CN103787593B

CN103787593B - A kind of preparation method of alkali-resistant glass fiber

Info

Publication number: CN103787593B
Application number: CN201410011984.3A
Authority: CN
Inventors: 张志坚; 花蕾; 袁向静; 崔丽荣
Original assignee: Jushi Group Co Ltd
Current assignee: Jushi Group Co Ltd
Priority date: 2014-01-10
Filing date: 2014-01-10
Publication date: 2016-08-24
Anticipated expiration: 2034-01-10
Also published as: CN103787593A

Abstract

The invention discloses the preparation method of a kind of alkali-resistant glass fiber, comprise the steps: that (1) removes the wetting agent of E fiberglass surfacing by roasting；(2) the E glass fibre after processing step (1) by silane coupling A 187 carries out surface process；(3) by silane coupling A 1100, nano zirconia particles is carried out surface modification；(4) nano zirconia particles after making step (3) process is attached to the E fiberglass surfacing after step (2) processes, and reacts 1～4 hour in 80～130 DEG C, obtains alkali-resistant glass fiber.The inventive method can be by being chemically modified the alkaline resistance properties improving E glass fibre on the basis of retaining the physical property that original E glass fibre is excellent to fiberglass surfacing.

Description

A kind of preparation method of alkali-resistant glass fiber

Technical field

The present invention relates to the preparation method of a kind of alkali-resistant glass fiber.

Background technology

Alkali-free glass fibre (E glass fibre) is a kind of extraordinary lightweight, enhancing material high-strength, multi-functional Material.The feature of alkali-free glass fibre is that its alkaline metal oxide content is less than 1%, with middle alkali or alkali resistance Its excellent physical properties compared by glass fibre and alkali resistance is poor, building, chemical attack, insulation material, The application in the alkali resistance fields such as high-end packaging material has significant limitation.In recent years, both at home and abroad alkaline-resisting Also made substantial amounts of work in the research of property glass fibre, but their achievement in research be mainly based upon right The adjustment of metal oxide component in glass formula, i.e. by adjusting ZrO₂And TiO₂In glass formula Content reach to improve the purpose of alkali resistance of glass fibre, but this method cost is high, glass simultaneously Formula changes also drawing process whole on glass fibre generation can affect the fluctuation that result in properties of product, and In adjusting content of glass fiber after metal oxide component, the mechanical property of glass fibre and other physics Performance can be greatly affected, so finding the preparation method of a kind of development of new type alkali-resistant fibre glass fibre, is protecting The alkaline resistance properties improving E glass fibre on the basis of staying the physical property of original E glass fibre excellence seems outstanding For important, but it is not yet seen the report of the summary of the invention to this type of alkali-resistant glass fiber.

Summary of the invention:

The technical problem to be solved in the present invention is to provide the preparation method of a kind of alkali-resistant glass fiber, is retaining By fiberglass surfacing is chemically modified on the basis of the physical property that original E glass fibre is excellent Improve the alkaline resistance properties of E glass fibre.

The present invention solves the technical scheme that above-mentioned technical problem used:

The preparation method of a kind of alkali-resistant glass fiber, comprises the steps:

(1) wetting agent of E fiberglass surfacing is removed by roasting；

(2) the E glass fibre after processing step (1) by silane coupling A 187 carries out surface process；

(3) by silane coupling A 1100, nano zirconia particles is carried out surface modification；

(4) nano zirconia particles after making step (3) process is attached to the E glass after step (2) processes Glass fiber surface, and react 1～4 hour in 80～130 DEG C, obtain alkali-resistant glass fiber.

In described step (1), sintering temperature is at 400-550 DEG C, and roasting time was at 3-5 hour.

In described step (2), described surface processes and uses infusion process, the most first by silane coupling A 187 Being made into water solution A, then make E glass fibre impregnate in water solution A, taking-up is drying to obtain silane coupled E glass fibre after agent process.

Further, in water solution A, silane coupling A 187 is 0.5～5:100 with the mass ratio of deionized water, It is preferably 1:100.

Further, described dipping is at room temperature carried out, and dip time is 1-2 minute.

In described step (3), the diameter of described nano zirconia particles is between 10～100 nanometers, excellent Elect 10～30 nanometers as.Described surface is modified recommendation and is adopted with the following method: make nano zirconia particles and silicon Alkane coupling agent A1100 reacts 4～24 hours in 60～100 DEG C in a solvent, is then centrifuged for repairing to surface Nano zirconia particles after decorations.

Further, described solvent can be toluene, ethanol, acetone, deionized water/alcohol mixed solvent etc., Preferably in deionized water/alcohol mixed solvent, more preferably mixed solvent, the volume ratio of deionized water and ethanol is 1: 1。

Further, nano zirconia particles is 1:1～5:1 with the mass ratio of silane coupling A 1100, preferably For 2:1.

Further, the reaction temperature of nano zirconia particles and silane coupling A 1100 preferably 80 DEG C, reaction Time is preferably 12 hours.

In described step (4), receiving after step (3) can being made in the way of using coating or dipping to process Rice Zirconia particles is attached to the E fiberglass surfacing after step (2) processes.

In described step (4), reaction temperature preferably 100 DEG C, preferably 2 hours response time.

Preparation method of the present invention, E glass fibre and nano zirconia particles use end with ring respectively The silane coupling A 187 of oxygen groups and end carry out surface process with the coupling agent A1100 of amino, due to Amino and epoxide group can occur ring-opening reaction at a certain temperature, so that the zirconium oxide of modified Nanoparticle can successfully receive the surface of glass fibre, and can enter fiberglass surfacing fully Row cladding, reaches the effect protected fiberglass surfacing under conditions of alkalescence, improves alkali resistance Effect.

Compared with prior art, the beneficial effects of the present invention is: the present invention is retaining original E glass fibre The alkaline resistance properties of E glass fibre it is effectively increased on the basis of excellent physical property.

Accompanying drawing explanation

Fig. 1 is the synthesis schematic diagram that A1100 modifies nano zirconia particles.

Fig. 2 is the synthesis schematic diagram that A187 modifies E woven glass roving fabric.

Fig. 3 is the synthesis schematic diagram of nano zirconia particles modified glass fibers.

Detailed description of the invention

Below by specific embodiment, technical scheme is described further, but the protection of the present invention Scope is not limited to this:

Embodiment 1

1. select a common non-twist E fibre glass roving A to be placed in 400 DEG C of muffle furnaces 3 hours, fill Divide and remove surface wetting agent；

2. configure the A187 deionized water solution of 1% concentration, this kind of is removed the fibre glass roving of wetting agent A takes out room temperature after impregnating 1-2 minute in the A187 solution of 1% concentration and dries standby；

3. modify nano zirconia particles with A1100: weigh nano zirconia particles 10 grams, ultrasonic disperse in In the there-necked flask of the deionized water/alcohol solvent (volume ratio 1:1) of 500ml, stirring, to mix homogeneously, is dripped Add the A1100 coupling agent of 5g, after keeping 80 DEG C of temperature reflux to react after dropping 12 hours, with at a high speed The nano zirconia particles through coupling agent surface modified isolated from solvent by centrifuge, then by these grains Son is distributed in deionized water impregnate the rove after A187 processes, and dip time is 3-10 minute；

The most impregnated sample is placed in the baking oven of 100 DEG C baking 2 hours, finally obtains finished product.

Whole course of reaction and product are shown in Fig. 1, Fig. 2 and Fig. 3.

All samples is all tested through alkali resistance, i.e. glass fibre alkali resistance method of testing-sodium hydroxide solution soaks Method (GB/T20102-2006).All samples, including roving A, sodium hydroxide impregnated non-twist slightly Yarn A, the roving A of nano zircite modified and the impregnated nano zircite of sodium hydroxide are modified Roving A, alkali-resistant glass fiber rove C and sodium hydroxide solution to impregnate alkali resistant glass fine The mechanical property (fracture strength) of dimension rove C is to test according to GB/T7690.3-2001 standard, and Collect data, be shown in Table 1.

From the point of view of data result, through rove A the breaking after alkaline solution boils of nano zircite modified Resistance to spalling retention rate is the highest, next to that alkali-resistant glass fiber, and the fracture strength of common E glass fibre Retention rate is minimum.

Table 1 yarn breakage intensity data contrast table

Claims

1. a preparation method for alkali-resistant glass fiber, comprises the steps:

(1) wetting agent of E fiberglass surfacing is removed by roasting；

(3) by silane coupling A 1100, nano zirconia particles being carried out surface modification, described surface is repaiied Decorations are adopted with the following method: make nano zirconia particles and silane coupling A 1100 in a solvent in 60～100 DEG C React 4～24 hours, be then centrifuged for obtaining the nano zirconia particles after surface is modified；

2. preparation method as claimed in claim 1, it is characterised in that: in described step (1), roasting Temperature is at 400-550 DEG C, and roasting time was at 3-5 hour.

3. preparation method as claimed in claim 1, it is characterised in that: in described step (2), described Surface process use infusion process.

4. preparation method as claimed in claim 3, it is characterised in that described infusion process will be particularly as follows: first will Silane coupling A 187 is made into water solution A, then makes E glass fibre be sufficiently impregnated with in water solution A, Take out and be drying to obtain the E glass fibre after silane coupler processes, silane coupler in described water solution A A187 is 0.5～5:100 with the mass ratio of deionized water.

5. the preparation method as described in one of Claims 1 to 4, it is characterised in that: in described step (3), The diameter of described nano zirconia particles is between 10～100 nanometers.

6. the preparation method as described in one of Claims 1 to 4, it is characterised in that: described solvent be toluene, Ethanol, acetone or deionized water/alcohol mixed solvent.

7. the preparation method as described in one of Claims 1 to 4, it is characterised in that: in step (3), receive Rice Zirconia particles is 1:1～5:1 with the mass ratio of silane coupling A 1100.

8. the preparation method as described in one of Claims 1 to 4, it is characterised in that: nano zirconia particles and The reaction temperature of silane coupling A 1,100 80 DEG C, the response time is 12 hours.

9. preparation method as claimed in claim 1, it is characterised in that: in step (4), reaction temperature Being 100 DEG C, the response time is 2 hours.