JPS60112617A - Preparation of modified alkali titanate - Google Patents

Abstract

PURPOSE:To prepare white modified alkali titanate having superior reinforcing effect for plastics, etc. and electric conductivity by calcining by heating alkali titanate at specified temp. in H2 atmosphere. CONSTITUTION:Alkali titanate expressed by the formula: M2O.nTiO2 (M is an alkali metal; n is 1-12) is charged in a closed furnace to be heated at high temp, and the air in the furnace is removed by evacuation or replaced with inert gas. After heating the furnace to 500-1,100 deg.C, gaseous H2 is introduced into the furnace and the charge is calcined for 20-180min to extract oxygen from the crystals of alkali titanate. By this process, modified alkali titanate useful as a reinforcing material for plastics, material for conductive paper and conductive ink, etc. is obtd. preserving white or slightly blue color tone without impairing heat resistance, reinforcing effect, and surface smoothening effect, etc. of alkali titanate.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a modified titanate alkali, and an object thereof is to provide a modified alkali titanate that has an excellent reinforcing effect on plastics, etc., and has excellent electrical conductivity. It is in.

With the development of science and technology and the diversification of needs, the development of high-performance, multifunctional materials has been actively conducted, and even in the plastics industry, various research efforts have been made on the development of conductive polymer materials. For example carbon particles or fibers or copper,
Polymer materials using metal powders such as silver and gold as conductive fillers have been proposed. However, carposi particles, carbon fibers, metal powders such as copper, silver, and gold are all black or have a color unique to the metal, and these conductive fillers are non-reinforcing fillers except for carbon fibers. It is a drug. Although carbon fiber is a reinforcing conductive filler, it is difficult to make the fiber length uniform and the aspect ratio becomes uneven, resulting in poor moldability and poor surface smoothness of molded products. Poor polishing properties.

In view of the above-mentioned circumstances, the inventors of the present invention have developed a conductive composition, a titanate having a metal coating, a method for producing the same, a method for producing a reduced alkali titanate, etc. using potassium titanate, and a filling material with excellent heat resistance and reinforcing properties. Although agents have been developed and applications are being filed, all of these are colored, making it difficult to apply them to applications where a white or pale color is desired. In view of the current situation, the present inventor has arrived at the present invention as a result of intensive research to develop a new material that does not have the above-mentioned drawbacks.

That is, the present invention is based on the general formula % formula % (1) [In the formula, M represents an alkali metal, and n represents an integer of 1 to 12.

] In a hydrogen atmosphere, an alkali titanate represented by
After heating and baking at 1100° C., the general formula % formula %: [In the formula, X represents a positive real number of 2 or less. M and n are the same as above. ] This relates to a method for producing a modified alkali titanate, which is characterized by obtaining a modified alkana titanate represented by the following.

The modified alkali titanate according to the present invention has a white color without losing any of the physical properties of the alkali titanate before modification, especially heat resistance, reinforcing properties when used as a composite material, and surface smoothness. Or, it maintains a very slight blue color tone and is used as a composite material without discoloring to black, black-purple, or black-brown like conventional reduced alkali titanate or hydrogenated titanium thorium. By using white color or a coloring agent in combination, it is possible to adjust the desired color tone to prevent static electricity, remove static electricity,
The suitability of conductive materials has been greatly improved compared to conventional reduced alkali titanates, etc., and in particular, white conductive materials such as sheets, papers, fabrics, and films have improved reinforcing properties and surface smoothness. It has high industrial applicability as a processing agent that can add conductivity without loss of conductivity. The electrically conductive alkali titanate of the present invention that does not impair whiteness can be widely used in various applications such as reinforcing materials for plastics, fillers for electrically conductive papers, and electrically conductive inserts.

In the present invention, the alkali titanate represented by the above general formula (1) is a known compound, which is conventionally produced by a hydrothermal synthesis method, a flux method, and a calcination method. . In the present invention, any known alkali titanate including the above general formula (INK) can be used, such as titanate:/WI sodium, potassium titanate,
Examples include lithium titanate. Particularly in the present invention, potassium titanate, represented by the formula 20.6TiO2, is advantageous in that it has excellent fire resistance, heat insulation, and mechanical strength, and also has excellent surface smoothness when used as a filler. Titanium concentrated alkali is generally in the form of powder or fibrous microcrystals, but any of these forms can be used in the present invention. The alkali titanate used in the present invention is preferably a fibrous material in order to meet the purpose of the present invention, and generally fibrous potassium titanate is practically preferred. A reinforcing filler having an aspect ratio of 5 μm or more and an aspect ratio of 20 or more, especially 100 or more is suitable as a reinforcing filler.

The modified alkali titanate of the present invention is prepared by adding the above-mentioned alkali titanate to 500 to 500 tons in a hydrogen atmosphere.

It can be manufactured by heating and firing with C. As will be described in detail later in Examples, for example, after putting an alkali titanate into a closed high-temperature heating furnace, the air in the system is removed under reduced pressure, or nitrogen gas is introduced into the furnace and the air is first replaced with nitrogen. Next, after the temperature is raised to 500-1100° C., hydrogen gas is introduced into the furnace to cause a reaction, and it is preferable to remove oxygen from the alkali titanate crystals and impart electrical conductivity. As the hydrogen residue used here, commercially available industrial hydrogen gas is sufficient and no special purification is required.

The heating and firing temperature of the present invention is usually 500 to 1100.
C., preferably in the range of 600 to 900, and the heating and baking time is usually in the range of 20 to 180 minutes, preferably 30 to 90 minutes. If the heating and firing temperature is lower than the above temperature, the desired modified alkali titanate cannot be obtained, whereas if the heating and firing temperature is too high, the temperature will exceed the melting point of the alkali titanate, and the alkali titanate will melt. It is not desirable to disassemble it. The heating and firing time is preferably within the above range in order to impart electrical conductivity without impairing the white color tone of the alkali titanate. If the heating and firing time is shorter than the above, the desired modified alkali titanate cannot be obtained, and if the heating and firing time is too long, the product gradually becomes colored and loses its whiteness, which is not preferable.

Examples are given below to make it even clearer.

Example ! Potassium titanate (manufactured by Otsuka Chemical Co., Ltd., Taste tD) 5
F was placed in a 30-proof platinum container, transferred to a siliconite tubular electric furnace, and nitrogen gas was flowed at a flow rate of 150 m1/min at room temperature for about 1 hour to adjust the atmosphere, and then heated to 500°C under nitrogen introduction.
The temperature was raised to .

Next, the introduced gas was changed to hydrogen gas, hydrogen scum was introduced at a flow rate of 150 txl/min, and the temperature was kept at 900°C for 1 hour.The electric furnace was then turned off, and the hydrogen was left to flow/cool down for 200 txl/min.
After changing the introduced gas to nitrogen gas at °C, it was taken out of the furnace.

By reducing the potassium titanate using the method described above, a white reduced potassium titanate with a slight blue tinge was obtained.

90 parts of reduced titanic acid obtained above, 5 parts of liquid parasitic acid
After mixing 10 parts well in a mortar, press molding at 50 #/d for 10 minutes in a mold with an inner diameter of 10 fins and a length of 20 mm. After applying silver paste on both sides of the molded product, use a digital multimeter (Takeda Riken). When the conductivity was measured using a
XlO'Ω is υ, and the volume resistivity using the following formula is 3.77
It was X10'Ω1.

Distance between electrodes (1) Example 2 In Example 1, the introduced waste was changed to hydrogen gas, and 150g of hydrogen gas was used. The same method as in Example 1 was carried out, except that the mixture was introduced at 850° C./min for 1.5 hours, and a white reduced potassium titanate with a slight blue tinge was obtained.

The volume resistivity was measured using the same method as in Example 1, and the measured resistance of the molded product was 1.79XIO6Ω.
The volume resistivity was 7.03×10′Ω.・(Hereafter
Up)

Claims (1)

[Claims] ■ General formula % formula % [In the formula, M is an alkali metal and n is an integer from 1 to I2. ] In a hydrogen atmosphere, an alkali titanate represented by
After heating and baking at 1100°C, the general formula % is obtained. [In the formula, X represents a positive real number of 2 or less. Δf and n are the same as above. ] A method for producing a modified alkali titanate, which comprises obtaining a modified alkali titanate represented by: (2) The method according to claim 1, wherein the alkali titanate is fibrous. (2) The method according to claim 2, wherein the fibrous alkali titanate has a fiber length of 5 μm or more and an aspect ratio of 20 or more.