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Preparation method of isocyanate modified polyether silicone oil nonionic emulsion and product and application thereof

A technology of polyether silicone oil and isocyanate, which is applied in textiles and papermaking, fiber treatment, carbon fiber, etc. It can solve the problems of poor storage stability, unstable storage of amino-modified silicone oil, hairiness, etc., and achieve reduced surface tension and good emulsion stability. , Lubrication effect of surface tension

Active Publication Date: 2019-07-23
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 product and application thereof
  • Preparation method of isocyanate modified polyether silicone oil nonionic emulsion and product and application thereof
  • Preparation method of isocyanate modified polyether silicone oil nonionic emulsion and product and application thereof

Examples

Experimental program
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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 preparation method of an isocyanate modified polyether silicone oil nonionic emulsion and a product and application thereof. The method comprises the steps of synthesizing double-end containing hydrogen silicone oil, synthesizing double-end hydroxyl modified silicone oil, synthesizing isocyanate modified polyether silicone oil, adding a proper amount of water for emulsifying, performing co-emulsifying with cationic amino modified epoxy silicone oil, and performing compounding to prepare a carbon fiber precursor oil agent. The technical problems met during an addition reaction of polyether modified silicone oil and high molecular weight polyethylene glycol monoallyl ether through containing hydrogen silicone oil that the reaction is difficult, the yield is low, theseparation purification is hard, and the color is dark are solved, and meanwhile the problems that the storage stability of amino modified silicone oil in the weak acid water phase is poor, compounding with cationic amino modified epoxy silicone oil is performed to prepare the carbon fiber precursor oil agent, after oiling, the carbon fiber precursor is stuck to rollers in the high-temperature drying and rolling process are solved.

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 Applications(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
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