CN1865536A - Preparation method of alkali metal titanium-based whisker and platelet - Google Patents

Preparation method of alkali metal titanium-based whisker and platelet Download PDF

Info

Publication number
CN1865536A
CN1865536A CN200610039687.5A CN200610039687A CN1865536A CN 1865536 A CN1865536 A CN 1865536A CN 200610039687 A CN200610039687 A CN 200610039687A CN 1865536 A CN1865536 A CN 1865536A
Authority
CN
China
Prior art keywords
alkali metal
titanium
preparation
tio
platelet
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN200610039687.5A
Other languages
Chinese (zh)
Other versions
CN100491603C (en
Inventor
陆小华
刘畅
秦夕峰
王昌松
冯新
王浩
杨祝红
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhenjiang Dibo New Mstar Technology Ltd
Original Assignee
Nanjing Tech University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanjing Tech University filed Critical Nanjing Tech University
Priority to CNB2006100396875A priority Critical patent/CN100491603C/en
Publication of CN1865536A publication Critical patent/CN1865536A/en
Application granted granted Critical
Publication of CN100491603C publication Critical patent/CN100491603C/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

A method for preparing alkali metal titanium-based whiskers and platelets comprises the steps of fully mixing titanium minerals, alkali metal-containing compounds, a fluxing agent, a reducing agent and water; the mass percentage of the fluxing agent in the mixture is10-50 percent of reducing agent, 1-40 percent of water and the balance of titanium mineral and alkali metal-containing compound; TiO synthesized by titanium mineral and alkali metal-containing compound2And M2O in a molar ratio of TiO2/M2O is 2.0-4.0, wherein M is an alkali metal; sintering the mixture at 800-1300 ℃ for 30 minutes-10 hours; and washing, dispersing, filtering and drying the sintered product. The alkali metal titanium-based whisker and the platelet prepared by the method have complete structures and uniform quality.

Description

The preparation method of a kind of alkali metal titanium-base crystal whisker and platelet
Technical field
The present invention relates to the preparation method of a kind of alkali metal titanium-base crystal whisker and platelet, be particularly for a kind of by the simple once sintered method of preparing alkali metal titanium-base crystal whisker and platelet.
Background technology
Alkali metal titanium-base crystal whisker and platelet have enhancing, effect such as heat insulation, can be applicable to industries such as plastics, coating, friction materials.Particularly crystal whisker of hexa potassium titanate has good mechanics and physicals, and excellent heat insulation, wear resistance can replace the strong carcinogen asbestos, have avoided environmental pollution like this, have improved the frictional coefficient and the thermostability of friction materials simultaneously [1], have significant social and economic benefit.
The method of traditional preparation process alkali metal titanium-base crystal whisker and platelet is with TiO 2Mix according to a certain percentage with alkaline carbonate, obtain through high-temperature calcination then [1-5], because TiO 2Expensive market value makes that the preparation cost of alkali metal titanium-base crystal whisker and platelet is too high, can not be by large-scale application.Simultaneously, use carbothermic method [6-8]From titanium ore preparation TiO 2The time, still needing through high-temperature calcination, this is the process of a high energy consumption, also is to cause TiO 2One of reason that price is high.Now with the ilmenite for the feedstock production alkali metal titanium-base crystal whisker mostly is two-step approach, promptly earlier with TiO in the ilmenite 2Enrichment becomes titanium slag, and at high temperature reaction generates the alkali metal titanate whisker with alkali metal compound more then [9]W.Akira etc. [10]With the ilmenite of acid treatment and alkali metal compound, graphite, prepare the alkali metal titanate whisker by high temperature sintering, this technology in fact still is two-step approach, at first comes enrichment TiO by the washing ilmenite 2, and then high temperature sintering goes out desired product, and this technology can produce waste water, is unfavorable for environmental protection.
Summary of the invention
The objective of the invention is to realize the high quality and low cost preparation of alkali metal titanium-base crystal whisker and platelet, is presoma with titanium minerals such as ilmenite, ilmenite concentrate, pseudobrookites, and the carbothermic reduction of titanium mineral is prepared TiO 2Process and TiO 2Sintering prepares the PROCESS COUPLING of titanium-base crystal whisker and platelet is in the same place, and a step obtains titanium-base crystal whisker and platelet product in the high-temperature fusant environment.
Purpose of the present invention can reach by following measure:
The preparation method of a kind of alkali metal titanium-base crystal whisker and platelet is characterized in that carrying out according to the following steps:
1. with titanium mineral, alkali metal-containing compound and fusing assistant, reductive agent, water, thorough mixing; Fusing assistant quality percentage composition is 10%~50% in the mixture, and reductive agent quality percentage composition is 1%~40%, and the quality percentage composition is 10%~50%, and all the other are titanium mineral and alkali metal-containing compound; Titanium mineral is amounted to into TiO with alkali metal-containing compound 2With M 2O, its mol ratio is TiO 2/ M 2O=2.0~4.0, wherein M is a basic metal;
2. with said mixture 800~1300 ℃ of following sintering 30 minutes~10 hours;
3. sintered product is washed dispersion, filtration, drying.
Wherein titanium mineral is ilmenite, ilmenite concentrate, pseudobrookite, ulvite or arizonite; Alkali metal-containing compound is nitrate, carbonate or the oxyhydroxide of lithium, sodium, potassium, rubidium, caesium; Fusing assistant is one or more in alkali-metal nitrate, vitriol or the muriate; Reductive agent is one or more in coke, charcoal, graphite or the coal.
The product that the present invention makes is alkali metal titanium-base crystal whisker or platelet M 0.2-2.0Fe 0-2.0Ti 0.2-6O 2-16, wherein the content of iron can be controlled by reductive agent.Product whisker length 10~100 μ m, diameter 1~4 μ m; Platelet diameter 8~15 μ m, thickness 1~3 μ m.The present invention directly is presoma with the titanium mineral, and the carbothermic reduction of titanium mineral is prepared TiO 2Process and TiO 2Sintering prepares the PROCESS COUPLING of titanium-base crystal whisker and platelet and is in the same place, shorten technical process, adopted melting method simultaneously, improved the crystal property of product, thereby be the method that a kind of low-cost and high-quality prepares alkali metal titanium-base crystal whisker and platelet, help suitability for industrialized production and application.The alkali metal titanium-base crystal whisker of the present invention preparation and platelet have excellent properties such as enhancing, heat insulation, friction.
Description of drawings
Fig. 1 is scanning electronic microscope (SEM) figure of iron titanate lithium platelet of the present invention.
Fig. 2 is scanning electronic microscope (SEM) figure of crystal whisker of hexa potassium titanate of the present invention.
Fig. 3 is scanning electronic microscope (SEM) figure of iron titanate caesium whisker of the present invention.
Embodiment
According to embodiment the present invention is further described below:
Embodiment 1.
1. preparation of raw material: ilmenite, Li 2CO 3, LiCl, graphite, H 2O.Above-mentioned raw materials uniform mixing, wherein mol ratio TiO 2/ Li 2O=2.0 contains 10wt%LiCl, graphitiferous 10wt%, moisture 50wt%; 2. mixed reaction mass is loaded in the alumina crucible, temperature of reaction is 800 ℃, and the reaction times is 10 hours; 3. the sintered product washing is disperseed; 4. filter; 5. following dry 2.5 hours at 150 ℃.
That said process obtains is Li 1.12Fe 0.62Ti 1.25O 4Platelet, diameter 8~15 μ m, thickness 1~3 μ m, quality is even, structural integrity.
Other embodiment are all by the method for embodiment 1, and concrete raw material composition, implementation condition and product characterize as shown in table 1.
Concrete raw material composition, implementation condition and the shape of product of table 1 embodiment 2~5
Other embodiment Raw material is formed (wt) TiO 2/M 2O mol ratio Sintering temperature and time Product and pattern Length μ m Diameter μ m Thickness μ m
Embodiment 2 Pseudobrookite, NaOH NaNO 350% charcoal, 1% water 10% 4.0 1300℃ 30min NaFeTiO 4Whisker 20~100 2~4
Embodiment 3 Ulvite, KNO 3 KCl,K 2SO 410% charcoal, coal 40% water 10% 3.5 1200℃ 2h K 2Ti 6O 13Whisker 10~60 1~3
Embodiment 4 Arizonite, Rb 2CO 3 RbNO 310% coal, 30% water 20% 3.0 1100℃ 8h RbFeTi 3O 8Platelet 8~12 1~3
Embodiment 5 Ilmenite concentrate, CsOH CsCl 20% coke 20% water 20% 2.5 1000℃ 5h Cs 0.75Fe 0.75T i 0.25O 2Whisker 10~80 1~3
Comparative example 1.
1. preparation of raw material: TiO 2, NaOH, H 2O.Above-mentioned raw materials uniform mixing, wherein mol ratio TiO 2/ Na 2O=2.0, moisture 40wt%; 2. mixed reaction mass is loaded in the alumina crucible, temperature of reaction is 1300 ℃, and the reaction times is 30min; 3. the sintered product washing is disperseed; 4. filter; 5. following dry 2.5 hours at 150 ℃.
What said process obtained is sodium hexatitanate whisker, its diameter 1~2.5 μ m, and length 10~30 μ m compare with embodiment 2, owing to changed the reaction precursor body, do not add fusing assistant, and the product crystallinity is relatively poor.
Comparative example 2.
1. preparation of raw material: arizonite, K 2CO 3, graphite, H 2O.Above-mentioned raw materials uniform mixing, wherein mol ratio TiO 2/ K 2O=3.0, graphitiferous 40wt%, moisture 10wt%; 2. mixed reaction mass is loaded in the alumina crucible, temperature of reaction is 1200 ℃, and the reaction times is 2 hours; 3. the sintered product washing is disperseed; 4. filter; 5. following dry 2.5 hours at 150 ℃.
What said process obtained is six potassium titanates, compares with embodiment 3, owing to do not add fusing assistant, the product pattern is a crystal block, inferior quality.
Comparative example 3.
1. preparation of raw material: ilmenite concentrate, Rb 2CO 3, RbNO 3, H 2O.Above-mentioned raw materials uniform mixing, wherein mol ratio TiO 2/ Rb 2O=4.0 contains 10wt%RbNO 3, moisture 20wt%; 2. mixed reaction mass is loaded in the alumina crucible, temperature of reaction is 1100 ℃, and the reaction times is 8 hours; 3. the sintered product washing is disperseed; 4. filter; 5. following dry 2.5 hours at 150 ℃.
The main component that said process obtains is an iron titanate rubidium particle, compares with embodiment 4, owing to do not add reductive agent, product is formed heterogeneity, inferior quality.
Comparative example 4.
1. preparation of raw material: ilmenite, CsOH, CsCl, graphite, H 2O.Above-mentioned raw materials uniform mixing, wherein mol ratio TiO 2/ Cs 2O=5.0 contains 60wt%CsCl, graphitiferous 0.5wt%, moisture 5wt%; 2. mixed reaction mass is loaded in the alumina crucible, temperature of reaction is 600 ℃, and the reaction times is 2 hours; 3. the sintered product washing is disperseed; 4. filter; 5. following dry 2.5 hours at 150 ℃.
What said process obtained is the iron titanate caesium, compares with embodiment 5, because these processing condition exceed processing range of the present invention, so the product pattern is particulate state, inferior quality.
By embodiment and comparative example more as can be seen: the present invention makes the crystalline quality obviously improve owing to add fusing assistant and reductive agent in reaction.Compare with traditional technology, the present invention has changed the reaction precursor body, and has shortened flow process, greatly reduces production cost, and therefore as seen, the present invention is fit to large-scale industrialization production.
Reference
[1] Feng Xin, Yang Zhuhong, Lu Xiaohua etc., the preparation method of crystal whisker of hexa potassium titanate, CN1323924A, 2001.
[2] Huai gift, Zhao Kuanfang, potassium titanate crystal whiskers preparation method, CN1093760,1994.
[3] Cheng Cunkang, Xu Hong, Hu Hengyao, Gu Hongchen, the preparation method of crystal whisker of hexa potassium titanate, CN1472369,2004.
[4]K.Isamu,A.Kenji,Production of potassium titanate fiber,JP10212625,1998。
[5]H.Ogawa,S.Takahashi,N.Itoi,Platy potassium titanate,process for producing the same,and friction material,US6677041,2000。
[6]S.A.F.Simon,M.D.John,Preparation of high-titania slag bycarbothermic smelting of ilmenite ore in electric-arc furnace,US2002-284636,2002。
[7]F.Lothar,B.A.Naghi,Process of producing synthetic rutilefrom ilmenite,AU 1998-63575,1998。
[8] what Anxi, preparation method of reduced ilmenite powder and uses thereof, CN1036228A.
[9]F.YOSHINORI,W.JIYUN,Production of titania fiber,JP60259625,1985。
[10]W.Akira,T.Yoshimitsu,S.Koji,F.Masashi,Production ofalkali titanate fiber,JP62207800,1987。

Claims (5)

1. the preparation method of alkali metal titanium-base crystal whisker and platelet is characterized in that carrying out according to the following steps:
1. with titanium mineral, alkali metal-containing compound and fusing assistant, reductive agent, water, thorough mixing; Fusing assistant quality percentage composition is 10%~50% in the mixture, and reductive agent quality percentage composition is 1%~40%, and the quality percentage composition is 10%~50%, and all the other are titanium mineral and alkali metal-containing compound; Titanium mineral is amounted to into TiO with alkali metal-containing compound 2With M 2O, its mol ratio is TiO 2/ M 2O=2.0~4.0, wherein M is a basic metal;
2. with said mixture 800~1300 ℃ of following sintering 30 minutes~10 hours;
3. sintered product is washed dispersion, filtration, drying.
2. preparation method according to claim 1 is characterized in that titanium mineral is ilmenite, ilmenite concentrate, pseudobrookite, ulvite or arizonite.
3. preparation method according to claim 1 is characterized in that alkali metal-containing compound is nitrate, carbonate or the oxyhydroxide of lithium, sodium, potassium, rubidium, caesium.
4. preparation method according to claim 1 is characterized in that fusing assistant is one or more in alkali-metal nitrate, vitriol or the muriate.
5. preparation method according to claim 1 is characterized in that reductive agent is one or more in coke, charcoal, graphite or the coal.
CNB2006100396875A 2006-04-20 2006-04-20 Preparation method of alkali metal titanium-based whisker and platelet Expired - Fee Related CN100491603C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB2006100396875A CN100491603C (en) 2006-04-20 2006-04-20 Preparation method of alkali metal titanium-based whisker and platelet

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNB2006100396875A CN100491603C (en) 2006-04-20 2006-04-20 Preparation method of alkali metal titanium-based whisker and platelet

Publications (2)

Publication Number Publication Date
CN1865536A true CN1865536A (en) 2006-11-22
CN100491603C CN100491603C (en) 2009-05-27

Family

ID=37424676

Family Applications (1)

Application Number Title Priority Date Filing Date
CNB2006100396875A Expired - Fee Related CN100491603C (en) 2006-04-20 2006-04-20 Preparation method of alkali metal titanium-based whisker and platelet

Country Status (1)

Country Link
CN (1) CN100491603C (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102677173A (en) * 2012-05-22 2012-09-19 中国科学院青海盐湖研究所 Preparation method of lead titanate whiskers
CN102787359A (en) * 2012-09-03 2012-11-21 中国科学院青海盐湖研究所 Preparation method for calcium titanate whiskers
CN104762659A (en) * 2015-05-08 2015-07-08 唐山晶须复合材料制造有限公司 Synthetic method for columnar sodium hexatitanate
CN116199268A (en) * 2023-04-06 2023-06-02 攀枝花学院 Preparation method of sodium iron titanate powder

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102677173A (en) * 2012-05-22 2012-09-19 中国科学院青海盐湖研究所 Preparation method of lead titanate whiskers
CN102787359A (en) * 2012-09-03 2012-11-21 中国科学院青海盐湖研究所 Preparation method for calcium titanate whiskers
CN102787359B (en) * 2012-09-03 2015-04-15 中国科学院青海盐湖研究所 Preparation method for calcium titanate whiskers
CN104762659A (en) * 2015-05-08 2015-07-08 唐山晶须复合材料制造有限公司 Synthetic method for columnar sodium hexatitanate
CN104762659B (en) * 2015-05-08 2017-11-07 唐山晶须复合材料制造有限公司 A kind of synthetic method of column sodium hexatitanate
CN116199268A (en) * 2023-04-06 2023-06-02 攀枝花学院 Preparation method of sodium iron titanate powder

Also Published As

Publication number Publication date
CN100491603C (en) 2009-05-27

Similar Documents

Publication Publication Date Title
KR102305363B1 (en) Potassium titanate powder, method for producing same, friction modifier, resin composition, friction material, and friction member
WO2022252931A1 (en) Antibacterial and antistatic laboratory ceramic countertop and preparation method therefor
CN100491603C (en) Preparation method of alkali metal titanium-based whisker and platelet
Bao et al. High quality and yield in potassium titanate whiskers synthesized by calcination from hydrous titania
TWI558657B (en) Application of carbon nanotubes on agglomerates of fine ore to increase the mechanical strength
CN111484050B (en) Preparation method of spheroidal alpha-phase nano-alumina
CN109081684A (en) A kind of preparation method of carbon nanotube enhancing alumina matrix composite
JP5133309B2 (en) Plate-like potassium titanate, method for producing the same, and friction material
CN100594183C (en) Method for preparing titanate based on carnallite and titanium-containing mineral
CN108328651A (en) The spherical potassium titanate preparation method of porous hollow
CN111841494A (en) Active carbon for air purification
JP2001253712A (en) Plate like potassium hexatitanate, plate like potassium tetratitanate, manufacturing method thereof and friction material
CN104894364A (en) A method of producing magnesium titanate and direct-reduced iron by coal-based reduction and magnetic separation of titanomagnetite
CN115874047A (en) Fluxed pellet containing specularite and preparation method thereof
CN1086426C (en) Prodn. method of potassium titanate whisker and fiber
CN115073147A (en) Preparation method of low-sodium and ultra-low-sodium tabular sintered corundum
CN112125343A (en) Iron oxide red for environment-friendly permanent magnet oxide and preparation method thereof
CN113321221A (en) Method for preparing white carbon black by using iron tailings
Aifen et al. Preparation of Barite/Titanium Dioxide Composite Powder by Hydrolysis of Titanium Oxysulfate.
CN109608210B (en) Metakaolin-based refractory material and preparation method thereof
CN106672960A (en) High-density graphite material and production process thereof
JP2023553197A (en) Amorphous tungstic acid fusion and tungsten oxide produced using the same
CN111547751A (en) Method for preparing porous alumina by using solid waste
KR20110019603A (en) Preparation of silver nano-powder from agcl by slurry reduction methods and silver nano-powder thereof
CN114890810B (en) Mullite lightweight aggregate with rice hull genetic structure and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
ASS Succession or assignment of patent right

Owner name: ZHENJIANG DURABLE ADVANCED NEW MATERIALS TECHNOLOG

Free format text: FORMER OWNER: NANJING UNIVERSITY OF TECHNOLOGY

Effective date: 20150324

C41 Transfer of patent application or patent right or utility model
COR Change of bibliographic data

Free format text: CORRECT: ADDRESS; FROM: 210009 NANJING, JIANGSU PROVINCE TO: 212000 ZHENJIANG, JIANGSU PROVINCE

TR01 Transfer of patent right

Effective date of registration: 20150324

Address after: 212000 No. 68 Linjiang West Road, Dagang District, Zhenjiang, Jiangsu, Zhenjiang

Patentee after: Zhenjiang Dibo new Mstar Technology Ltd.

Address before: 210009 Nanjing City, Jiangsu Province, the new model road No. 5

Patentee before: Nanjing Tech University

CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20090527