MODIFIED AEROGEL POWDER WITH SPECIAL FUNCTION GROUP FOR USE IN PLASTIC COMPOSITE AND FIBER SPINNING AND PREPARATION METHOD THEREOF

Abstract

A surface modified aerogel powder with special function group for used in plastic composite and fiber spinning applications are made from the following steps: (1) mixing step; (2) hydrolysis step; (3) condensation step within dispersion condition; (4) surface modification step; (5) solvent evaporation and drying step.

Claims

1. A method for manufacturing a function group modified aerogel particle for textile and fiber spinning, comprising: mixing step: blending an alkoxysilane compound mixed with a function group modified alkoxysilane compound and an organic solvent to form a mixture solution; hydrolysis step: adding one acid catalyst to the mixture solution for the hydrolysis reaction; condensation plus dispersion step: adding one base catalyst to the mixture solution for condensation reaction, and then adding a dispersing solvent during the condensation reaction with rapid stir, so that the mixture solution forms function group modified aerogel particles after gelation and dispersion; surface function group modification step: adding a surface modifier into the function group modified aerogel particles to further modify function group on the surface of each function group modified aerogel particle; and solvent evaporation and drying step: when the surface modified aerogel particles are formed in the dispersion solvent, evaporating the solvent at a high temperature or filtrating the surface modified aerogel particles with a colander, and later removing the solvent in a high-temperature dry oven to obtain the dried surface modified aerogel powder.

2. The manufacturing method of a function group modified aerogel particle for textile and fiber spinning as claimed in claim 1, wherein the function group modified alkoxysilane compound is a hydrophilic function group modified alkoxysilane compound selected from the group consisting of R group-trimethoxysilane (R-TMS) and R group-triethoxysilane (R-TES); each R group is a hydrophilic group comprising a carboxyl group (COOH), an amino group (NH.sub.2), an imino group (NH), a hydroxyl group (OH), an amido group (CONH), an epoxy group (COHCOH), an uricyl group (NHCONH), an isocyanate group (NCO), or an isocyanurate group (NCON) and has 1-8 carbon atom(s).

3. The manufacturing method of a function group modified aerogel particle for textile and fiber spinning as claimed in claim 1, wherein the function group modified alkoxysilane compound is a hydrophobic function group modified alkoxysilane compound selected from the group consisting of R group-trimethoxysilane (R-TMS), R group-triethoxysilane (R-TES), R group olefinic silica gel, and R group olefinic silane coupling agent; each R group is a hydrophobic group comprising an alkyl group (CH.sub.3), an alkenyl group (CCH.sub.2), an ester group (COO), an ether group (COC), an aromatic group (C.sub.6H.sub.4), or a halogen (X) and has 1-13 carbon atom(s).

4. The manufacturing method of a function group modified aerogel particle for textile and fiber spinning as claimed in claim 1, wherein the dispersion solvent is a hydrophilic solvent selected from the group consisting of water, distilled water, deionized water, alcohol, ether, ketone, carboxylic acid and amine.

5. The manufacturing method of a function group modified aerogel particle for textile and fiber spinning as claimed in claim 1, wherein the dispersion solvent is a hydrophobic dispersion solvent selected from the group consisting of ketone, ether, ester, aromatic hydrocarbon and alkane.

6. The manufacturing method of a function group modified aerogel particle for textile and fiber spinning as claimed in claim 1, wherein the surface function group modification step is provided for modifying the surface function group of the gelated mixture solution to enable the surface of the aerogel particle to form a complete function modified aerogel particle, enhancing the force between the aerogel powder and a substrate, and improving the aerogel's uniformity in a substrate to prevent breakage upon spinning caused by aggregation of the aerogel powder; wherein the surface modifier is a hydrophilic surface function group modifier selected from the group consisting of R group-trimethoxysilane (R-TMS) and R group-triethoxysilane (R-TES), and each R group is a hydrophilic group comprising a carboxyl group (COOH), an amino group (NH.sub.2), an imino group (NH), a hydroxyl group (OH), an amido group (CONH), an epoxy group (COHCOH), an uricyl group (NHCONH), an isocyanate group (NCO), or an isocyanurate group (NCON) and has 1-8 carbon atom(s), or the surface modifier is a hydrophobic surface function group modifier selected from the group consisting of R group-trimethoxysilane (R-TMS), R group-triethoxysilane (R-TES), R group olefinic silica gel, and R group olefinic silane coupling agent, and each R group is a hydrophobic group comprising an alkyl group (CH.sub.3), an alkenyl group (CCH.sub.2), an ester group (COO), an ether group (COC), an aromatic group (C.sub.6H.sub.4), or a halogen (X) and has 1-13 carbon atom(s).

7. The manufacturing method of a function group modified aerogel particle for textile and fiber spinning as claimed in claim 1, wherein the solvent evaporation and drying step further comprises: evaporating the solvent under ambient pressure and high temperature or filtrating the aerogel particle with a colander, and then drying the function group modified aerogel particle at 60-250 C., wherein the drying is performed by a fluidized bed reactor, a thermostatic drying oven, a roll drying machine, an agitated dryer, a spray dryer or a vacuum drying equipment.

8. The manufacturing method of a function group modified aerogel particle for textile and fiber spinning as claimed in claim 1, wherein in the condensation reaction, the diameter, porosity and cavity size of the surface function group modified aerogel particle are tuned according to a reaction condition including the content of the alkoxysilane, the content of the function group modified alkoxysilane, the content of the solvent, the solvent viscosity, the content of the acid catalyst, the content of the base catalyst, the content of the dispersion solvent and the stirring rate.

9. The manufacturing method of a function group modified aerogel particle for textile and fiber spinning as claimed in claim 1, wherein in the condensation reaction, the mixture solution gelates to form the function group modified aerogel particle during the stir at 200 rpm to 2000 rpm, and the function group modified aerogel particle has diameter of 10 nm-500 m.

10. A function group modified aerogel particle for textile and fiber spinning made according to the method as claimed in claim 1, wherein the function group modified aerogel particle is provided for being added to a substrate to improve the addition amount of the surface function group modified aerogel powder, enhance the spinning property of aerogel powder plastic during spinning process, and improve the applicability of the function group modified aerogel powder.

11. The function group modified aerogel particle for textile and fiber spinning as claimed in claim 10, wherein the spinning technique is common circular spinning, special-shaped section spinning, two components core-shell coaxial spinning, two components side-by-side spinning or multi-components multilateral spinning, so as to manufacture low-density, high warmth keeping, high coldness defending, anti-melting-drop and thermal insulative functional fiber.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0023] FIG. 1 is a flow chart of hydrophilic function group modification in this invention;

[0024] FIG. 2 is an SEM image of the function group modified aerogel powder prepared in this invention;

[0025] FIG. 3 is a TEM image of the function group modified aerogel powder prepared in this invention;

[0026] FIG. 4 is a picture of the hydrophilic amino group modified aerogel powder and the same blending Nylon particle prepared in this invention;

[0027] FIG. 5 is a picture of the hydrophobic methyl group modified aerogel powder and the same blending polypropylene particle prepared in this invention;

[0028] FIG. 6 is a picture of the function group modified aerogel powder and spinning fiber in this invention;

[0029] FIG. 7 is an SEM image of the section cut from the spinning fiber blending the function group modified aerogel powder in this invention;

[0030] FIG. 8 is a magnified SEM image of the section cut from the spinning fiber blending the function group modified aerogel powder in this invention; and

[0031] FIG. 9 is a magnified SEM image of the section cut from the spinning fiber blending the function group modified aerogel powder in this invention.

DETAILED DESCRIPTION OF THE INVENTION

[0032] The detailed description and preferred embodiments of the invention will be set forth in the following content, and provided for people skilled in the art so as to understand the characteristics of the invention.

[0033] Please refer to FIG. 1, which reveals the embodiment of preparing method of hydrophilic aerogel particle and hydrophobic aerogel particle in this invention, including the following steps: mixing step (S1), hydrolysis step (S2), condensation plus dispersion step (S3), surface function group modification step (S4) and solvent evaporation and drying step (S5). Wherein:

[0034] The mixing step (S1): An alkoxysilane compound mixed with function group modified alkoxysilane blends an organic solvent to form a mixture solution. The alkoxysilane compound is the precursor like tetramethoxysilane (TMOS), tetraethoxysilane (TEOS) or tetramethyl orthosilicate. The function group modified alkoxysilane is a hydrophobic compound like methyltrimethoxysilane (MTMS) or a hydrophilic compound like aminopropyltriethoxysilane (APTE), to which an organic solvent is added to form a mixture solution. The hydrophilic function group modified alkoxysilane compound is one or a combination of several materials selected from the group consisting of R group-trimethoxysilane (R-TMS) or R group-triethoxysilane (R-TES); each R group is a hydrophilic group comprising a carboxyl group (COOH), an amino group (NH.sub.2), an imino group (NH), a hydroxyl group (OH), an amido group (CONH), an epoxy group (COHCOH), an uricyl group (NHCONH), an isocyanate group (NCO), or an isocyanurate group (NCON) and has 1-8 carbon atom(s), as shown in the mixing step (S1). Whereas the hydrophobic function group modified alkoxysilane compound is one or a combination of several materials selected from the group consisting of R group-trimethoxysilane (R-TMS), R group-triethoxysilane (R-TES), R group olefinic silica gel, or R group olefinic silane coupling agent; each R group is a hydrophobic group comprising an alkyl group (CH.sub.3), an alkenyl group (CCH.sub.2), an ester group (COO), an ether group (COC), an aromatic group (C.sub.6H.sub.4), or a halogen (X) and has 1-13 carbon atom(s), as shown in the mixing step. The molar ratio of alkoxysilane compound and the function group modified alkoxysilane compound is within 0.0 mol % to 100.0 mol %. The addition of the modifier is to modify the function group in the microstructure of aerogel system. The content of alkoxysilane compound and hydrophobic function group modified alkoxysilane mixture is within 1.0 mol % to 60 mol %. The content of the organic solvent is within 99 mol % to 40 mol %.

[0035] The hydrolysis step (S2): add an acid catalyst to the mixture solution for hydrolysis, wherein the ratio between the total content of the alkoxysilane plus the function group modified alkoxysilane and the acid catalyst is 1:0.5-1:0.0001. Some aerogel modification process does not need to add acid catalyst to trigger hydrolysis.

[0036] In addition, the ratio of alkoxysilane compound and acid catalyst is 1:0.0001 to 1:0.5. When the ratio between the total content of the alkoxysilane plus the function group modified alkoxysilane and the acid catalyst is 1:0.0001, the hydrolysis takes 360 minutes. When the ratio between the total content of the alkoxysilane plus the function group modified alkoxysilane and the acid catalyst is 1:0.5, the hydrolysis takes 20 minutes. This thereby shows that the time of hydrolysis reduces as the content of acid catalyst increases.

[0037] The condensation plus dispersion step (S3): add a base catalyst to the mixture solution for condensation reaction. The ratio of acid catalyst's alcoholic solution and base catalyst's aqueous and alcoholic solution is 10:10 to 10:40. If the molar ratio of the base catalyst and the acid catalyst is 1.0:1.0 to 3.0:1.0, there is no need to add acid catalyst for hydrolysis but add proper amount of base catalyst for condensation.

[0038] In the base catalyst's alcoholic solution, the time of condensation is reduced notably as the content of the base catalyst increases (namely the gelation time of aerogel). When base catalyst: acid catalyst is 1.0:1.0, the gelation takes 1600 minutes. When base catalyst: acid catalyst is 3.0:1.0, the gelation time is reduced to 5 minutes. The process without the hydrolysis by acid catalyst can undergo condensation with addition of proper amount of base catalyst. Hence the process time can be adjusted by the content of base catalyst.

[0039] When the condensation reaction of the condensation plus dispersion step is nearly finished, the mixture solution forms sol first. Add a large amount of immiscible hydrophobic dispersion solvent to the mixture solution under the sol condition and rapidly stir at 200 rpm to 2000 rpm, so the mixture solution is influenced by the force of dispersion solvent under rapid stir to disperse the sol solution and forms 10 nm-500 m sol particle, which later gelates to form pearly or spherical wet-gel particle. Above mentioned wet-gel particle has diameter of 10 nm-500 m, and the volume ratio of the mixture solution and dispersion solvent is 1.0:0.5-1.0:5.0. The more the content of dispersion solvent has, the better the uniformity and dispersion of the aerogel particle prepared has.

[0040] The dispersion solvent for the preparation of hydrophilic aerogel particle in the condensation plus dispersion step (S3) can be water, distilled water, deionized water, C1-C16 alcohol, C2-C16 ether, C3-C16 ketone, C2-C16 ester, C1-C16 carboxylic acid, C1-C16 amine and so on. Practically, one or a mixture of different composition of water, distilled water, deionized water, methanol, ethanol, acetone, dibutyl ether, ethyl acetate, n-butyl acetate, formic acid or ammonia.

[0041] The dispersion solvent for the preparation of hydrophobic aerogel particle in the condensation plus dispersion step (S3) can be C3-C16 ketone, C2-C16 ether, C6-C16 aromatic hydrocarbon, C5-C16 alkane, C2-C16 halogenated ether, C2-C16 halogenated ester, C2-C16 aryl halide, C2-C16 haloalkane and so on. Practically, one or a mixture of different composition of acetone, dibutyl ether, ethyl acetate, n-butyl acetate, cyclohexane, n-hexane, toluene, kerosene or cleaning naphtha.

[0042] The surface function group modification step (S4): Add further surface modifier into the dispersion system of function group modified wet-gel particle for further modification. Herein the aim of modifying the function group of the aerogel powder is explicated as below: When the content of the function group modifier in step (1) is higher than 50 mol %, there is no need for further surface modification. Besides, the aim of the surface modification step is to modify the surface function group of aerogel's entire structure, so that both the surface of aerogel's micropore and main body are modified sufficiently. The hydrophilic surface function group modified alkoxysilane is one or a combination of several materials selected from the group consisting of R group-trimethoxysilane (R-TMS) or R group-triethoxysilane (R-TES); each R group is a hydrophilic group comprising a carboxyl group (COOH), an amino group (NH.sub.2), an imino group (NH), a hydroxyl group (OH), an amido group (CONH), an epoxy group (COHCOH), an uricyl group (NHCONH), an isocyanate group (NCO), or an isocyanurate group (NCON) and has 1-8 carbon atom(s), as shown in the modification step (S4). Whereas the hydrophobic surface function group modified alkoxysilane compound is one or a combination of several materials selected from the group consisting of R group-trimethoxysilane (R-TMS), R group-triethoxysilane (R-TES), R group olefinic silica gel, or R group olefinic silane coupling agent; each R group is a hydrophobic group comprising an alkyl group (CH.sub.3), an alkenyl group (CCH.sub.2), an ester group (COO), an ether group (COC), an aromatic group (C.sub.6H.sub.4), or a halogen (X) and has 1-13 carbon atom(s), as shown in the mixing step.

[0043] The solvent evaporation and drying step (S5): when the surface modified aerogel wet-gel particle is formed in the dispersion solvent, evaporate the solvent at a high temperature to obtain the surface modified aerogel particle, or filtrate the above mentioned surface modified aerogel wet-gel particle with a colander. Remove the large amount of dispersion solvent from the surface modified aerogel wet-gel system to obtain the surface modified aerogel particle. Preferably, dry with fluidized bed reactor or thermostatic drying oven at 60-250 C. to fast dry the solvent-containing surface modified aerogel particle, so that the dried surface modified aerogel powder can be obtained.

[0044] Through this, spherical, uniform in size and highly porous surface modified aerogel powder is prepared, which enhances the modification uniformity in outer and inner structure of the modified aerogel particle. In addition, through this technique, the surface function group modified aerogel can apply to various organic substrates like plastics, rubbers or adhesives. The applicability of aerogel powder increases. Especially the preparation of the surface function group modified aerogel powder can apply to textile or and fiber spinning. It can notably improve the amount of addition and blending uniformity of the surface function group modified aerogel powder in plastic's post-processing and on fiber spinning substrate to enhance the machinability of the surface function group modified aerogel powder and plastic composite, to enhance the spinning property of aerogel particle during spinning process, and to facilitate the mass production of the aerogel for the expansion of industrial application.

[0045] Please refer to FIGS. 2 and 3, which is transmission electron microscope (TEM) image and scanning electron microscope (SEM) image of the distribution and apparent size of the surface function group modified aerogel particle dispersed at 1600 rpm rapid stir. The images show that the apparent structure of the surface function group modified aerogel particle prepared has high uniformity with a spherical structure of diameter about 30-200 nm.

[0046] Please refer to FIGS. 4 and 5, which is the hydrophilic amino group modified aerogel particle and the same blending Nylon-6 and the hydrophobic methyl group modified aerogel particle and the same blending polypropylene (PP) particle. The images show that the surface function group modified aerogel particle prepared in this technique can highly blend different plastic substrates to form the plastic particle of high concentration of aerogel powder.

[0047] Please refer to FIG. 6, which is the surface function group modified aerogel particle prepared with different hydrophilic amino group and the Nylon spinning fiber blending 5%, 10% and 20% amino surface function group modified aerogel in the embodiment of this invention. The picture shows that the Nylon plastic blending 5%, 10% and 20% amino surface function group modified aerogel particle can produce the surface function group modified aerogel spinning fiber through spinning technique. The fiber spinning using the reeling technique of the function group modified aerogel particle can apply to common circular spinning, special-shaped section spinning, two components core-shell coaxial spinning, two components side-by-side spinning or multi-components multilateral spinning, so as to manufacture low-density, high warmth keeping, high coldness defending, anti-melting-drop and thermal insulative functional fiber.

[0048] Please refer to FIGS. 7, 8 and 9, which are SEM images of different magnifications of the spinning fiber section of 20% amino surface function group modified aerogel blending Nylon. FIG. 7 shows the whole spinning fiber section of 20% amino surface function group modified aerogel blending Nylon at 500 magnification. FIG. 8 shows a single spinning fiber section of 20% amino surface function group modified aerogel blending Nylon at 7,000 magnification. FIG. 9 shows entire spinning fiber section of 20% amino surface function group modified aerogel blending Nylon at 50,000 magnification. As shown in the pictures, the apparent structure of the fiber section of the amino modified aerogel particle has high uniformity with a spherical structure of diameter about 30-200 nm, which is in accordance with the apparent structure of the surface function group modified aerogel powder shown in FIGS. 2 and 3. This signifies that the surface function group modified aerogel powder prepared is very suitable for spinning fiber application.

[0049] While the invention has been described in connection with what is considered the most practical and preferred embodiment, it is understood that this invention is not limited to the disclosed embodiment but is intended to cover various arrangements included within the spirit and scope of the broadest interpretation so as to encompass all such modifications and equivalent arrangements.