Zirconium modified silicon resin impregnating compound as well as preparation method and application thereof

A technology of modified silicon and sizing agent, which is applied in the field of sizing agent to improve the effect of temperature resistance

Active Publication Date: 2022-03-25
NORTHEASTERN UNIV LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are no related reports involving the infiltration and sizing of basalt fibers with zirconium-modified silicone resin and the interaction between the surface of basalt fibers and the coating interface.

Method used

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  • Zirconium modified silicon resin impregnating compound as well as preparation method and application thereof
  • Zirconium modified silicon resin impregnating compound as well as preparation method and application thereof
  • Zirconium modified silicon resin impregnating compound as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The zirconium-modified silicone resin in this example is prepared by the following method: first mix 0.02mol methyltriethoxysilane (MTES) and 0.005mol zirconium oxychloride octahydrate (ZrOCl 2 ·8H 2 O) Mix and stir until the zirconium oxychloride dissolves, then add 0.03mol of N-β-(aminoethyl)-γ-aminopropylmethyldimethoxysilane (KH602); 2ml of distilled water was added dropwise to carry out the hydrolysis-copolymerization reaction. After stirring for 40 min, 0.6g of glacial acetic acid (HA) was added until the resin was water-soluble. Finally, 0.002525 mol of hexamethyldisiloxane (HMDS) was added to the beaker as an end-capping agent, and the reaction was completed after stirring for 30 min. The synthesized zirconium-modified silicone resin sizing agent was named ZSR-1, and then diluted into a solution with a solid content of 0.7%, infiltrated and coated with basalt fibers, and the infiltrated fibers were designated as ZRBF-1.

Embodiment 2

[0042] The zirconium-modified silicone resin in this example is prepared by the following method: first mix 0.02mol methyltriethoxysilane (MTES) and 0.001mol zirconium oxychloride octahydrate (ZrOCl 2 ·8H 2 O) Mix and stir until the zirconium oxychloride dissolves, then add 0.03mol of N-β-(aminoethyl)-γ-aminopropylmethyldimethoxysilane (KH602); 2ml of distilled water was added dropwise to carry out the hydrolysis-copolymerization reaction. After stirring for 40 min, 0.6g of glacial acetic acid (HA) was added until the resin was water-soluble. Finally, 0.00255 mol of hexamethyldisiloxane (HMDS) was added to the beaker as an end-capping agent, and the reaction was completed after stirring for 30 min. The synthesized zirconium-modified silicone resin sizing agent was named ZSR-2, and then diluted into a solution with a solid content of 0.7%, infiltrated and coated with basalt fibers, and the infiltrated fibers were designated as ZRBF-2.

Embodiment 3

[0044]The zirconium-modified silicone resin in this example is prepared by the following method: first mix 0.02mol methyltriethoxysilane (MTES) and 0.0015mol zirconium oxychloride octahydrate (ZrOCl 2 ·8H 2 O) Mix and stir until the zirconium oxychloride dissolves, then add 0.03mol of N-β-(aminoethyl)-γ-aminopropylmethyldimethoxysilane (KH602); 1.75ml of distilled water was added dropwise to carry out the hydrolysis-copolymerization reaction. After stirring for 40 min, 0.9g of glacial acetic acid (HA) was added until the resin was water-soluble. Finally, 0.002575 mol of hexamethyldisiloxane (HMDS) was added to the beaker as an end-capping agent, and the reaction was completed after stirring for 30 minutes. The synthesized zirconium-modified silicone resin sizing agent was named ZSR-3, and then diluted into a solution with a solid content of 0.7%, infiltrated and coated with basalt fibers, and the infiltrated fibers were designated as ZRBF-3.

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Abstract

The invention belongs to the technical field of sizing agents, and particularly relates to a zirconium modified silicon resin impregnating compound as well as a preparation method and application thereof. The invention relates to a zirconium modified silicon resin impregnating compound which comprises the following components: zirconium oxychloride octahydrate (ZrOCl2. 8H2O), silicate ester, amino silane, organic acid and an end-capping reagent, the preparation method comprises the following steps: carrying out hydrolysis-copolymerization reaction on zirconium oxychloride octahydrate (ZrOCl2. 8H2O), silicate ester and amino silane, and adding organic acid and an end-capping reagent to finally obtain the zirconium modified silicon resin impregnating compound. The mechanical property test result of the basalt fiber single yarn shows that after heat treatment at 300 DEG C, the breaking strength of the ZRBF-2 group fiber is 376 N, and the breaking strength retention rate is 86.3%; the breaking strength of the BF fiber which is not subjected to infiltration treatment is 287.8 N and is far lower than that of ZRBF-2, so that the zirconium modified silicon resin impregnating compound can effectively improve the temperature resistance of the basalt fiber.

Description

technical field [0001] The invention belongs to the technical field of sizing agents, and in particular relates to a zirconium-modified silicone resin sizing agent and its preparation method and application. Background technique [0002] Basalt fiber is a continuous fiber made of natural volcanic extrusive rock, which is melted at a high temperature of 1500~1700°C and rapidly drawn. The main components include SiO 2 、Al 2 o 3 , CaO, MgO, Fe 2 o 3 And FeO, which has the advantages of excellent mechanical properties, high temperature resistance, stable chemical properties, low cost, environmental protection and non-toxicity, and does not contain carcinogens or other substances that are harmful to health. Basalt fiber fabrics have potential application prospects in many fields, such as refractory materials, filter materials, building materials, thermal insulation materials, etc. Fracture, difficult weaving, limited application. Therefore, at present, basalt fiber is gener...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/00C03C25/40C03C25/1095
CPCC08G79/00C03C25/40C03C25/1095
Inventor 罗洪杰王诏田程岩吴林丽
Owner NORTHEASTERN UNIV LIAONING
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