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Polyurethane structure-modified epoxy resin sizing agent emulsion and its preparation and application

An epoxy resin and polyurethane technology, applied in textiles and papermaking, fiber processing, carbon fiber, etc., can solve the problems of inability to meet the application requirements of the final composite material, the stability of the sizing agent emulsion is reduced, and the elasticity and wear resistance are lost. Conducive to stable industrial production, good application stability and low cost

Active Publication Date: 2016-06-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In practical engineering applications, after adding clustering functional additives to the water-based emulsion sizing agent, there are technical problems such as the stability of the sizing agent emulsion is reduced, easy to separate, and the solid content is not easy to control.
At the same time, due to the addition of components of clustering functional additives, the sizing carbon fibers are likely to harden, and lose the elasticity and wear resistance required for later fiber processing and molding, which cannot meet the application requirements of the final composite material.

Method used

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  • Polyurethane structure-modified epoxy resin sizing agent emulsion and its preparation and application
  • Polyurethane structure-modified epoxy resin sizing agent emulsion and its preparation and application
  • Polyurethane structure-modified epoxy resin sizing agent emulsion and its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-12

[0042] One, the preparation of the epoxy resin composition of polyurethane modification

[0043] Put the quantitative epoxy resin mixture in a 250ml four-neck flask with a mechanical stirring device, heat to 110°C, control the vacuum pressure at 100-0.1mmHg, and vacuum dehydrate for 2 hours until no bubbles are generated. Cool down to 70°C, remove the vacuum device, and insert a condenser tube. Under the protection of high-purity nitrogen, a quantitative amount of hexamethylene diisocyanate (HDI) was slowly added dropwise into the flask with a micro metering pump. After the dropwise addition, it was reacted at 70°C for 1 hour, and then the temperature was raised to 95°C. ℃ for more than 2 hours, sampling for infrared analysis, when the results show that there is no -NCO group, the polyurethane structure modified epoxy resin composition is prepared. The type and amount of epoxy resin mixture used, and the amount of hexamethylene diisocyanate (HDI) are shown in Table 1.

[004...

Embodiment 13-24

[0059] One, the preparation of the epoxy resin composition of polyurethane modification

[0060] Put the quantitative epoxy resin mixture in a 250ml four-neck flask with a mechanical stirring device, heat to 110°C, control the vacuum pressure at 100-0.1mmHg, and vacuum dehydrate for 2 hours until no bubbles are generated. Cool down to 70°C, remove the vacuum device, and insert a condenser tube. Under the protection of high-purity nitrogen, a quantitative amount of isophorone diisocyanate (IPDI) was slowly added dropwise to the flask with a micro metering pump. After the dropwise addition, it was reacted at 70°C for 1 hour, and then heated to 95°C After reacting for more than 2 hours, a sample was taken for infrared analysis, and when the result showed no -NCO group, a polyurethane structure-modified epoxy resin composition was obtained. The type and amount of epoxy resin mixture used, and the amount of isophorone diisocyanate (IPDI) are shown in Table 4.

[0061] Table 4. Re...

Embodiment 25-36

[0076] One, the preparation of the epoxy resin composition of polyurethane modification

[0077] Put the quantitative epoxy resin mixture in a 250ml four-neck flask with a mechanical stirring device, heat to 110°C, control the vacuum pressure at 100-0.1mmHg, and vacuum dehydrate for 2 hours until no bubbles are generated. Cool down to 50°C, remove the vacuum device, and insert a condenser tube. Under the protection of high-purity nitrogen, a quantitative amount of diphenylmethane diisocyanate (MDI) was slowly added dropwise into the flask with a micrometering pump. After the dropwise addition, it was reacted at 50°C for 1 hour, and then heated to 85°C. After reacting for more than 2 hours, a sample was taken for infrared analysis, and when the result showed no -NCO group, a polyurethane structure-modified epoxy resin composition was obtained. The type and amount of epoxy resin mixture used, and the amount of diphenylmethane diisocyanate (MDI) are shown in Table 7.

[0078] T...

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Abstract

The invention relates to a polyurethane structure modified epoxy resin sizing agent emulsion, which comprises the following ingredients: 55-78wt% of polyurethane structure modified epoxy resin composition, 20-40wt% of surfactant, 0.5-2wt% of anti-oxidant, 1-2wt% of levelling agent and 0.5-1wt% of antifreezing agent. The preparation method comprises the following steps: performing vacuum-pumping and dehydrating the bisphenol A epoxy resin to the condition that no bubbles can be generated, cooling and adding isocyanate to prepare a epoxy resin composition; mixing a surfactant and an antioxidant are mixed and homogenized in a reaction vessel according to the above material fraction, then adding deionized water, a levelling agent and an antifreezing agent gradually to obtain the polyurethane structure modified epoxy resin sizing agent emulsion. The carbon fiber prepared by the polyurethane structure modified epoxy resin sizing agent emulsion has good convergence, wear resistance and toughness, the convergence and wear resistance are easily and freely adjusted through the isocyanate component; a cluster agent is not required at the anaphase of the carbon fiber sizing agent, and on-site secondary mixing is not required, the application stability is good, the carbon fiber pasting wellability is good, and the polyurethane structure modified epoxy resin sizing agent emulsion is benefit for industrial stabilization and production of carbon fiber.

Description

technical field [0001] The invention belongs to the field of preparation of water-based epoxy sizing agent emulsion, and in particular relates to a polyurethane structure-modified epoxy resin sizing agent emulsion with good bundling properties and wear resistance, as well as its preparation and application. Background technique [0002] High-performance fibers represented by carbon fibers, graphite fibers, glass fibers, and aramid fibers are important basic reinforcement materials for the production of fiber-reinforced resin-based composites. Taking the engineering manufacturing of high-performance carbon fiber and graphite fiber as an example, in the production process, the surface chemical treatment and sizing of the fiber is an indispensable link in the research and production of carbon fiber ("Carbon Fiber and Graphite Fiber" by He Fu, Chemical Industry Press, 2010). Through the carbon fiber surface treatment and sizing process, on the one hand, the bundling properties,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/58D06M15/564D06M101/40
Inventor 季春晓刘瑞超曹阿民黄正林黄翔宇朱宗元刘礼华常丽许璐璐
Owner CHINA PETROLEUM & CHEM CORP
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