KR101058379B1 - A method for preparing flake-type titanic acid whiskers and flake-type titanic acid whiskers prepared by the same - Google Patents

A method for preparing flake-type titanic acid whiskers and flake-type titanic acid whiskers prepared by the same Download PDF

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KR101058379B1
KR101058379B1 KR1020100066816A KR20100066816A KR101058379B1 KR 101058379 B1 KR101058379 B1 KR 101058379B1 KR 1020100066816 A KR1020100066816 A KR 1020100066816A KR 20100066816 A KR20100066816 A KR 20100066816A KR 101058379 B1 KR101058379 B1 KR 101058379B1
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titanic acid
whisker
titanate
present
flake
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KR1020100066816A
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Korean (ko)
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김승진
박응균
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동해케미칼공업주식회사
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J6/00Heat treatments such as Calcining; Fusing ; Pyrolysis
    • B01J6/001Calcining
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/003Titanates
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16DCOUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D69/00Friction linings; Attachment thereof; Selection of coacting friction substances or surfaces
    • F16D69/02Composition of linings ; Methods of manufacturing
    • F16D69/027Compositions based on metals or inorganic oxides

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • Thermal Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

Provided is a method for preparing flaky titanic acid whiskers and a flaky titanic acid whisker produced thereby.
Method for producing flaky titanic acid whisker according to the present invention comprises the steps of mixing a titanium compound, potassium carbonate and magnesium oxide; Calcining the mixture to 900 to 1100 ° C .; And crushing the calcined mixture. The method for preparing flaky titanic whiskers according to the present invention does not use solvents or strong bases. By using no solvents, the manufacturing cost is lowered, and the manufacturing process is simplified, and the economic efficiency is improved.

Description

Method for preparing flake-type titanic acid whiskers and flake-type titanic acid whiskers prepared by the same}

The present invention relates to a method for producing flaky titanic acid whiskers and to a flaky titanic acid whisker produced thereby, more specifically, it does not use solvents or strong bases, thereby reducing corrosion on equipment and reducing manufacturing costs by not using coarse solvents. The present invention relates to a method for preparing a flaky titanic whisker which has been lowered and has improved economic efficiency by simplifying the manufacturing process, and a titanic acid whisker produced thereby.

Whisker titanates have excellent mechanical performance due to various physicochemical performances due to the unique tunnel structure of the material. For example, due to high infrared reflectance, low thermal conductivity, high abrasion resistance, electrical insulation and dielectric constant, and high chemical stability, the application range is wide, especially in the automotive industry. In particular, potassium magnesium titanate containing potassium and magnesium as a flaky whisker is used as a brake pad of a luxury car as a friction material, and the expected demand for this brake pad in 2010 is about 2700 × 10 4 . This corresponds to 1280 tonnes of potassium magnesium titanate. In addition, applications in thermal insulation, heat / insulation materials and building materials are expected to exceed approximately 10,000 tonnes.

In addition, thermoplastics and thermoplastic composites reinforced with potassium magnesium titanate are ideal materials for automobile manufacturing and various precision instruments. According to statistics, plastic demand in China's auto industry is about 93.54 × 10 4 tons in 2010. In addition, other performance characteristics of potassium magnesium titanate whiskers are constantly being developed and used in the fields of paint, military, chemical industry, and paper.

However, a high temperature and basic environment is required in the synthesis process, and a high production cost is required because the use of a coarse solvent requires a large amount of equipment, and a subsequent treatment such as brine washing is required. Therefore, application of potassium magnesium titanate at home and abroad is required. This is limited.

The production method of such whisker titanate includes a calcination method, an improved calcination method (KDC method, a rapid cooling calcining method, a slow cooling calcining method), a hydrothermal method, a melting method, a coarse solvent method, and a crushing method. Among them, the calcination method and the improved calcination method are used as the main production method of the titanic acid whisker because the manufacturing process is simple and mass production is possible, and more than half of the titanic acid whiskers are manufactured by the above method.

The calcination method based titanic acid whisker production according to the prior art is generally disclosed as a process of mixing the potassium source compound and the titanium compound in a constant molar ratio. That is, according to the conventional method, potassium magnesium titanate, a whisker titanate, is made of TiO 2 , a titanate, and K 2 CO 3 (potassium carbonate), which is a potassium source, and an appropriate amount of auxiliary components (e.g., co-solvent) is added, and then, at high temperature. It is produced by calcination and complex processing. For example, Korean Patent No. 10-0732278 (hereinafter referred to as "the prior art") of Otsuka Chemical Co., Ltd. is fixed after mixing 294 g of titanium dioxide with 128 g of anhydrous potassium carbonate, 200 g of KCl, 56 g of magnesium hydroxide, and 40 mg of water. After pressing into a shape, it is calcined at 1050 ° C. for 1 hour, pulverized, washed with an acid of a certain pH, dried and calcined at 600 ° C. for 12 hours. However, such a prior art process is complicated, long cycle, and also used a large amount of co-solvent KCl and strong basic magnesium hydroxide during the synthesis process, causing the corrosion of the equipment at high temperature conditions. Accordingly, there is a need for development of a method for producing a whisker titanate in a more economical manner.

It is therefore an object of the present invention to provide a method for producing a whisker in the form of a plate which is capable of producing potassium magnesium titanate whisker in a short cycle in a more economical manner.

Another problem to be solved by the present invention is to provide a titanic acid whisker in the form of pieces prepared by the above method.

In order to solve the above problems, the present invention provides a flaky whisker production method, the method comprising the steps of mixing a titanium compound, potassium carbonate and magnesium oxide; Calcining the mixture to 900 to 1100 ° C .; And crushing the calcined mixture to provide a method for preparing flaky titanic acid whiskers.

In one embodiment of the present invention further comprises the step of forming the mixed mixture in a predetermined form between the mixing step and the calcination step, the calcination step is a microwave heating method is used. In addition, the titanium compound is rutile titanium dioxide, fusiform or brookite titanium dioxide, preferably rutile titanium dioxide.

The titanium compound, potassium carbonate and magnesium oxide are mixed in a mass ratio of 40:20:10 to 20, and more preferably the titanium compound, potassium carbonate and magnesium oxide are mixed in a mass ratio of 40:20:15. In addition, the mass ratio of the mixed raw materials can be adjusted within the range of ± 10% by weight, the calcination step is carried out for 0.2 to 3 hours.

The present invention also provides a flaky titanic acid whisker produced by the above-described method, wherein the whisker titanate is potassium magnesium titanate, and the whisker titanate is rutile titanium dioxide (China Gansu or Jinan Heungsan), potassium carbonate And calcined from a mixture of magnesium oxide.

According to the method for producing a whisker titanate according to the present invention, since the solvent and the strong base are not used, the corrosion of the equipment can be reduced, and the manufacturing cost is reduced by not using the co-solvent, and the economic efficiency is improved by simplifying the manufacturing process. In addition, the use of microwave, a non-contact heating method can solve the problem of corrosion, replacement of the heating equipment.

1 is an SEM image of flaky potassium titanate prepared according to an embodiment of the present invention.
FIG. 2 is an SEM image of flaky potassium magnesium titanate prepared according to another embodiment of the present invention. FIG.

The present invention is to synthesize a titanate whisker as a new synthetic production technology in order to solve the problems of the prior art. In the present specification, potassium titanate containing potassium and magnesium is used as the whisker titanate, but the scope of the present invention is not limited thereto, and any new metal may be contained in the whisker titanate, which is also described below. As long as the production method according to the present invention is followed, it is within the scope of the present invention.

Since the method for producing whisker titanate according to the present invention does not use coarse solvents or strong bases during the synthesis process, it is possible to reduce corrosion on equipment and at the same time lower raw material costs (coating solvents), and the manufacturing process is simplified compared to the prior art. In addition, the production cost of the titanic acid whisker was lowered by activating / accelerating the synthesis reaction by a micro heating or a heating calcination process performed under micro assistance.

In one embodiment of the present technology, a magnesium titanate whisker was prepared by the following method.

First, a titanium compound (rutile titanium dioxide), potassium carbonate, and magnesium oxide are mixed as raw materials, and the mixture is calcined at high temperature to primarily prepare flaky magnesium titanate. That is, the present invention uses magnesium oxide (eg, industrially active magnesium oxide (magnesium oxide)) as a magnesium source, and not magnesium hydroxide, and in one embodiment of the present invention, the calcination process is performed by micro heating alone or This was used as a supplemental way.

Specific synthesis process of potassium magnesium titanate according to an embodiment of the present invention is as follows.

First, titanium dioxide (TiO 2 ), potassium carbonate and magnesium oxide are sufficiently mixed in a mass ratio of 40: 20: 10 to 20, and water is appropriately added to the mixing process to form the mixture. The mixing may be dry mixing, wet mixing, or dry mixing after wet mixing, and the molding is pressed into an arbitrary shape at an appropriate pressure. If the amount of water added during mixing is large, the raw material may be molded as it is without pressure.

In the present invention, the ratio of 40:20:15 is shown as a mass ratio of the three raw materials, which are particularly suitable for the synthesis of flaky potassium magnesium titanate. When the content of magnesium oxide decreases, the content of rod-like and particulate potassium titanate (magnesium) in the synthetic product increases, and the mass ratio of the three raw materials can be adjusted within a range of ± 10 mass%. Magnesium oxide in the raw material is better the smaller the particle size, it can be selected as a high purity industrial activated magnesium oxide (light magnesium) as the magnesium oxide.

Thereafter, the mixture is molded into a predetermined shape and then calcined at 900 to 1100 ° C. for 0.2 to 3 hours. The high temperature calcination may be used in general electric heating, silicon carbide or molybdenum silicide heating, etc., in one embodiment of the present invention, the calcination process is heated under micro heating or micro-auxiliary conditions. It is possible that the micro heating can activate / accelerate the reaction of the production of potassium magnesium titanate to lower the calcination temperature, and also to shorten the calcination time and save energy. The mixture of potassium magnesium titanate and potassium magnesium titanate of the present invention can absorb microwaves and generate heat quickly, and if necessary, an absorbent material can be added separately. Therefore, the calcination equipment of the titanic acid whisker manufacturing apparatus according to the present invention may include a microwave heating furnace.

Thereafter, the calcined molding is pulverized, and the pulverized titanic whisker pulverized after the pulverizing process may be washed and dried. The high temperature calcining proceeds directly at 900 to 1100 ° C. for 0.2 to 3 hours. The pulverization may be used a variety of pulverizers, such as a drum-type crusher, it is preferable to use a jaw crusher during the washing and drying after the crushing. In the treatment of the calcined product may proceed directly to the grinding method, and may also proceed to the washing / drying method or acidic water washing drying method after grinding. Alkaline, dilute hydrochloric acid, or dilute acetic acid can be used for washing the water, and the pH value is 7 to 8.5. In the calcination process, about 15 wt% to 50 wt% of KCl may be added to the total mass ratio of the three raw materials. The addition of KCl and the acid wash process affect the final whiteness of the product.

In the case of producing potassium magnesium titanate according to the method for producing whiskers according to the present invention as described above, since both strong bases and cosolvents may not be used as raw materials, there is no corrosion on the equipment in the synthesis process, raw material consumption is low, and the process is low. Simple, suitable for large scale production, and low manufacturing cost.

Hereinafter, a method for preparing titanic acid whiskers according to various embodiments of the present invention will be described in more detail.

Example 1

1) The titanic acid compound (rutile titanium dioxide (TiO 2 ) or domestic titanium dioxide (TiO 2 ) from China (Shanghai)), potassium carbonate and magnesium oxide were sufficiently mixed in a mass ratio of 40:20:15, and an appropriate amount of water was added thereto. . After drying, it was ground.

2) The ground mixture of step 1) was calcined by microwave at 1050 ° C. for 1 hour, cooled in a furnace to 400 ° C. and then cooled by air.

3) Subsequently, the calcination product of step 2) was pulverized to prepare flaky potassium titanate shown in FIG. 1.

Referring to Figure 1, it can be seen that the magnesium magnesium titanate prepared according to the present embodiment has excellent uniformity as a flaky form.

Example  2

1) Titanium compound (China (Jinan Yeoheung) acid or domestic rutile titanium dioxide (TiO 2 )), potassium carbonate and magnesium oxide are sufficiently mixed in a mass ratio of 40:20:15, and an appropriate amount of water is added and 10 MPa pressure is applied. Pressurized to form a pillar shape of 3cm in diameter, 3cm in height.

2) The molded product of step 1) was calcined in a microwave at 1050 ° C. for 1 hour, cooled to 400 ° C. in a furnace, and then air cooled.

3) Crush the resulting calcined product of step 2), wash with acidic water and dry. The photograph of the plate-shaped potassium titanate obtained from this is as shown in FIG.

2, it can be seen that the plate-shaped potassium magnesium titanate is more finely prepared than in FIG.

Claims (12)

As a method for producing flaky titanic acid whiskers, the method
Mixing the titanium compound, potassium carbonate and magnesium oxide mixed in a mass ratio of 40:20:10 to 20;
Calcining the mixture at 900 to 1100 ° C. by microwave heating; And
And crushing the calcined mixture.
The method of claim 1,
The method of claim 1, further comprising the step of molding the mixed mixture in a predetermined form between the mixing step and the calcining step.
delete The method of claim 1,
The titanium compound is a rutile type, fusiform or brookite type titanium dioxide whisker manufacturing method, characterized in that.
The method of claim 4, wherein
The titanium compound is a rutile titanium dioxide whisker production method, characterized in that the.
delete The method of claim 1,
And said titanium compound, potassium carbonate and magnesium oxide are mixed in a mass ratio of 40:20:15.
delete The method of claim 1,
The calcination step is flaky titanic acid whisker manufacturing method, characterized in that performed for 0.2 to 3 hours.
delete delete delete
KR1020100066816A 2010-07-12 2010-07-12 A method for preparing flake-type titanic acid whiskers and flake-type titanic acid whiskers prepared by the same KR101058379B1 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101319298B1 (en) 2011-09-29 2013-10-18 국방과학연구소 Titanium dioxide nanowhickers and method of producing the same by using a cycling heat treatment
KR102080505B1 (en) * 2019-08-13 2020-02-24 주식회사 경남케미컬 Potassium titanate and method for producing thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004316904A (en) 2003-03-31 2004-11-11 Tokico Ltd Friction material for brake
JP2009280499A (en) * 2009-09-01 2009-12-03 Otsuka Chem Co Ltd Plate-like potassium tetratitanate, its production method and friction material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004316904A (en) 2003-03-31 2004-11-11 Tokico Ltd Friction material for brake
JP2009280499A (en) * 2009-09-01 2009-12-03 Otsuka Chem Co Ltd Plate-like potassium tetratitanate, its production method and friction material

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101319298B1 (en) 2011-09-29 2013-10-18 국방과학연구소 Titanium dioxide nanowhickers and method of producing the same by using a cycling heat treatment
KR102080505B1 (en) * 2019-08-13 2020-02-24 주식회사 경남케미컬 Potassium titanate and method for producing thereof

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