JPS63112724A - Method and apparatus for production of carbonized fiber cloth - Google Patents

Abstract

PURPOSE:To obtain the titled product having excellent heat resistance, thermal shock resistance, chemical resistance, electric conductivity as well as mechanical strength, etc., by immersing a fiber cloth for a carbonization processing to a mixed raw material solution having a specific composition, drying and heating and calcining the treated cloth under high pressure at high temperature. CONSTITUTION:An aqueous solution of (A) thermosetting urea resin (melamine co-condensing type) and (B) zinc chloride or chloride of other metal are blend with (C) diammonium phosphate or a mixture of boric acid and borax as a flameproofing agent and (D) hard carbon powder to provide a solvent solution of mixed raw materials. Then fiber cloth of a raw material for carbonization processing is uniformly sufficiently immersed to said solution. The immersed fiber cloth of raw material is further dried and then heated and calcined under high pressure at high temperature to provide the aimed product.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention is characterized by the fact that conventionally commercially available carbon cloths and cloths made from carbon fibers have no loss of their properties, and have good heat resistance and high thermal shock resistance. Chemical resistant
This invention relates to the production of fiber cloth that has electrical conductivity over a wide range from semiconductivity to metal-like regions, a small neutron absorption cross section, excellent surface activity, and mechanical properties. A mixed solution of methanol alcohol and volatile glue liquid using formaldehyde, zinc chloride, diammonium phosphate, or (borax-borax mixture) and hard carbon powder, which are the main components of the fiber cloth of this invention, as mixed raw materials. Mix and stir thoroughly to make a sticky liquid material. The composition of these raw materials is generally as follows.

Formaldevi? Total amount nt, 2o in ooog
y methanol alcohol // 1 in 1,0OOf
809 volatile glue substance 〃600 in 1,000f
Hereinafter, these mixed raw material solvent solutions will be referred to as (A).

On the other hand, in order to carbonize the fiber cloth, a mixture of volatile glue and diammonium phosphate is prepared, thoroughly mixed and dissolved in methanol alcohol, and the mixture is placed in the raw material solution and soaked evenly and thoroughly. Then let it dry. The composition of these raw materials is generally as follows.

Volatile glue substance Total weight 1.000 f6209
Diammonium phosphate N 1,000I! 1st year of junior high school
809 Methanol Alcohol /1. 1,0OOof
The medium weight is 200g.

Hereinafter, these mixed raw material solvent solutions will be referred to as (B).

After drying the fiber cloth to be carbonized, it is further put into the raw material and soaked in it well, dried again, and fired at high heat under high pressure to form carbonized fibers. Conventionally, fiber paper or cloth is coated (impregnated) with a coating liquid consisting of a solvent solution of thermoplastic synthetic resin, its copolymer, or thermosetting synthetic resin, and carbon, black, etc. There are various known methods for imparting specific physical properties by heating or heating and pressing.In other words, thermoplastic resins or copolymers thereof are used.Furthermore, thermosetting resins are known. There are those in which a fiber cloth is impregnated with a solvent solution of a thermosetting resin, and those in which a fiber cloth is placed in a solvent solution of a thermosetting resin and cured.

However, although conventionally known products of this kind can be provided with certain desired specific physical properties, they do not have excellent electrical conductivity and mechanical strength as intended by the present invention.
It cannot be said that it has weather resistance and breathability while also having flammability, water resistance, heat resistance, flame resistance, etc., and for this reason, it cannot be said that it has weather resistance and breathability. Including wraps, neck wraps, supports, interior materials for pond construction, such as adhesion to ceilings, walls, wainscoting, floorboards, or underlaying, exterior materials, etc. As a radio wave shielding material, it has not been suitable for so-called multi-purpose use, where it can be applied to the inside wall of a broadcasting room in a broadcasting station, a radio room of a ship, or a cockpit of an aircraft, and exhibit the above characteristics at the same time. Therefore, from this point of view, in order to satisfy some of the above characteristics at the same time, some kind of secondary countermeasure treatment corresponding to the purpose of use is required, which causes many technical problems from the manufacturing perspective and costs. There were also problems from the above.The present invention solves the above problems by selecting the two types of mixed solvent solution raw materials selected as a result of various experimental studies, and by combining them. Due to its characteristics, the advantages and disadvantages of carbon should be considered to complement or aggravate each other, and it also exhibits the unique electrical conductivity of carbon. When we examined the physical properties of carbonized fiber cloth obtained by impregnating it and firing it under high pressure and high heat, we found that it had almost all of the desired electrical conductivity, mechanical strength, and other properties depending on the intended use. The present invention was completed by successfully solving the defects of conventional products at once.The first feature of the present invention is that the fiber cloth can be carbonized without losing its characteristic properties. It has excellent surface activity and air permeability, and it is easy to make from thin carbon fiber cloth to thick carbon fiber cloth, and if necessary, colored carbon fiber cloth can also be produced at the same time as carbonization.The purpose of the present invention is to Excellent conductivity and mechanical strength (compressive strength, tensile strength), flexibility,
An object of the present invention is to provide at low cost a carbonized fiber cloth suitable for multiple uses, such as having good weather resistance, excellent air permeability, and excellent surface activity, as well as water resistance and heat resistance, and to provide the general public with a method for producing the same. Become. The powder used in the present invention has a particle size of 100 to 200 microns obtained by pulverizing each powder separately by a conventional method (using a roll mill or a ball mill). The hard carbon powder has a particle size of 1
A powder having a particle diameter of 100 to 120 microns is used by heating and firing a powder of 20 to 250 microns in an inert gas atmosphere in an electric firing furnace. Although the mixing ratio of the mixed solvent solution cannot be fixed depending on the use and purpose of the product, the above-mentioned combination seems to be generally good. If necessary, a hexametaphosphate as a dispersant and an alkylsulfonate as a penetrant are mixed into the mixed solvent solution. Stearate or silicone liquid may also be added to the release agent. There is a difference in atmospheric temperature between summer and winter, and ammonium chloride is used to adjust this.

On the other hand, the fabric used as the carbonized fiber cloth is preferably a cotton cloth or a mixed woven cloth woven with natural fibers and synthetic fibers, and the coarseness and density of the weave ρ does not matter. For example, both plain weave and twill weave can be used for hot plating, ranging from rope-like weaves to close-woven, solid-weave-like weaves. But preferably
It is preferable that the material is not a single-woven material, but has a relatively short impregnating time with the raw material solvent solution and a material that evaporates quickly. These fiber cloths are impregnated with the above-mentioned raw material solvent solution (normal dipping method). Now, how to make a carbonized fiber cloth according to the present invention and its manufacturing method will be explained step by step with reference to the drawings. In Figures 1 and 2, it is soaked into the fiber cloth. This shows the method of mixing raw material solvent solutions.First, as shown in Figure 1, (1) the glue substance (2) is dissolved in methanol alcohol, and then (3)
), the volatile substance liquid of (4) was mixed well, and a mixture of the carbon powder bed of (5) and the zinc chloride of (6) was mixed on the other hand. Now, make the mixed raw material solvent solution <A>.

On the other hand, the mixed raw material solvent solution in Figure 2 is prepared by dissolving the glue material (8) in the methanol alcohol solution (7), and then mixing the volatile substance liquid (9) and diammonium phosphate (10) (stirring). Then, prepare the second mixed raw material solvent solution (B) as described above.The raw material solvent solution (A) is also
B> The mixing amount is also prepared depending on the use of the carbonized fiber cloth product. Figure 3 shows the roll-wound raw material fiber cloth (11) to be carbonized (12) heated to 30 degrees C in the presence of the raw material solvent solution (B) (rotated in the tank 13). The roll (14) (which may be plural) is continuously impregnated with the solvent solution of the raw material, and the excess solvent solution is squeezed off through the ironing roll (15).In this case, impregnation of the fiber cloth Needless to say, the viscosity of the solvent solution depends on the viscosity of the solvent solution and the length of the impregnation time.In the present invention, the viscosity of the solvent solution is CD, 400.
A short impregnation time (1-2 minutes) at 50°C is sufficient. Next, the obtained impregnated cloth is heated in the heating machine (16) (in a constant temperature oven at 060 degrees Celsius) to evaporate the volatile content and moisture in the solvent solution, and then the raw material solvent solution (19) is heated.
It is further sent to the solvent solution bath of (17)' which is heated to 45 degrees C in the presence of
) is continuously introduced into the drying oven (21) (constant temperature of 080 degrees) after thoroughly impregnating the solvent solution (19) with ) to evaporate the volatile content and moisture in the solvent solution, and dry it well.Then it is shaped in the second hot roller press (22), and then the second hot roller press in (23). By conducting, the carbonized fiber cloth is heated and fired under pressure to obtain a long carbonized fiber cloth having a smooth surface.

The ambient temperature of the secondary hot roller press (23) is constantly exposed to high temperatures. Thus (24
) is produced as a carbonized fiber cloth.The two pieces of cloth are rolled up into wine rolls or cut into flat sheets. The thickness of the sheet obtained above can be varied from a thin film-like sheet to a sheet by appropriately adjusting the amount of impregnated solvent solution, the roller pressure during firing, etc. within the range of the above conditions, taking into account the thickness of the fiber cloth. Even thick ones can be obtained. In the above, the purpose of sequentially conducting the fiber cloth impregnated with the solvent solution to the first and second niblets is to accelerate the firing in advance in the first press and at the same time obtain a smooth surface after firing. Pressure temperature and time depend on product usage and
Although it cannot be fixed depending on the purpose and the amount of solvent solution impregnated into the fiber cloth, if the impregnated amount is 7ooy7rrt and the thickness of the carbonized fiber cloth after the first nibrush is desired to be set to 05 to 0, am/m, the first Roller pressure 50-60kg/in one press
The pressure time at α is 1 minute to promote the first firing. The conditions for the first press are as follows:
The roller pressure is 70 to 150 kg/ci, and the pressing time is 1 minute to complete firing and obtain a carbonized fiber cloth.

The heating temperature for both the first press and the nib press is determined by the pressurization time and degree of pressurization. That is, the roll pressure, temperature and time are interrelated within the ranges mentioned above, and if any of them deviates from the above ranges, not only will it not be possible to obtain a product of the desired quality, but it will also not be possible to provide the product with desirable substances. do not have. Comparing the characteristics of the carbonized fiber cloth thus formed into a molded article with conventional products, it was found that conventionally commercially available carbonized carbon fibers were extremely brittle and easily torn due to the nature of their processing, or were difficult to solidify. The closer it is, the harder it is. The carbonized fiber cloth produced by the method of the present invention is strong, flame resistant, easy to cut without any carbon powder falling off after molding, and has good adhesive properties and can be attached to various objects. . Due to its molding properties, it can be easily attached to uneven objects. It has many uses, and when used in buildings, it can be used as wall lining, under tatami floors, on ceiling panels, for rolling down, and for embedding carbon in the land of buildings. Another soil improvement item will be buried in the soil. Since it electrically blocks radio waves, it can be used as a radio wave blocking material on the inner walls of broadcasting stations, radio rooms of ships, etc.

It can also be used inside household utensils, beds, and mats. Best of all, the clothes and underwear that we wear on a daily basis, or the items mentioned above (loin wraps, body wraps, arm wraps, neck wraps, headbands, eye patches, shoe insoles, etc.) that are worn on a living body. It has many uses, such as in support supports, health equipment, and medical equipment.

[Brief explanation of the drawing]

Figures 1 and 2 are block diagrams showing an example of the preparation process of the raw material solvent solution required for the production of the present invention, and Figure 3 is a schematic explanatory diagram showing an example of the production process of the present invention. . 11...Raw fiber cloth 12...Raw material solvent solution (B) 13...Solvent solution tank (A) 14...Roller 15...・Stretching roller 16...Heating machine I7...Solvent solution tank (B) 18...Roller 19...Raw material solvent solution (A) "20...・・・・Stretching roller 21 ・・・Drying oven 22 ・・・Next hot, roller press 23 ・・・
...Secondary hot roller press 24...Carbonized fiber cloth (final product) Fig. 1 Fig. 2

Claims (1)

[Claims] A thermosetting urea resin (melamine cocondensation type) and an aqueous solution of zinc chloride or other metal chloride are mixed with diammonium phosphate, a boric acid-borax mixture, and hard carbon powder as flame retardants. A solution is prepared, the raw material fiber cloth to be carbonized is immersed evenly and well, and then dried and fired at high temperature under high pressure to produce a carbonized fiber cloth.