JPS62297235A - Apparatus for producing gel fiber - Google Patents

Abstract

PURPOSE:To obtain a gel fiber having various cross-section and uniform fiber diameter, stably over a long period, by supplying a specific sol solution through a sol solution spray nozzle into a cylindrical vessel furnished with a heating means, a humidifying means and a cooling means, etc. CONSTITUTION:A sol solution is produced by hydrolyzing an aqueous solution composed of a metal alkoxide [e.g. Si(OC2H5)4] and/or a substituted metal alkoxide [e.g. Si(OC2H5)3(CH3)]. The sol solution is supplied to a rotary container 5 of a cylindrical vessel 1 through a circular sol nozzle 53 or 22 having an inner diameter of 0.5-2mm and is cooled to 0-10 deg.C with a rotary container cooling pipe 6. Separately, the cylindrical vessel 1 is supplied with steam from a steam-supplying pipe 2 and the inside of the vessel 1 is maintained to 60-100 deg.C and >=60% humidity by controlling the heater 4. The rotary container 5 is rotated with a motor 7 at a rotational speed of about 1,500rpm to effect the centrifugal spraying of the sol in fibrous form through the sol nozzle 53 and the instantaneous solidification of the sprayed fibers. The obtained gel fiber having a circular cross-section of about 0.05mm in diameter and a length of about 13cm is received in a container.

Description

[Detailed Description of the Invention] 3. Detailed Description of the Invention (a) Field of Industrial Application - Day B! More specifically, the present invention relates to a gel fiber manufacturing machine for manufacturing gel fibers that are raw materials for glass fibers.

(b) Prior Art A method of producing glass by drying an alkoxytosyl solution obtained by mixing several metal alkyl alkoxides with alcohol, water, and a catalyst to form a gel, and then baking it in a kiln, is as follows. This method is well known as the sol-gel method.

In this sol-gel method, a metal alkyl alkoxide mixture in a sol state can be processed and molded to produce fibers and thin films of glass. Among these methods, a conventional method for producing gel fibers is to place a sol that has reached a certain viscosity into a container with holes, and then rotate the container to shake off the sol and form it into a fiber shape. It has been known.

(c) Problems to be solved by the invention However, when producing gel fibers by the above method, the viscosity range of the sol in which the fibers can be produced is narrow < (1
Furthermore, the viscosity of the sol is easily affected by temperature, humidity, etc., so the viscosity increases over time, resulting in the fiber diameter becoming thicker and causing variations in the fiber diameter. There were problems such as gelation occurring in the sol spout and sol storage container during spinning, making long-term spinning difficult.

The present invention has been made in view of this situation, and it is an object of the present invention to provide a gel fiber manufacturing machine that has a particularly constant fiber diameter and is capable of manufacturing fibers over a long period of time.

(d) Means for Solving the Problems According to the present invention, a sol solution supply port containing a metal alkoxide as a main component is provided in the upper part, and one or more spout ports for the sol solution are provided in the lower part of the side surface, and the rotating a cylindrical container body configured to allow cooling; a cooling means provided on the outer periphery of the cylindrical container body and capable of cooling the cylindrical container body to 0 to 10°C;
A container capable of accommodating the fibrous gel released from the spout when the cylindrical container body is rotated, and a heating means and humidifying means capable of maintaining the atmosphere inside the container at a temperature of 60 to 100°C and a humidity of 60% or more. Provided is a gel fiber manufacturing machine comprising:

The cylindrical container body used in this invention is preferably a cylindrical container body that is connected to a rotating means and has a rotating shaft connected to its upper part. Further, a spout for spouting out the sol solution is provided on the rotating side surface of the cylindrical container body, but the shape of this spout is preferably circular, in which case the inner diameter is 0.
5 to 2.0 ml11 is preferred.

Further, the spout may have an open end surface exposed on the side surface of the cylindrical container body, but the opening portion may also be provided so as to protrude to the outside of the side surface. Preferably, the protrusion has a conical shape. Further, it is preferable that the protruding direction is bent in a direction opposite to the rotating direction of the cylindrical container body. In this case, the bent state is such that the central axis of the sol spout provided at the tip of the protrusion is 0 to 90 degrees in the opposite rotation direction with respect to the direction of the centrifugal force acting on the protrusion when viewed from the top plan view. For horizontal planes, point downward.
Preferably, it is bent in the range of ~90°.

The cooling means provided on the outer periphery of the cylindrical container may be any means as long as it can cool the cylindrical container to a desired temperature, that is, 0 to 10"C, for example, by circulating cooling water. Examples include those with a transparent structure.

As a container capable of accommodating the released fibrous gel of the present invention, it is preferable to use a container that is equipped with a steam supply port, a steam discharge port, and heating and temperature control means, and is configured to maintain a constant humidity and temperature atmosphere. The humidified/heated atmosphere to be controlled has a humidity of 60% or more and a temperature of 60 to 10 degrees Celsius.

Furthermore, the outlet may be provided with a cooling means for cooling the steam to be discharged, and in this case, the cooling means is provided outside the container.

In this invention, the cylindrical container is rotatably supported at the center of the container, and is used such that at least the sol solution spout of the cylindrical container is located within the container.

Further, the rotational speed of the cylindrical container body is 1000 to 3000 r.
, p, m, are preferred.

The sol solution used in the production machine of the present invention is a sol solution obtained by hydrolyzing an aqueous solution comprising a metal alkoxide and/or a substituted metal alkoxide, or a concentrated sol solution.

The above-mentioned metal alkoxide may be any metal as long as it can form a gel by heat treatment and dehydration, such as silicon alkoxide, aluminum alkoxide, titanium alkoxide, boron alkoxide, sodium alkoxide, calcium alkoxide, etc. Aluminum alkoxide and titanium alkoxide are preferred.

In addition, a lower alkoxy group is suitable for the alkoxy group,
Examples include methoxy group, ethoxy group, propioxy group, and the like.

Examples of the metal alkoxides include silicon tetraethkind Si (OCtHs), triethoxyaluminum AI (OCxHS), tetraisopropioxytitanium T1 (0-iC3H7), and tetraethoxyzirconium Zr (OCtHS)4. silicon tetraethoxide is preferred.

Further, examples of the aliphatic hydrocarbon group substituted with the alkoxy group of the metal alkoxide include lower alkyl groups, vinyl groups, etc. Substituted metal alkoxides substituted with lower alkyl groups include, for example, S + (OCfH5
)3(CH3), Si(OCtH5)y(CHa)t
, S i (OCtH5)s (CxHs), S i (OC
tH5)t(CtHs)t, Si(OCtH5)s(
iCsHt), S i(OCyH5)t(i CsHv
)t, T i(0-i CsHt)a(CfHs), T
1(0-iC, Hヮ)*(C!Hs)t, A I(0
-i Cd]t)t(CH3), A I(0-I Cs
H7) t(CfH%), A](0-i CsH?)(
CHs)t,B (OCzHS)! (C2HS), Ca(OCtH5) (CtHC), and the like.

Examples of the aromatic hydrocarbon group substituted with the alkoxy group of the metal alkoxyde include phenyl groups or phenyl groups substituted with lower alkyl groups such as methyl, ethyl, and propyl groups.

Examples of the alkyl-substituted amino group on which the alkoxy group of the metal alkoxide is substituted include amino groups substituted with lower alkyl groups such as methyl, ethyl, or propyl groups.

The mixing weight ratio of the metal alkoxide and the substituted metal alkoxide is l:
1 to 5:1 is preferred.

As the aqueous solvent containing the metal alkoxide or the mixture of metal alkoxide and substituted metal alkoxide, a mixed solution of water and a lower alcohol such as methanol, ethanol, propatool, etc. is used as in the conventional method.

Further, as the hydrolysis catalyst, hydrochloric acid, sulfuric acid, ammonia aqueous solution, etc. are used as in the conventional method.

When an aqueous solution consisting of a metal alkoxide and/or a substituted Group 1 alkoxide is hydrolyzed to form a sol solution,
The hydrolysis reaction may be carried out by adding the hydrolysis catalyst to these aqueous solutions and stirring at room temperature, or the hydrolysis reaction may be accelerated by slightly raising the temperature. Further, the above hydrolysis reaction may be carried out by simultaneously adding and mixing a metal alkoxide, a substituted metal alkoxide, an aqueous solvent, and a hydrolysis catalyst.

The sol solution used in this invention has a viscosity of about 10 poise.

(E) Effect According to this invention, the sol solution, which has been cooled to a predetermined temperature and whose viscosity has been adjusted, is discharged in the form of threads from the sol solution spout into a predetermined humidified/heated atmosphere by centrifugal force, and is Due to the rapid environmental changes at the 200° C., gel fibers with a constant diameter and an appropriate hardness are produced.

The present invention will be described in detail below with reference to Examples, but the present invention is not limited thereby.

(f) Example FIG. 1 is an external view schematically showing an example of a gel fiber manufacturing machine of the present invention, and FIG. 2 is an explanatory view of the configuration of a longitudinal section thereof.

In Figures 1 and 2, (1) is an outer container, (2
) is the steam supply pipe, (3) is the steam discharge pipe, (4)
is a heater, (5) is a rotating container, (6) is a cooling pipe for cooling the rotating container, and (7) is a variable motor.

As shown in Fig. 2, the outer container (1) has a well-shaped recess (8) in which the center of the upper surface is recessed inward and has no bottom, and at the bottom thereof there is a cylindrical partition wall that reaches all the way to the bottom. (
9) is provided. A predetermined gap (10) is provided between the recess (8) and the partition wall (9), so that the inside of the container (1) communicates with outside air.

In addition, a steam supply pipe (2) is connected to the top surface of the container (1), and a steam discharge pipe (3) is connected to the bottom surface, and the bottom surface of the connection part of the steam discharge pipe (3) is convex to the outside. A cooling pipe (42) for circulating cold water for steam cooling is provided around the convex portion (41). These adjust the inside of the container (1) to maintain a predetermined humidity.

As shown in Fig. 3, the rotating container (5) is a cylindrical container (
At the center of the upper surface of 51) is a rotating shaft (11) for rotating the rotating container.
) and a sol solution inlet (
52) is provided. Also, at the lower side of the rotating container, there is a sol solution spout (inner diameter 1.0 II) that spouts the sol solution.
1m) (53) are set at equal intervals on the same horizontal plane.

Another example of the rotating container is shown in FIG. 4(a).

As shown in (b), each sol solution spouting part (2
1) is provided in a protruding conical shape, and a sol solution spout (inner diameter 1.0 m5) (22) is set at the tip of this conical shape. In this case, each sol solution spouting part (21) is bent and protrudes in a direction opposite to the rotation direction (a) of the rotating container. That is, the central axis (23) of the sol solution spout is about 120 degrees in the reverse rotation direction (b) with respect to the tangential direction (24) of the sol solution spout (FIG. 4(b)), Approximately 45 degrees downward (c) from the horizontal plane (25) (Fig. 4 (a)
) is set. The rotating container (5) configured as described above is inserted into the well-shaped recess (8) of the outer container (1), and the sol spouting port (53) or sol spouting part (21) of the rotating container is inserted into the well-shaped recess (8) of the outer container (1). The rotating shaft (9) of the rotating container is connected to a variable motor (7) and fixed at a position that can be located in the predetermined gap (10).

On the other hand, around the fixed rotating container (5) and on the side wall surface of the well-shaped recess (8), the rotating container (5)
A rotating vessel cooling pipe (6
) is attached.

A gel fiber was manufactured by preparing the sol solution sample shown below in the gel fiber manufacturing machine configured as described above. That is, S i (OCtHs) a 40mQ, S i (
OCtH5)3(CHs) 10iL' Ethanol5
0+ll12. Water 8-o and 1. ON -1-(Cl
1t*Q, to prepare a 1l aqueous solution with a pH of about 3, and this aqueous solution was hydrolyzed for 1 hour to obtain a uniform alkoxide sol solution. This was further dried until the viscosity became 5 to 250 poise. This sol solution was supplied into the rotating container (5) from the sol solution inlet (52) using a syringe.

Then, cold water was circulated through the cooling pipe (6) for cooling the rotating container to cool the sol solution in the rotating container to 0 to 10°C. On the other hand, steam is supplied from the steam supply pipe (2) to the external container body (1).
the outer container (1) by adjusting the heater (4).
) After maintaining the internal environment at 80% humidity and 80℃,
When the rotating container (5)' was rotated by the variable motor (7) at a rotation speed of 1500 r, p, m, the alkoxide sol solution in the rotating container (5) was caused by centrifugal force.
The fibrous sol is shaken out from the sol solution spout (53), and this fibrous sol is instantly solidified by moisture and heat in the above-mentioned humidity and temperature environment to become gel fibers, and the net (12)
fell on top. The gel fiber obtained as described above had a circular cross-sectional diameter of 0.05 mm+ and a length of about 13 ci.

(g) Effects of the invention According to the gel fiber manufacturing machine of this invention, the gel fiber production machine has a low viscosity (5 to 50%).
It is possible to produce fibers from a sol of about 15 poise), and fibers can be produced over a long period of time (at least 5 hours or more). Furthermore, it is possible to produce fibers with uniform diameters. By selecting the cross-sectional shape of the sol solution outlet, gel fibers having various cross-sectional shapes can be obtained. Furthermore, by making the sol solution spout have a protruding shape, the diameter of the outer container can be made smaller than that of a normal container, and furthermore, the gel fiber produced inside the outer container can be prevented from breaking. Can be done.

[Brief explanation of drawings]

Fig. 1 is an external view showing an outline of an example of the gel fiber manufacturing machine of the present invention, Fig. 2 is an explanatory diagram of its vertical cross-sectional configuration, and Fig. 3 is a structure of a rotating container used in the gel fiber manufacturing machine of the present invention. FIG. 4 is a structural explanatory diagram showing another example of the rotary container shown in FIG. 3. (1)...Outer container, (2)...
Steam supply pipe, (3)...Steam discharge pipe,
(4)... Heater, (5)... Rotating container, (6)... Cooling pipe for cooling the rotating container, (7)...
...Variable motor, (8) ... Well-shaped recess, (11) ... Rotating shaft, (52)
... Sol solution inlet, (53) (22) ...
... Sol solution spout, (21) ... Sol solution spout, tnl No. 4 (a) Figure (b) Ear & J group viewed from above (a)

Claims (1)

[Claims] 1. A supply port for a sol solution obtained by hydrolyzing an aqueous solution consisting of a metal alkoxide and/or a substituted metal alkoxide at the top, and one or more spout ports for the sol solution at the bottom of the side. A cylindrical container body configured to be equipped and rotatable, a cooling means provided on the outer periphery of the cylindrical container body and capable of cooling the cylindrical container body to 0 to 10°C, and a rotation of the cylindrical container body. A container capable of accommodating the fibrous gel ejected from the spout, and an atmosphere inside the container at a temperature of 60 to 100°C.
A gel fiber manufacturing machine comprising a heating means and a humidifying means capable of maintaining humidity at 60% or more. 2. The gel fiber manufacturing machine according to claim 1, wherein the sol ejection port is circular with an inner diameter of 0.5 to 2.0 mm.