 2 hours, cool to 60°C, add p...

Embodiment 2

[0047] Add 180.47g of dried octamethylcyclotetrasiloxane and 17.75g of end-capping agent 1,1,3,3-tetramethyldisiloxane into a four-port open reaction kettle equipped with a thermometer and agitator and 3.00 g of concentrated sulfuric acid were reacted in an oil bath at 45° C. for 7 hours under the protection of nitrogen. Then add 10.20g of sodium bicarbonate to continue the reaction for 2 hours to neutralize the catalyst. Suction filtration is performed after the reaction, and the filtrate is placed in an oil bath at 120° C. for vacuum rotary evaporation to remove unreacted substances. Terminal hydrogen silicone oil.

[0048] Dry the ethylene glycol monoallyl ether with anhydrous sodium sulfate for more than 7 hours, and then pour the ethylene glycol monoallyl ether into the reaction kettle. Put 1500 molecular weight double-ended hydrogen-containing silicone oil into another reaction kettle, pass nitrogen gas into the oil bath at 120°C to remove water for 2 hours, cool to 60°...

Embodiment 3

[0050] Add 186.12g of dried octamethylcyclotetrasiloxane and 13.40g of end-capping agent 1,1,3,3-tetramethyldisiloxane into a four-port open reaction kettle equipped with a thermometer and agitator and 3.00 g of concentrated sulfuric acid were reacted in an oil bath at 45° C. for 7 hours under the protection of nitrogen. Then add 10.20g of sodium bicarbonate and continue to react for 2 hours to neutralize the catalyst. After the reaction, carry out suction filtration, and place the filtrate in an oil bath at 120°C for vacuum rotary evaporation to remove unreacted substances. Terminal hydrogen silicone oil.

[0051] Dry the ethylene glycol monoallyl ether with anhydrous sodium sulfate for more than 7 hours, and then pour the ethylene glycol monoallyl ether into the reaction kettle. Put 2000 molecular weight double-ended hydrogen-containing silicone oil into another reaction kettle, pass nitrogen gas into an oil bath at 120°C to remove water for 2 hours, cool to 60°C, add plati...

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Abstract

The invention provides a method for preparing isocyanate-modified polyether silicone oil nonionic emulsion and its products and applications, including the synthesis of double-end hydrogen-containing silicone oil, the synthesis of double-end hydroxyl modified silicone oil, and the synthesis of isocyanate-modified polyether silicone oil. Add appropriate amount of water to emulsify, co-emulsify with cationic amino-modified epoxy silicone oil, and compound to prepare carbon fiber raw silk oil. The present invention overcomes the technical problems that polyether modified silicone oil encounters through the addition reaction of hydrogen-containing silicone oil and high-molecular weight polyethylene glycol monoallyl ether, such as difficult reaction, low yield, difficult separation and purification, and dark color. Amino-modified silicone oil has poor storage stability in weakly acidic water phase. It is compounded with cationic amino-modified epoxy silicone oil to prepare carbon fiber precursor oil. After oiling, the carbon fiber precursor will stick to the roll during high-temperature drying and winding.

Description

technical field [0001] The present invention relates to the preparation, product and application of a modification aid used in the production of polyacrylonitrile carbon fiber precursors, in particular to a preparation method of isocyanate-modified polyether silicone oil nonionic emulsion and its product and application . Background technique [0002] The role of the oil agent used in the production of carbon fiber precursors is mainly to increase the strength of carbon fiber precursors and play an antistatic role on the fiber surface. It is especially important to prevent carbon fiber precursors from being caused by high temperature (200~300°C) during pre-oxidation. Fiber sticking, paralleling, fusing and burning, so the oil used for carbon fiber precursors generally uses modified silicone oil, usually epoxy-modified silicone oil, amino-modified silicone oil and polyether (polyethylene glycol) modified silicone oil three Classes and their combinations. Modified silicone o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D06M15/647D06M15/65C08G77/46C08G77/12C08G77/38D06M101/40
CPCC08G77/12C08G77/38C08G77/46D06M15/647D06M15/652D06M2101/40
Inventor 杨春才贾宏菲李健华
Owner 吉林乾仁新材料有限公司