JPS5939382B2 - Method for reinforcing inorganic fibers - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION In the present invention, inorganic fibers 5 immediately after cotton production are fed into a surface treatment tank 1, and the general formula is T i (0R)4 (R=C4 crosspiece).

C3H7, C2H5] The organic titanium compound treated vapor 19 and the water vapor 18 are brought into continuous contact with the inorganic fibers 5, and the concentration ratio of the above water vapor 18 and the treated vapor 19 with respect to the direction of transport of the inorganic fibers 5 is adjusted. Relating to a method for reinforcing inorganic fibers characterized by providing a gradient,
The purpose is to provide a method for reinforcing inorganic fibers that can more reliably strengthen the inorganic fibers with a protective film.

Generally, inorganic fibers such as glass wool and rock wool have a very high tensile strength (200 to 300 kg/my?t) unless there is mechanical or chemical surface damage after melt spinning.

In order to avoid this mechanical and chemical surface damage, for example, with respect to long glass fibers, various resin coatings called sizing agents are uniformly applied to the fiber surfaces.

However, since inorganic fibers such as glass wool and rock wool are made in large quantities by the disc method or high-speed air blowing method, the surface treatment during cotton production is limited to a binder spray, which forms a uniform film on the fiber surface. It was not possible to do so, and droplets were partially attached.

For this reason, even after surface treatment, wool-like short glass fibers were significantly degraded by mechanical contact after cotton-making.

In view of these circumstances, in order to form a uniform protective film on the surface of wool-like glass short fibers and maintain their initial strength, a surface treatment agent is sprayed in vapor form immediately after cotton production to coat the fiber surface at high temperature. Methods of causing chemical reactions such as thermal decomposition are being considered, but at present, satisfactory results have not been obtained because the uniformity and thickness of the film attached to the fiber surface are still insufficient.

Generally, inorganic short fibers such as glass wool and rock wool are produced by introducing mineral raw materials melted at a high temperature of 1,300 to 1,500 degrees Celsius onto a disk rotating at high speed, and the centrifugal force of the fibers forming the fibers from around the disk or ejecting them from a nozzle. It is blown away by high-speed airflow or flame and turned into fibers.

These fibers are fed into a collection box by the transport air current, collected on a conveyor net conveyor belt, etc., and transported.

The present invention treats inorganic fibers that are loosely deposited on a conveyor net (belt) immediately after cotton production with an organic titanium compound during cotton collection, and will be described in detail below with reference to the accompanying drawings.

First, the above-mentioned inorganic fiber 5 immediately after cotton-making is left as it is (
(without applying a large external force) into the surface treatment tank 1.

FIG. 1 schematically illustrates an embodiment of the apparatus used in the treatment method according to the present invention, in which 1 is a cylindrical surface treatment tank, inside which guide blades 2 are spirally arranged. It is a provision.

A hole-shaped defect 3 is provided in the center of the guide blade 2,
A processing steam introduction pipe 4 is inserted along the central axis.

Reference numeral 6 indicates a discharge nozzle for discharging heated air containing processing steam 19, which is provided on the introduction pipe 4 at appropriate intervals.

The number is not particularly limited.

Reference numeral 7 denotes a guide outer cylinder of the surface treatment tank 1, into which steam 8 is introduced to maintain the internal temperature of the treatment tank at the treatment temperature.

9 is an introduction pipe for heated air containing water vapor 18, and 10 is an exhaust pipe.

1L12 is a porous portion of the wall of the surface treatment tank 1, which is processed to allow heated air to be introduced and exhausted.

13 is a transmission shaft, which is connected to an electric motor (not shown in the figure).

14 is the bearing, 15 is the support arm of the bearing, 16° 17
are conveyors for transportation.

After cotton-making, the wool-like inorganic fibers 5 loosely deposited on the conveyor 16 are continuously fed into the surface treatment tank 1.

The surface treatment tank 1 is rotated by a transmission shaft 13, and the inorganic fibers 5 are slowly moved within the surface treatment tank 1 by the guide blades 2.

Further, heated air containing water vapor 18 is introduced into the surface treatment tank 1 through the introduction pipe 9, flowed in a countercurrent to the transfer of the inorganic fibers 5, and exhausted through the exhaust pipe 10.

Furthermore, an organic titanium compound T i (0R)4(R-=C4
Heated air containing treated steam 19 of 'Hg, C3H72C2H5] is ejected from the discharge nozzle 6.

The organic titanium compound treatment vapor 19 and the water vapor 18 form a complex amorphous titanium compound film on the surface of the inorganic fiber 5 depending on the ambient temperature, their respective concentrations, and their concentration ratio.

Figure 2 shows the concentration distribution in the surface treatment tank 1 accompanying such treatment, where the water vapor concentration is highest at the introduction position A, and is sequentially consumed until it is the most diluted at the exhaust position B. becomes.

On the other hand, the concentration of the treated steam is uniformly discharged in the surface treatment tank 1, but the surplus steam that is not consumed is pushed away by the heated air containing water vapor in the direction of the inlet of the inorganic fiber 5. The B position tends to be the highest and the A position the lowest.

On the other hand, Figure 3 shows the concentration ratio (H20/T i (0R)4) and the hardness and alkali resistance of the film properties. gradually increases, and as shown in FIG. 3, the properties of the film produced differ depending on the position within the surface treatment tank.

The characteristics of the treatment method of the present invention reside in the above points, and the properties of the film formed on the fiber surface differ in the thickness direction, and in the above example, the part close to the fiber surface has very good alkali resistance. The part near the surface becomes a hard film.

In addition, organic titanium compound T i (QC4 crosspiece) 4, Ti
When performing surface treatment on inorganic fibers using (OCaH7)+ and Ti(OC2H5)4, N2 is generally used as a carrier gas for each compound, and the vapor concentration of the organic titanium compound is 1000 to 2500 p.
pm1 flow rate 50-3oool/min, temperature 200-350℃
, water vapor concentration 1000~5000ppm1 flow rate 50~
3001/min, temperature 200-350℃, processing time 1-5
The surface treatment can be carried out under similar conditions for each compound within a range of 10 minutes.

In the present invention, as described above, inorganic fibers immediately after cotton production are fed into a surface treatment tank, and an organic titanium compound having the general formula T1(OR)4 [R2C4H9, C3H7, C2H5] is prepared. Since the inorganic fibers are continuously brought into contact with the treatment steam and water vapor, the organic titanium compound undergoes a hydrolysis-condensation polymerization reaction to form a protective film of an amorphous titanium compound on the surface of the inorganic fibers. It is possible to obtain high-strength inorganic fibers that maintain initial strength by suppressing mechanical and chemical deterioration of the fibers.

Further, since the gas phase treatment is performed, the treatment vapor and water vapor can smoothly diffuse and permeate into the fine spaces between the fibers, and there is an advantage that a uniform protective coating can be applied to the fiber surface.

Moreover, during this treatment, the present invention creates a gradient in the concentration ratio of water vapor and treatment steam in the direction of transport of the inorganic fibers, so it is possible to create a difference in properties between the inner layer and the surface layer of the film itself. Therefore, by setting the gradient of this concentration ratio variously, there is an advantage that films having various characteristics depending on the application can be formed.

For example, as shown in the illustrated example, when the water vapor flow is made countercurrent, the concentration ratio just before the inorganic fibers are carried out from the surface treatment tank is higher than the above concentration ratio immediately after the inorganic fibers are sent into the surface treatment tank. As mentioned above, in the early stages of film formation, the water vapor concentration is low, resulting in a film with good alkali resistance, and in the later stages of film formation, the water vapor concentration increases and a hard film is formed. An excellent protective film with high mechanical strength and good alkali resistance can be obtained.

Since the thickness of the film increases in proportion to the treatment time, it can be easily adjusted by, for example, adjusting the rotation speed of the surface treatment tank and changing the transport speed of the inorganic fibers.

The present invention will be specifically described below based on examples.

〔Example〕

Sio2: 40% by weight, can: 40% by weight A403
'15 weight arc MgO: A mineral material having a rock wool composition consisting of 5 weight arcs was melted in an electric furnace at 1500°C, and the molten material was made into cotton by the disk method.

The cotton manufacturing disk used had a diameter of 200 mmφ and a rotation speed of 3.
Cotton was made under the conditions of 00Orpm throughput of 0.5t/hour,
The fibers loosely deposited on the conveyor belt at the bottom of the cotton collection box were continuously conveyed in a loose state into a 400 mmφ x 2000 mmL treatment tank and treated under the following conditions.

However, the temperature of the guide outer cylinder was 200° C., and the residence time of the fibers in the processing tank was 110 seconds.

Surface treatment materials and conditions Tetrabutoxy titanium (Ti(OBu)4) Vapor concentration 2000 ppm Carrier gas N2 flow rate 501X min. The fiber diameter of the glass wool was 10 to 15 μφ, and the average film thickness of the amorphous titanium compound on the fiber surface was 180×.

The results of measuring the tensile strength of the glass wool subjected to the above treatment and the untreated glass wool were as follows.

1) Untreated glass wool 85ky/mm11)
Surface-treated glass wool 195 kg/mA Also, the tensile strength after immersion treatment in cement alkali (80°C) for 40 hours was as follows.

1) Untreated glass wool 32kg/mm11)
Surface treated glass wool 177kg/mA In addition, cement alkali is NaOH0.88g/l, KOH3,4
5 g/Cca(on)2o, 48 g/l was used, and the strength measurement conditions were as follows.

Glass wool length 20m7IL Tensile speed 5mm/min Number of samples 40 each In addition, tetrapropoxy titanium (Ti (0C3H7)
4) Tetraethoxytitanium (Ti(OC2N5)4)
) can also be processed under the same conditions as above.

[Brief explanation of drawings]

FIG. 1 is a partially cross-sectional schematic side view of an embodiment of the apparatus used in the present invention, and FIG. Figure 3 is a diagram showing the relationship between the concentration ratio of water vapor and treated steam, hardness, and alkali resistance, in which 1 is a surface treatment tank, 5 is an inorganic fiber, and 18
indicates water vapor, and 19 indicates treated steam.

Claims (1)

[Claims] 1. Immediately after cotton production, the inorganic fiber is sent into a surface treatment tank and the general formula is 'I" r (0R) 4 CR" C4H9t C
3H7, C2H5] and water vapor are brought into continuous contact with the inorganic fibers, and a gradient is created in the concentration ratio of the water vapor and the processing vapor with respect to the direction of transport of the inorganic fibers. A method for reinforcing inorganic fibers.