CN114890462A - Preparation method of columnar potassium hexatitanate - Google Patents
Preparation method of columnar potassium hexatitanate Download PDFInfo
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- CN114890462A CN114890462A CN202210531580.1A CN202210531580A CN114890462A CN 114890462 A CN114890462 A CN 114890462A CN 202210531580 A CN202210531580 A CN 202210531580A CN 114890462 A CN114890462 A CN 114890462A
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- Prior art keywords
- potassium
- columnar
- raw material
- containing raw
- potassium hexatitanate
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- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 34
- 239000011591 potassium Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 239000010936 titanium Substances 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000008117 stearic acid Substances 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 17
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 7
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 4
- 239000011736 potassium bicarbonate Substances 0.000 claims description 4
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 4
- 235000011181 potassium carbonates Nutrition 0.000 claims description 4
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 4
- 239000002783 friction material Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005245 sintering Methods 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000006872 improvement Effects 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 4
- 239000010425 asbestos Substances 0.000 description 3
- 229910052895 riebeckite Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The application discloses a preparation method of columnar potassium hexatitanate, which sequentially comprises the following steps: s1, mixing a titanium-containing raw material and a potassium-containing raw material according to the proportion of 5-8 Ti/K2, adding 2-5% of stearic acid for mixing, and grinding and crushing the mixed materials; s2, 10-20% of the material is left on a 150-micron sieve; s3, placing the mixture into a high-temperature furnace for calcination, setting the calcination temperature to be 800-1200 ℃, setting the heating rate to be 5-10 ℃/min, calcining for 4-8 hours, and then cooling to the room temperature at the rate of 2-5 ℃/min; and S4, crushing and grading to obtain a columnar potassium hexatitanate product. The invention has simple synthesis process, is obtained by one-time sintering method, does not need acid and alkali treatment in subsequent production and has short production period. The method greatly reduces the production cost, does not discharge waste water and is friendly to environment improvement. Its microcosmic shape is columnar, structure is stable, and when it is added in friction material, it can greatly raise friction coefficient.
Description
Technical Field
The invention relates to potassium titanate, in particular to a preparation method of columnar potassium hexatitanate.
Background
The potassium titanate is represented by the chemical formula K 2 O·nTiO 2 (n-2, 4, 6, 8) and the crystalline substance was measured by a rotary target X-ray powder diffractometer. Different n, potassium titanate has different structures and characteristics and is used in different fields. The potassium dititanate has unstable structure and can be used for preparing precursors of potassium hexatitanate and potassium octatitanate. The potassium tetratitanate has ion exchange capacity and high performanceThe chemical property of (A) is mainly used for precursors of ion exchangers, nuclear waste treatment and the like; the potassium hexatitanate and the potassium octatitanate have similar structures, high mechanical property, good chemical stability, heat resistance and heat insulation, good wear resistance, large cost performance and large specific surface area, are mainly used for reinforcing composite materials, modifying engineering plastics, reinforcing ceramics, metals and friction materials, and can also be used for heat insulation and heat resistance materials, catalyst carriers, thermal spraying and infrared reflection coatings.
Potassium titanate friction materials have been developed in recent years as friction control agents that primarily control the performance of friction materials. The heat resistance and the frictional wear performance of the asbestos-containing friction material are poor, and particularly the wear resistance in a high-temperature area is obviously reduced, so that the brake heat fading phenomenon is caused. In addition, as is well known, asbestos is a carcinogenic substance, dust is easily generated to affect environmental protection and human health, and the use is increasingly limited. Under such circumstances, there is an urgent need to develop an alternative to asbestos. In response to this requirement, it has been proposed that friction materials using non-toxic potassium titanate whiskers as a friction control agent and having been widely used mainly for automobile brake pads, which friction materials have the advantageous advantage of excellent sliding properties and good braking effect, with little damage to the brake disc. However, this material has insufficient wear resistance and wears at a high rate particularly in a high-temperature region. They also do not allow the braking noise generated during braking to be completely eliminated. Further, since the potassium titanate whiskers are fibrous and have poor fluidity, they tend to deposit on the walls of the feed channels and to clog the channels when producing friction materials, and this is a problem in the art. Meanwhile, the whisker material is easy to absorb into a breathing passage and is harmful to human health, so that the whisker material is limited in use in many countries.
Disclosure of Invention
The invention aims to provide a preparation method of columnar potassium hexatitanate, which comprises the steps of adding an auxiliary agent into a titanium-containing raw material and a potassium-containing raw material, grinding, mixing, crushing, calcining at high temperature, crushing and grading to obtain the columnar potassium hexatitanate. According to the invention, the columnar potassium hexatitanate can be obtained by changing the ratio of titanium to potassium, adding an auxiliary agent and calcining at high temperature. The columnar potassium hexatitanate is calcined at high temperature, and part of rutile type titanium dioxide is separated out on the surface, so that the obtained potassium hexatitanate has a stable structure and the friction coefficient is greatly improved.
In order to achieve the above object, the present invention provides the following technical solutions.
The embodiment of the application discloses a preparation method of columnar potassium hexatitanate, which sequentially comprises the following steps:
s1, mixing a titanium-containing raw material and a potassium-containing raw material according to the proportion of 5-8 Ti/K2, adding 2-5% of stearic acid for mixing, and grinding and crushing the mixed materials;
s2, 10-20% of the material is left on a 150-micron sieve;
s3, placing the mixture into a high-temperature furnace for calcination, setting the calcination temperature to be 800-1200 ℃, setting the heating rate to be 5-10 ℃/min, calcining for 4-8 hours, and then cooling to the room temperature at the rate of 2-5 ℃/min;
and S4, crushing and grading to obtain a columnar potassium hexatitanate product.
Preferably, in the above method for preparing columnar potassium hexatitanate, the titanium-containing raw material is one or more of rutile titanium oxide, anatase titanium oxide, brookite titanium oxide, or metatitanic acid.
Preferably, in the preparation method of the columnar potassium hexatitanate, the potassium-containing raw material is one or more of potassium carbonate and potassium bicarbonate.
The invention has simple synthesis process, is obtained by one-time sintering method, does not need acid and alkali treatment in subsequent production and has short production period. The method greatly reduces the production cost, does not discharge waste water and is friendly to environment improvement. Its microcosmic shape is columnar, structure is stable, and when it is added in friction material, it can greatly raise friction coefficient.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the description below are only some embodiments described in the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a SEM photograph of a product obtained in an embodiment of the present invention;
figure 2 shows the XRD pattern of the product obtained in the example of the present invention.
Detailed Description
Technical solutions in the embodiments of the present invention will be described in detail below, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Mixing a titanium-containing raw material (the titanium-containing raw material is anatase titanium oxide with the content of more than 98%) and a potassium-containing raw material (the potassium-containing raw material is a mixture of potassium carbonate and potassium bicarbonate, wherein the potassium carbonate: potassium bicarbonate is 1: 1) according to the mass fraction of 3% of stearic acid and the proportion of 6.5 to Ti/K2, and then crushing the mixture to 10-20% of residues on a 150 mu m sieve by a ball mill. Putting the crushed raw materials into a high-temperature furnace for calcining, setting the sintering temperature to be 1200 ℃, and the heating rate to be: the temperature of the mixture is 5 ℃/min,
the sintering time is 4 hours, and then the temperature is reduced to the room temperature according to the speed of 3 ℃/min. And crushing and grading the sintered product by using a hammer mill to obtain a columnar potassium hexatitanate product with the average particle size of 30-40 mu m.
The SEM picture and XRD pattern of the product are shown in figure 1 and figure 2.
The present embodiments are to be considered as illustrative and not restrictive, and the scope of the patent is to be determined by the appended claims.
Claims (3)
1. The preparation method of columnar potassium hexatitanate is characterized by sequentially comprising the following steps of:
s1, mixing a titanium-containing raw material and a potassium-containing raw material according to the proportion of 5-8 Ti/K2, adding 2-5% of stearic acid for mixing, and grinding and crushing the mixed materials;
s2, 10-20% of the material is left on a 150-micron sieve;
s3, placing the mixture into a high-temperature furnace for calcination, setting the calcination temperature to be 800-1200 ℃, setting the heating rate to be 5-10 ℃/min, calcining for 4-8 hours, and then cooling to the room temperature at the rate of 2-5 ℃/min;
and S4, crushing and grading to obtain a columnar potassium hexatitanate product.
2. The method for preparing columnar potassium hexatitanate according to claim 1, wherein the titanium-containing raw material is one or more of rutile type titanium oxide, anatase type titanium oxide, brookite type titanium oxide, or metatitanic acid.
3. The method for preparing columnar potassium hexatitanate according to claim 1, wherein the potassium-containing raw material is one or more of potassium carbonate and potassium bicarbonate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210531580.1A CN114890462A (en) | 2022-05-17 | 2022-05-17 | Preparation method of columnar potassium hexatitanate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210531580.1A CN114890462A (en) | 2022-05-17 | 2022-05-17 | Preparation method of columnar potassium hexatitanate |
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| Publication Number | Publication Date |
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| CN114890462A true CN114890462A (en) | 2022-08-12 |
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| CN202210531580.1A Pending CN114890462A (en) | 2022-05-17 | 2022-05-17 | Preparation method of columnar potassium hexatitanate |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100112350A1 (en) * | 2007-03-29 | 2010-05-06 | Koji Tanimizu | Method of manufacturing alkali metal titanate and hollow body particle thereof, product thereof, and friction material containing the product |
| CN102070188A (en) * | 2010-12-09 | 2011-05-25 | 江南大学 | Method for preparing difficult-to-harden potassium titanate with low hygroscopicity and high bulk density |
| CN102849790A (en) * | 2012-09-27 | 2013-01-02 | 攀枝花学院 | Preparation method of columnar hexagonal potassium titanate |
| CN105050958A (en) * | 2013-03-18 | 2015-11-11 | 东邦钛株式会社 | Method for producing potassium titanate |
| CN112479251A (en) * | 2020-12-12 | 2021-03-12 | 张家港大塚化学有限公司 | Preparation method of large-particle-size non-fibrous potassium hexatitanate |
-
2022
- 2022-05-17 CN CN202210531580.1A patent/CN114890462A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100112350A1 (en) * | 2007-03-29 | 2010-05-06 | Koji Tanimizu | Method of manufacturing alkali metal titanate and hollow body particle thereof, product thereof, and friction material containing the product |
| CN102070188A (en) * | 2010-12-09 | 2011-05-25 | 江南大学 | Method for preparing difficult-to-harden potassium titanate with low hygroscopicity and high bulk density |
| CN102849790A (en) * | 2012-09-27 | 2013-01-02 | 攀枝花学院 | Preparation method of columnar hexagonal potassium titanate |
| CN105050958A (en) * | 2013-03-18 | 2015-11-11 | 东邦钛株式会社 | Method for producing potassium titanate |
| CN112479251A (en) * | 2020-12-12 | 2021-03-12 | 张家港大塚化学有限公司 | Preparation method of large-particle-size non-fibrous potassium hexatitanate |
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Application publication date: 20220812 |