High-silica glass fiber cloth and preparation method thereof

Abstract

The invention relates to the technical field of glass fibers, in particular to high-silica glass fiber cloth and a preparation method thereof.The preparation method comprises the following steps that glass fiber precursors are woven into cloth, and first glass fiber cloth is obtained; immersing the first glass fiber cloth in an impregnating compound for impregnating treatment to obtain second glass fiber cloth; performing acid leaching treatment on the second glass fiber cloth to obtain third glass fiber cloth; washing the third glass fiber cloth with water and then carrying out vacuum treatment to obtain fourth glass fiber cloth; and carrying out thermal sintering treatment on the fourth glass fiber cloth to obtain the high-silica glass fiber cloth. The high-silica glass fiber cloth obtained by the preparation method has relatively high mechanical strength.

Description

Technical Field

[0001] The invention relates to the technical field of glass fibers, and in particular to a high-silica glass fiber cloth and a preparation method thereof. Background Art

[0002] High silica glass fiber is the abbreviation of high-purity silicon oxide amorphous continuous fiber, with a silicon oxide content of 96-98%. It is widely used in spacecraft thermal ablation protection materials, high temperature resistant insulators, high temperature gas dust collection, liquid filtration, metal melting filtration, purification, etc.

[0003] The process principle of high-silica glass fiber is to utilize the separation of two or more incompatible liquid phases during the melting or cooling process of glass to form micro-inhomogeneities, and to utilize the phase separation of its structure to produce it. When the glass fiber is subjected to acid leaching treatment, the B2O3-Na2O phase dissolves into the acid solution, leaving behind a microporous silica skeleton. Subsequent high-temperature treatment closes the micropores to obtain a highly stable fiber material. However, the outflow of the B2O3-Na2O phase will inevitably lead to a decrease in the mechanical strength of the high-silica glass fiber. Although high-temperature treatment can improve the fiber strength to a certain extent, the fiber strength is still insufficient, which limits the use scenarios of the high-silica glass fiber. Summary of the invention

[0004] The purpose of the present invention is to solve the problems described in the above background technology. A high-silica glass fiber cloth and a preparation method thereof are provided. The high-silica glass fiber cloth obtained by the preparation method has higher fiber strength.

[0005] The technical solution adopted by the present invention to solve the technical problem is: a method for preparing high-silica glass fiber cloth, the preparation method comprising the following steps:

[0006] S1, weaving glass fiber raw yarn into cloth to obtain a first glass fiber cloth;

[0007] S2, immersing the first glass fiber cloth in a sizing agent for sizing treatment to obtain a second glass fiber cloth;

[0008] S3, subjecting the second glass fiber cloth to an acid leaching treatment to obtain a third glass fiber cloth;

[0009] S4, washing the third glass fiber cloth with water and then performing vacuum treatment to obtain a fourth glass fiber cloth;

[0010] S5. Performing thermal sintering on the fourth glass fiber cloth to obtain high-silica glass fiber cloth.

[0011] In the above technical solution, the surface of the first glass fiber cloth is treated by a wetting agent to form a film layer on the surface of the first glass fiber cloth. During acid leaching, the surface film layer is partially decomposed into nano-silicon dioxide under the catalysis of acid solution, and the B2O3-Na2O phase in the glass fiber is dissolved in the acid solution, and micropores are generated on the glass fiber. The residual acid solution is removed by water washing. Under the action of vacuum, the nano-silicon dioxide will be deposited into the micropores. Finally, during the thermal sintering treatment, the nano-silicon dioxide is combined with the glass fiber and the micropores are automatically closed, thereby enhancing the fiber strength of the glass fiber.

[0012] Preferably, the glass fiber precursor is prepared by a SiO2-B2O3-Na2O ternary system method.

[0013] Preferably, in step S2, the components of the wetting agent include a silane coupling agent and tetraethyl orthosilicate, and the volume ratio of the silane coupling agent to tetraethyl orthosilicate is 2:(1-3). Further preferably, the volume ratio of the silane coupling agent to tetraethyl orthosilicate is 1:1.

[0014] Preferably, in step S2, the conditions for the infiltration treatment are: an infiltration time of 1-2 hours and an infiltration temperature of 50-60°C. Preferably, in step S3, the acid leaching treatment is specifically: immersing the second glass fiber cloth in an acid solution at 80-90°C for 1-3 hours, and performing ultrasonic treatment at the same time.

[0015] The acid solution is selected from one of sulfuric acid, hydrochloric acid or nitric acid.

[0016] Preferably, the acid solution is hydrochloric acid, and the concentration of the hydrochloric acid is 2-5 mol / L. More preferably, the concentration of the hydrochloric acid is 4-5 mol / L.

[0017] Preferably, in step S4, the vacuum treatment is to place the washed third glass fiber in a closed container and perform vacuuming, so that the third glass fiber is kept in a vacuum environment for 5-10 minutes.

[0018] Preferably, in step S5, the heat sintering treatment is specifically as follows: sintering the fourth glass fiber cloth at 150-250°C for 10-15 minutes, then heating it to 600-800°C and sintering it for 0.5-1.5 hours. Further preferably, sintering the fourth glass fiber cloth at 200°C for 10-15 minutes, then heating it to 600-700°C and sintering it for 0.5-1.5 hours.

[0019] Preferably, after step 3 and step S4 are cyclically repeated at least 3 times, the operation of step S5 is continued.

[0020] A high-silica glass fiber cloth is prepared by the preparation method as described above.

[0021] The beneficial effects of the present invention are:

[0022] 1. The present invention forms a film layer on the surface of the first glass fiber cloth by using a sizing agent, decomposes ethyl orthosilicate under the catalysis of acid solution to form nano-silicon dioxide, fills the nano-silicon dioxide into the micropores of the glass fiber, and uses thermal sintering treatment to combine the nano-silicon dioxide with the glass fiber and seal the micropores, thereby greatly enhancing the fiber strength of the glass fiber and increasing the silicon oxygen content of the glass fiber cloth.

[0023] 2. The present invention uses ultrasonic treatment to assist the uniform deposition of nano-silicon dioxide into micropores, and makes the micropores generated when the B2O3-Na2O phase is dissolved in the acid solution uniformly distributed, so that the effect of reducing the fiber strength during the acid leaching treatment of the glass fiber is weakened.

[0024] 3. The present invention first weaves the glass fiber raw yarn into glass fiber cloth and then performs subsequent treatment, which is conducive to the deposition of nano-silicon dioxide on the surface of the glass fiber cloth, thereby increasing the deposition rate of nano-silicon dioxide into micropores. DETAILED DESCRIPTION

[0025] It should be noted that the following detailed descriptions are illustrative and are intended to provide further explanation of the present application. Unless otherwise specified, all technical and scientific terms used herein have the same meanings as those commonly understood by those skilled in the art to which the present application belongs.

[0026] It should be noted that the terms used herein are only for describing specific embodiments and are not intended to limit the exemplary embodiments according to the present application. As used herein, unless the context clearly indicates otherwise, the singular form is also intended to include the plural form. In addition, it should be understood that when the terms "comprise" and / or "include" are used in this specification, it indicates the presence of features, steps, operations, devices, components and / or combinations thereof.

[0027] The present invention is further described in conjunction with specific examples. The following examples are only for explaining the present invention, but do not constitute a limitation of the present invention. The test samples and test processes used in the following examples include the following (if the specific experimental conditions are not indicated in the examples, they are usually in accordance with conventional conditions or the conditions recommended by the reagent company; the reagents, consumables, etc. used in the following examples, if not otherwise specified, can all be obtained from commercial channels).

[0028] Example 1

[0029] A method for preparing high-silica glass fiber cloth, the steps of the preparation method are as follows:

[0030] S1, weaving glass fiber raw yarn into cloth to obtain a first glass fiber cloth, wherein the glass fiber raw yarn is prepared by a SiO2-B2O3-Na2O ternary system method;

[0031] S2, immersing the first glass fiber cloth in a sizing agent at 55° C. for 2 hours to obtain a second glass fiber cloth, wherein the sizing agent comprises a silane coupling agent and tetraethyl orthosilicate, and the volume ratio of the silane coupling agent to the tetraethyl orthosilicate is 1:1;

[0032] S3, immersing the second glass fiber cloth in an acid solution at 85° C. for 3 hours to obtain a third glass fiber cloth, wherein the acid solution is 2 mol / L hydrochloric acid;

[0033] S4, washing the third glass fiber cloth with water and placing it in a sealed container for vacuuming, so that the third glass fiber is kept in the vacuum environment for 10 minutes, to obtain a fourth glass fiber cloth;

[0034] S5. Sinter the fourth glass fiber cloth at 200° C. for 15 minutes, and then heat it to 600° C. and sinter it for 1 hour to obtain a high-silica glass fiber cloth.

[0035] Example 2

[0036] A method for preparing high-silica glass fiber cloth, the steps of the preparation method are as follows:

[0037] S1, weaving glass fiber raw yarn into cloth to obtain a first glass fiber cloth, wherein the glass fiber raw yarn is prepared by a SiO2-B2O3-Na2O ternary system method;

[0038] S2, immersing the first glass fiber cloth in a sizing agent at 55° C. for 2 hours to obtain a second glass fiber cloth, wherein the sizing agent comprises a silane coupling agent and tetraethyl orthosilicate, and the volume ratio of the silane coupling agent to the tetraethyl orthosilicate is 1:1;

[0039] S3, immersing the second glass fiber cloth in an acid solution at 85° C. for 3 hours to obtain a third glass fiber cloth, wherein the acid solution is 3 mol / L hydrochloric acid;

[0040] S4, washing the third glass fiber cloth with water and placing it in a sealed container for vacuuming, so that the third glass fiber is kept in the vacuum environment for 10 minutes, to obtain a fourth glass fiber cloth;

[0041] S5. Sinter the fourth glass fiber cloth at 200° C. for 15 minutes, and then heat it to 600° C. and sinter it for 1 hour to obtain a high-silica glass fiber cloth.

[0042] Example 3

[0043] A method for preparing high-silica glass fiber cloth, the steps of the preparation method are as follows:

[0044] S1, weaving glass fiber raw yarn into cloth to obtain a first glass fiber cloth, wherein the glass fiber raw yarn is prepared by a SiO2-B2O3-Na2O ternary system method;

[0045] S2, immersing the first glass fiber cloth in a sizing agent at 55° C. for 2 hours to obtain a second glass fiber cloth, wherein the sizing agent comprises a silane coupling agent and tetraethyl orthosilicate, and the volume ratio of the silane coupling agent to the tetraethyl orthosilicate is 1:1;

[0046] S3, immersing the second glass fiber cloth in an acid solution at 85° C. for 3 hours to obtain a third glass fiber cloth, wherein the acid solution is 4 mol / L hydrochloric acid;

[0047] S4, washing the third glass fiber cloth with water and placing it in a sealed container for vacuuming, so that the third glass fiber is kept in the vacuum environment for 10 minutes, to obtain a fourth glass fiber cloth;

[0048] S5. Sinter the fourth glass fiber cloth at 200° C. for 15 minutes, and then heat it to 600° C. and sinter it for 1 hour to obtain a high-silica glass fiber cloth.

[0049] Example 4

[0050] A method for preparing high-silica glass fiber cloth, the steps of the preparation method are as follows:

[0051] S1, weaving glass fiber raw yarn into cloth to obtain a first glass fiber cloth, wherein the glass fiber raw yarn is prepared by a SiO2-B2O3-Na2O ternary system method;

[0052] S2, immersing the first glass fiber cloth in a sizing agent at 55° C. for 2 hours to obtain a second glass fiber cloth, wherein the sizing agent comprises a silane coupling agent and tetraethyl orthosilicate, and the volume ratio of the silane coupling agent to the tetraethyl orthosilicate is 1:1;

[0053] S3, immersing the second glass fiber cloth in an acid solution at 85° C. for 3 hours to obtain a third glass fiber cloth, wherein the acid solution is 5 mol / L hydrochloric acid;

[0054] S4, washing the third glass fiber cloth with water and placing it in a sealed container for vacuuming, so that the third glass fiber is kept in the vacuum environment for 10 minutes, to obtain a fourth glass fiber cloth;

[0055] S5. Sinter the fourth glass fiber cloth at 200° C. for 15 minutes, and then heat it to 600° C. and sinter it for 1 hour to obtain a high-silica glass fiber cloth.

[0056] Example 5

[0057] A method for preparing high-silica glass fiber cloth, the steps of the preparation method are as follows:

[0058] S1, weaving glass fiber raw yarn into cloth to obtain a first glass fiber cloth, wherein the glass fiber raw yarn is prepared by a SiO2-B2O3-Na2O ternary system method;

[0059] S2, immersing the first glass fiber cloth in a sizing agent at 55° C. for 2 hours to obtain a second glass fiber cloth, wherein the sizing agent comprises a silane coupling agent and tetraethyl orthosilicate, and the volume ratio of the silane coupling agent to the tetraethyl orthosilicate is 1:0.5;

[0060] S3, immersing the second glass fiber cloth in an acid solution at 85° C. for 3 hours to obtain a third glass fiber cloth, wherein the acid solution is 4 mol / L hydrochloric acid;

[0061] S4, washing the third glass fiber cloth with water and placing it in a sealed container for vacuuming, so that the third glass fiber is kept in the vacuum environment for 10 minutes, to obtain a fourth glass fiber cloth;

[0062] S5. Sinter the fourth glass fiber cloth at 200° C. for 15 minutes, and then heat it to 600° C. and sinter it for 1 hour to obtain a high-silica glass fiber cloth.

[0063] Example 6

[0064] A method for preparing high-silica glass fiber cloth, the steps of the preparation method are as follows:

[0065] S1, weaving glass fiber raw yarn into cloth to obtain a first glass fiber cloth, wherein the glass fiber raw yarn is prepared by a SiO2-B2O3-Na2O ternary system method;

[0066] S2, immersing the first glass fiber cloth in a sizing agent at 55° C. for 2 hours to obtain a second glass fiber cloth, wherein the sizing agent comprises a silane coupling agent and tetraethyl orthosilicate, and the volume ratio of the silane coupling agent to the tetraethyl orthosilicate is 1:1.5;

[0067] S3, immersing the second glass fiber cloth in an acid solution at 85° C. for 3 hours to obtain a third glass fiber cloth, wherein the acid solution is 4 mol / L hydrochloric acid;

[0068] S4, washing the third glass fiber cloth with water and placing it in a sealed container for vacuuming, so that the third glass fiber is kept in the vacuum environment for 10 minutes, to obtain a fourth glass fiber cloth;

[0069] S5. Sinter the fourth glass fiber cloth at 200° C. for 15 minutes, and then heat it to 600° C. and sinter it for 1 hour to obtain a high-silica glass fiber cloth.

[0070] Comparative Example 1

[0071] A method for preparing high-silica glass fiber cloth, the steps of the preparation method are as follows:

[0072] S1, weaving glass fiber raw yarn into cloth to obtain a first glass fiber cloth, wherein the glass fiber raw yarn is prepared by a SiO2-B2O3-Na2O ternary system method;

[0073] S2, immersing the first glass fiber cloth in a sizing agent at 55° C. for 2 hours to obtain a second glass fiber cloth, wherein the sizing agent comprises a silane coupling agent and tetraethyl orthosilicate, and the volume ratio of the silane coupling agent to the tetraethyl orthosilicate is 1:1;

[0074] S3, immersing the second glass fiber cloth in an acid solution at 85° C. for 3 hours to obtain a third glass fiber cloth, wherein the acid solution is 4 mol / L hydrochloric acid;

[0075] S4, washing the third glass fiber cloth with water and placing it in a sealed container for vacuuming, so that the third glass fiber is kept in the vacuum environment for 10 minutes, to obtain a fourth glass fiber cloth;

[0076] S5. Sinter the fourth glass fiber cloth at 600° C. for 1 hour to obtain a high-silica glass fiber cloth.

[0077] Comparative Example 2

[0078] A method for preparing high-silica glass fiber cloth, the steps of the preparation method are as follows:

[0079] S1, weaving glass fiber raw yarn into cloth to obtain a first glass fiber cloth, wherein the glass fiber raw yarn is prepared by a SiO2-B2O3-Na2O ternary system method;

[0080] S2, immersing the second glass fiber cloth in an acid solution at 85° C. for 3 hours to obtain a third glass fiber cloth, wherein the acid solution is 4 mol / L hydrochloric acid;

[0081] S3, washing the third glass fiber cloth with water and placing it in a sealed container for vacuuming, so that the third glass fiber is kept in the vacuum environment for 10 minutes, to obtain a fourth glass fiber cloth;

[0082] S4. Sinter the fourth glass fiber cloth at 200° C. for 15 minutes, and then heat it to 600° C. and sinter it for 1 hour to obtain a high-silica glass fiber cloth.

[0083] A glass fiber from the high-silica glass fiber cloth prepared by the preparation method described in Example 1-6 and Comparative Example 1-2 was taken, and the tensile strength of the glass fiber was tested using a mechanical testing machine. The test results are shown in Table 1.

[0084] Table 1

[0085] project Tensile strength(MPa) Silicon oxygen content (%) Example 1 662 ＞97 Example 2 765 ＞97 Example 3 796 ＞97 Example 4 822 ＞97 Example 5 782 ＞97 Example 6 832 ＞96 Comparative Example 1 721 ＞97 Comparative Example 2 545 ＞95

[0086] From the comparison of Examples 1-4, it can be seen that with the increase of the acid concentration, the tensile strength of the glass fiber gradually increases. This may be because the increase in the acid concentration preserves the strength of the glass fiber and is conducive to the production of nano-silica; from the comparison of Example 1 and Examples 4 and 5, it can be seen that the tensile strength of the glass fiber first decreases and then increases with the increase of the volume ratio of the silane coupling agent and tetraethyl orthosilicate. This may be because with the increase of tetraethyl orthosilicate, the dissolution of the B2O3-Na2O phase in the glass fiber is hindered, resulting in an increase in the tensile strength of the glass fiber, but also a decrease in the silicon oxygen content in the glass fiber; from the comparison of Example 1 and Comparative Example 1, it can be seen that low-temperature pre-sintering during the thermal sintering treatment helps the nano-silica in the micropores to combine with the glass fiber, thereby enhancing the tensile strength of the glass fiber.

[0087] In this specification, each embodiment is described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the embodiments can be referred to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant parts can be referred to the method part.

[0088] The above is a detailed introduction to a high-silica glass fiber cloth and a preparation method thereof provided by the present invention. This article uses specific examples to illustrate the principles and implementation methods of the present invention. The description of the above embodiments is only used to help understand the method and core idea of ​​the present invention. It should be pointed out that for ordinary technicians in this technical field, without departing from the principle of the present invention, the present invention can also be improved and modified in a number of ways, and these improvements and modifications also fall within the scope of protection of the claims of the present invention.

Claims

1. A method for preparing high-silica glass fiber cloth, characterized in that: The preparation method comprises the following steps: S1, weaving glass fiber raw yarn into cloth to obtain a first glass fiber cloth; S2, immersing the first glass fiber cloth in a sizing agent for sizing treatment to obtain a second glass fiber cloth; S3, subjecting the second glass fiber cloth to an acid leaching treatment to obtain a third glass fiber cloth; S4, washing the third glass fiber cloth with water and then performing vacuum treatment to obtain a fourth glass fiber cloth; S5. Performing thermal sintering on the fourth glass fiber cloth to obtain high-silica glass fiber cloth.

2. The preparation method according to claim 1, characterized in that: The glass fiber raw yarn is prepared by SiO2-B2O3-Na2O ternary system method.

3. The preparation method according to claim 1, characterized in that: In step S2, the components of the wetting agent include a silane coupling agent and tetraethyl orthosilicate, and the volume ratio of the silane coupling agent to tetraethyl orthosilicate is 2:(1-3).

4. The preparation method according to claim 1, characterized in that: In step S2, the conditions of the infiltration treatment are: infiltration time 1-2h, infiltration temperature 50-60°C.

5. The preparation method according to claim 1, characterized in that: In step S3, the acid leaching treatment is specifically: immersing the second glass fiber cloth in an acid solution at 80-90° C. for 1-3 hours, while performing ultrasonic treatment, The acid solution is selected from one of sulfuric acid, hydrochloric acid or nitric acid.

6. The preparation method according to claim 5, characterized in that: The acid solution is hydrochloric acid, and the concentration of the hydrochloric acid is 2-5 mol / L.

7. The preparation method according to claim 1, characterized in that: In step S4, the vacuum treatment is to place the washed third glass fiber in a closed container and perform vacuuming, so that the third glass fiber is kept in a vacuum environment for 5-10 minutes.

8. The preparation method according to claim 1, characterized in that: In step S5, the thermal sintering treatment is specifically as follows: sintering the fourth glass fiber cloth at 150-250° C. for 10-15 minutes, and then heating it to 600-800° C. for 0.5-1.5 hours.

9. The preparation method according to claim 1, characterized in that: After step 3 and step S4 are repeated at least 3 times, the operation of step S5 is continued.

10. A high-silica glass fiber cloth, characterized in that: The high-silica glass fiber cloth is prepared by the preparation method according to any one of claims 1 to 9.