JPS6024061B2 - Surface treatment method for inorganic fibers - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for surface treatment of inorganic fibers, and its purpose is to efficiently form a mixed coating of a titanium compound and a zircon compound with high adhesion and hardness on the surface of inorganic fibers. To provide a method for surface treatment of inorganic fibers, which can be formed into a rough texture and which can protect the inorganic fibers from mechanical and chemical deterioration, thereby obtaining a weave with a large protective effect on initial strength.

After melt spinning, glass fibers have a very high tensile strength (200 to 300
k9/masu).

In order to avoid this mechanical and chemical surface damage, various resin films called sizing agents are applied to the fiber surface of long glass fibers by dipping, roll coating, spraying, etc., for example. However, since glass wool, rock wool, etc. are produced in large quantities by the disk method or spraying method, surface treatment during cotton production is difficult. Methods of causing chemical reactions such as thermal decomposition on the fiber surface are being considered, but in addition to insufficient uniformity and thickness of the film attached to the fiber surface, processing efficiency is also low. The current situation is that no satisfactory results have been obtained. In general, inorganic fibers are produced by introducing mineral raw materials melted at a high temperature of 1,300 to 1,500 degrees Celsius onto a disk that rotates at high speed, and forming fibers from around the disk due to the centrifugal force, or by blowing them away with high-speed airflow or flame ejected from a nozzle. It becomes fibrous. These fibers are sent into a collection box by the transport air current, collected on a compare net, conveyed, and then processed into a board by spraying with resin, etc., or subjected to particle removal, defiberization, and granulation processes. After that, it is used as a raw material for other secondary products.

When we examine the fiber strength in the above process, it is as high as 200-300 kg/fence immediately after cotton milling, and 170-300 kg/fence during cotton collection.
It becomes 230kg/co, and after further shedding and opening, it becomes 40~10
It was found that it was significantly inferior to 0k9/masu. This strength reduction is mostly caused by mechanical contact between fibers,
Therefore, this strength deterioration can be prevented by forming a protective film on the fiber surface. The present invention is characterized in that a film containing an organic titanium compound as a main component from the viewpoint of film formation speed and an organic zircon compound for imparting alkali resistance is formed on the fiber surface.

First, in carrying out the method of the present invention, a solution of tetrabutoxy or tetrapropoxyzircon [Zr (OR
) 4, R = C3 days 7, C4 days 9] is atomized in the required amount, sprayed (dispersed), and placed in the surface treatment tank as it is (without applying large force). A heater or a heating steam pipe is attached to the surface treatment tank so that the inside can be heated. Steam and water vapor of organic titanium or organic halogenated titanium compound [Ti(OR)nC141n, R=C3day7,C4day9,n=1-4] are introduced into the wool put into the heated treatment tank. Then, the tetrabutoxy or tetrabropoxy zircon previously sprayed in liquid form is vaporized in the treatment tank, and a mixed film of hydrolyzed and condensed amorphous titanium and amorphous zircon compounds is formed on the entire surface of the wool. Here, the organic titanium or organic halogenated titanium compound and the vapor of tetrabutoxy or tetrapropoxy zircone are extremely unstable in the presence of moisture and easily cause a hydrolysis reaction. Therefore, excessive contact between processing agent vapor and water vapor should be avoided.
In particular, tetrabutoxy or tetrapropoxyzircon is extremely unstable in moisture, so it is difficult to transport it through piping in a vapor state. Therefore, it is necessary to atomize the necessary amount of liquid and spray it on collected wool in advance. It has been found that it is possible to vaporize the organic titanium or organic titanium halide by heating it in a bath and utilizing the heat retained in the vapor of the organic titanium or organic halogenated titanium compound. That is, in the method of the present invention, wool coated with the necessary amount of tetraptoxy or tetrapropoxy zircon by spraying is placed in a treatment tank heated to a treatment temperature (usually 100 to 350 oo), and then an initial stage is heated to 100 to 350 q0 in the same manner. Steam of an organic titanium or organic titanium halide compound having a concentration of 500 to 400 and humidity-controlled air of 100 to 350 qo and having a water vapor concentration of 500 to 8000 are blown into the processing tank. In this case, if the water vapor concentration is too low, the processing speed will be slow and efficiency will be low, while if the water vapor concentration is too high, the stability of the processing agent will deteriorate.
Efficiency decreases. The fine-grained zircon compound treatment agent heated in the treatment tank immediately vaporizes and becomes vapor, and while mixing with the titanium compound vapor and water vapor, it diffuses into the narrow gaps between the wool and coats the surface of all the fibers with titanium. Forms a mixed film of compounds and zircon compounds. In addition, most of the processing agent is effectively consumed while flowing through narrow wool spaces, and a small amount of the processing agent is discarded undecomposed. In the present invention, as mentioned above, the general formula is Zr(OR)4 [where R=C3
7, C4, 9] is used as an organic titanium compound with the general formula Ti(OR) 141n [where R=C3
Day 7, C4 is treated with compounds represented by n = 1 to 4, respectively, so the organic zirconium compound gives greater alkali resistance, and the organic titanium compound gives greater hardness. High strength fibers with little alkali deterioration can be obtained. In addition, during the treatment, first, atomized droplets of an organic zirconium compound are sprinkled, and then 1
Since the vapor of a high-temperature organic titanium compound heated to 00 to 350 oo is brought into contact with water vapor, the organic zirconium compound, which is unstable in water, is sufficiently coated on the surface of the inorganic fiber in a stable state without contacting with water. can be brought into contact with
Moreover, the organic zirconium compound after contact reacts reliably with the heat of the steam of the inorganic titanium compound treated later and the water vapor, and a mixed film with the reactant of the organic titanium compound can be stably applied over the entire surface of the fiber. I can do it. Furthermore, since it is a gas phase treatment, it has the advantage of being able to sufficiently diffuse and permeate into minute gaps, allowing a protective film to be uniformly and efficiently applied over the entire fiber surface. The present invention will be specifically described below based on examples.

Example A rock wool composition consisting of Si024 t%, Ca04 x%, mountain 20315M%, and Mg05wt% was used as an example mineral material. This material was melted in a 1500qo electric furnace, and the molten material was manufactured by the disk method. It was cotton.

The diameter of the cotton milling disk used was 20 mm, and the number of revolutions was 300.
Q blood, processing amount is 0.5 t/hour. Cotton was produced under the above conditions, and the fibers loosely deposited on the comparer net at the bottom of the cotton collection box were loosely put into a treatment tank and treated under the following conditions. 1 Treatment agent...tetrabutoxytitanium and isopropoxyzircon 2 Dimensions of treatment tank...
...30 mn L x 40 m pig W x 30 mw 3 days Temperature inside the treatment tank...250o04 Initial concentration of treatment agent
...Tetrapoxytitanium 150Q bait (steam temperature; 250pm), isopropoxyzircon 1300 blood 5 Water vapor concentration in humidified air...200Q side (air temperature; 250pm) 6 Treatment Time: The fiber obtained after 2 minutes has a fiber diameter of 1.
The average thickness of the produced film was about 190A.

When tensile strength was measured for the samples treated in this manner and those not treated, the results shown in the table below were obtained.

[Tensile strength measurement results] However, the tensile strength measurement conditions were as follows.

1 Sample wool length: 1 yen 2 Tensile speed: 5 sides/min 3 Alkaline solution...0.8 chicks r-NaOH/1,
3.458-K〇H/1,0.4&y-Ca(〇H)2
/I PH=12.6 4 Number of samples 40 each

Claims (1)

[Claims] 1 The general formula of inorganic fiber immediately after cotton production is Zr(OR)_4
After spraying atomized droplets of an organic zirconium compound represented by the formula {R=C_3H_7, C_4H_9}, 1
The general formula heated to 00-350℃ is Ti(OR)nCl
_4-n {in the formula R=C_3H_7, C_4H_9, n=
1 to 4} A method for surface treatment of inorganic fibers, the method comprising bringing the vapor of an organic titanium compound represented by 1 to 4} into contact with water vapor.