JPS597657B2 - Inorganic fiber surface treatment method - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention provides an inorganic fiber 1 having a general formula of Ti(O
R) nCl4-n (R-C4H,, C3H7, n=1
- 3) An inorganic fiber surface treatment method characterized in that vapor 2 of an organic halogenated titanium compound represented by formula 2 is sprayed alternately with water vapor 3 to form a film on the surface of the inorganic fiber 1 by a hydrolytic condensation reaction, The purpose is to coat all fibers with a coating of sufficient thickness and uniformity on the fiber surface during the production of inorganic fibers.
An object of the present invention is to provide an inorganic fiber surface treatment method that can obtain inorganic fibers that have a large initial strength protection effect by protecting the inorganic fibers from mechanical and chemical deterioration.

In general, inorganic fibers such as glass wool and rock wool have a very high tensile strength (200 to 300 kg/ma) if no mechanical or chemical surface damage occurs after melt spinning.

In order to avoid this mechanical and chemical surface damage, for example, with respect to long glass fibers, various resin films called sizing agents are uniformly applied by dipping, roll coating, spraying, etc.

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. unable to
Droplets were partially attached.

For this reason, the strength of wool-like glassy staple fibers is significantly reduced by mechanical contact after cotton-making.

In view of the above circumstances, in order to form a uniform protective film on the surface of wool-like glass fibers and maintain initial strength, for example, immediately after cotton-making, a surface treatment agent is sprayed in vapor form on the high-temperature fiber surface. Methods of causing chemical reactions such as thermal decomposition in fibers are being considered, but at present, satisfactory results have not been obtained because the film attached to the fiber surface is not uniform or thick enough. be.

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 can be blown away by high-speed air currents or fire and become fibers.

These fibers are sent into a collection box by the transport air current, collected on a conveyor net, conveyor belt, etc., and transported, and then processed into a board by spraying with resin, etc.
Alternatively, it can be used as a raw material for other secondary products after undergoing processes such as particle removal, defoaming, and granulation.

When examining the fiber strength in the above process, it was as high as 200 to 300 kg/m4 immediately after cotton production, and 1.7 kg/m4 during cotton collection.
0 to 230 kg/m7, and then 40 to 100 kg/m7 after shedding and opening. It was found that the value becomes significantly smaller than L.

Most of these strength deteriorations occur due to mechanical contact between fibers, and therefore, these strength deteriorations can be prevented by forming a protective film on the fiber surface.

In the present invention, during cotton collection, inorganic fibers loosely deposited on a conveyor net (or conveyor belt) are continuously fed as they are into a surface treatment chamber.

The inorganic fibers fed into the chamber are first coated with organic titanium rogenide (Ti(OR) nC 14
n, R-C4 H9, C3H7, n=1-3) The vapor of the compound is sprayed from a nozzle or the like, and the vapor is adsorbed and adhered to the entire surface of the fibers, even in the thickness direction of the fiber strip.

These inorganic fibers move slowly and continuously, and then wet air containing water vapor, nitrogen, etc. are blown from a nozzle or the like.

At this time, for example, Ti(OBu)2C on the surface of the inorganic fiber.
12 easily forms an amorphous titanium compound film through hydrolytic condensation.

The present invention will be explained in detail below based on the accompanying drawings.

In Figure 1, the molten mineral material is dropped from a melting furnace such as an electric furnace or a cupola directly or through a gutter onto a rotating distribution disk that rotates at high speed, and is finely divided (atomized) by the rotating distribution disk. The accelerated melt is supplied to the cotton making disk 4.

Fiber-forming particles are formed on the cotton-making disk 4, and inorganic fibers 1 are formed in the circumferential direction by centrifugal force.

These inorganic fibers 1 are turned 90 degrees by an air ring (carrying gas jet ring) 5 attached to the rear of the cotton making disk 4 and collected in a cotton collection box 6.

Furthermore, since the particles (shots) 7 are scattered in the circumferential direction without being changed in direction by air, they are separated from the inorganic fibers 1.

The bottom of the cotton collection box 6 consists of a mesh conveyor belt 9 supported by roller pieces 8 so as to move in the direction indicated by the arrow.

The inorganic fibers 1 deposited on the conveyor belt 9 are transported into a surface treatment chamber 10.

The surface treatment chamber 10 is made up of several processing steam boxes 11 and steam boxes 12 connected alternately, and at the top of each box there are nozzles 13 for spouting organic halogenated titanium compound vapor 2 and water vapor 3. 14 is installed.

At the bottom of the surface treatment chamber 10, a section of the conveyor belt 90 has a suction box 15 installed with its open side adjacent the underside of the upper belt and connected to any suitable air evacuation device.

In addition, in FIG. 2, after cotton-making, the small inorganic fibers 1 deposited on the conveyor belt 9 with significant strength deterioration are transported by the conveyor belt 9 to the processing steam box 11, where the organic halogenated titanium compound 2 is injected from the nozzle 13.

The inorganic fiber 1 that has sufficiently adsorbed the processing material vapor on the fiber surface is then conveyed to the steam box 12, where it is also passed through the same nozzle 14.
A gas containing water vapor 3 is injected from the tank.

As a result, the organic halogenated titanium compound is easily hydrolyzed and condensed on the fiber surface to form an amorphous titanium compound film.

Furthermore, these fibers are transported to the next processing steam box 11 and subjected to the same treatment as described above, and further transported to the steam box 12 where they are hydrolyzed and condensed, and by repeating these treatments, the film thickness on the fiber surface gradually increases. I will do it.

Organic titanium halide compounds are T I ( ocs H
7) nc i 4n is more Ti(OC4H,)nC14
-N is more easily hydrolyzed than organic
・The optimum water vapor concentration for the vapor 2 of the titanium halogenide compound is different, but for example, the optimum water vapor concentration for the vapor 2 of the organic titanium halide compound is 2000 ppm and the vapor temperature is 20.
Flow rate 50l/dry air etc. as carrier gas at 0℃
When injecting the water vapor 3 from the nozzle 13 at a concentration of 10,000 ppm and a temperature of 200° C., the water vapor 3 is injected from the nozzle 14 at a flow rate of 50 l/min using air or nitrogen as a carrier gas to completely eliminate all organic halogenated titanium compounds. Water vapor is in excess and sufficient hydrolysis and condensation can be carried out.

The gases ejected from the nozzles 13 and 14 form conical jets as shown in FIG. 2, and the intersections with the fibers form circles, with adjacent circles touching each other.

This allows the fibers to be uniformly adsorbed by steam not only in the flow direction of the fibers but also in the thickness direction.

Furthermore, the above-mentioned uniformity can be further improved by using the processing agent as a gas instead of liquid particles.

In the present invention, as mentioned above, the general formula of the inorganic fiber immediately after cotton production is Ti(OR)ncl4, (R=C4
Since the vapor of an organic titanium halogenide compound represented by H, C3H7, n = 1 to 3) is sprayed alternately with water vapor to form a film by a hydrolytic condensation reaction on the surface of the inorganic fiber, it is a spray method. Unlike the spraying of droplets, the vapor phase treatment allows the steam to penetrate into the narrow spaces between the fibers, creating a titanium compound coating on the surface of all fibers, not only long fibers but also short fibers. It is possible to form inorganic fibers with high strength by preventing a large deterioration of the initial strength immediately after cotton making.

In addition, there is a vapor-phase pyrolysis method, which is the same vapor-phase processing method, but the processing time is limited to a short period due to the cooling time of the inorganic fibers immediately after production, but the present invention does not require high temperatures, so the processing time is It is possible to produce a sufficiently long and sufficiently thick film with sufficient reinforcing and protective effect.

Moreover, since the organic titanium compound and water vapor are sprayed alternately, the number of alternating spraying treatments can be easily increased or decreased depending on the degree of damage during treatment of inorganic fibers or the purpose of use. The thickness of the treated film can be adjusted to the optimum thickness.

In addition, in the present invention, when vapor of an organic halogenated titanium compound and water vapor are simultaneously injected, hydrolysis occurs before the vapor reaches the surface of the inorganic fiber, and the resulting white powder loosely adheres to the surface of the inorganic fiber. , it is easily attached and detached and does not form a protective film.

Moreover, even if the vapor of the organic titanium chloride compound and the water vapor are treated separately for a long time, the thickness of the film remains the same, and the film thickness is insufficient, so that the protective effect is also small.

Therefore, a film thickness sufficient to withstand mechanical and chemical damage can be obtained by alternately treating the film with vapor of an organic titanium chloride compound and water vapor several times.

The film on the fibers obtained by this method has a hardness similar to that of a thermoplastic resin film, and does not cause fibers to adhere to each other.

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

Example Si0240% by weight, Ca040% by weight, AI2031
A glass wool material having a glass composition consisting of 5% by weight and 5% by weight of Mg0 was melted in an electric furnace at 1500°C, and the molten material was heated to a cotton manufacturing disk with a diameter of 200φ and a rotation speed of 3000 rpm.
, Cotton was produced under the condition that the processing amount was 0.5 t/hour, and the steam and water vapor of the following treatment materials were sequentially and alternately applied to the fibers loosely deposited on the conveyor net at the bottom of the cotton collection box from separate nozzles, 5 times each. I sprayed it one by one.

Treated material〉 The fiber diameter of the glass wool treated as above is 10~
It was 15μφ.

The fiber surface film thickness was about 5 ooA.

As a result of measuring the expansion strength of these glass wolves, Met.

The tensile strength measurement conditions were as follows.

[Brief explanation of the drawing]

FIG. 1 is a schematic process explanatory diagram of an embodiment of the present invention, and FIG. 2 is a partially omitted perspective view of the same, in which 1 is an inorganic fiber, 2 is an organic titanium rogenide compound, and 3 is a water vapor show.

Claims (1)

[Claims] 1 The general formula T i (
OR ) nC 14-n ( R = C4H9, C3H
7. An inorganic fiber surface treatment method, which comprises spraying vapor of an organic halogenated titanium compound represented by n=1 to 3) alternately with water vapor to form a film on the surface of the inorganic fiber by a hydrolytic condensation reaction.