CN102839424A - Method for preparing potassium hexatitanate whisker - Google Patents
Method for preparing potassium hexatitanate whisker Download PDFInfo
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- CN102839424A CN102839424A CN2012103747309A CN201210374730A CN102839424A CN 102839424 A CN102839424 A CN 102839424A CN 2012103747309 A CN2012103747309 A CN 2012103747309A CN 201210374730 A CN201210374730 A CN 201210374730A CN 102839424 A CN102839424 A CN 102839424A
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Abstract
The invention discloses a method for preparing a potassium hexatitanate whisker, belonging to the field of chemical industry. The method comprises the following steps of: a, uniformly mixing 100-mesh titanium-containing raw material and potassium-containing raw material according to mole rate of TiO2 to K2O being 3-6; b, placing the materials in an environment at temperature of 1100-1300 DEG C and sintering for 1-5 hours to make the materials fully reacted; and c, rapidly cooling the sintered materials, fully dissociating in an environment at constant temperature of 60-80 DEG C by using water, filtering, drying, and thus obtaining the potassium hexatitanate whisker. The process flow is simple, production period is short, yield is high, meanwhile, a production process of a precursor or a post-period recrystallization conversion process in the prior art is reduced, energy consumption is saved, and production cost is reduced. The cooled materials are fully dissociated in the environment at constant temperature of 60-80 DEG C by using the water, so that the potassium hexatitanate whisker has good purity and is suitable for industrial production.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of preparation method of crystal whisker of hexa potassium titanate.
Background technology
Whisker (Whiskers) is a kind of fibrous single crystal; The transverse section is close to consistent, and the external and internal compositions height is complete, and length-to-diameter ratio is generally more than 5～1000; Diameter is usually between 200nm～100 μ m, but the diameter of whiskers with special property is generally between 1～10 μ m.Potassium titanate crystal whisker also is potassium titanate fiber, is white needle-like crystals, and density is 3.2g/cm
3, have good thermotolerance, chemicalstability and chemical resistance, have high surface strength (>700kg/mm
2) and high Young's modulus (>2800kg/mm
2).Be at first E.I.Du Pont Company by the U.S. at the synthetic fifties, at first as heat-resisting, heat insulation with the starting material exploitation, be applied to universe and military aspect.At present, potassium titanate crystal whisker is mainly as the absorbing material of strongthener, high-temperature resistant coating, electro-conductive fiber and the radioactive substance of macromolecular material etc.That application is maximum in potassium titanate crystal whisker is crystal whisker of hexa potassium titanate (K
2Ti
6O
13), it is the most stable compound of potassium titanate crystal whisker series, the whisker excellent property is not with diluted acid, diluted alkaline, salts solution and organic solvent reaction.
At present, the technology of preparing of crystal whisker of hexa potassium titanate mainly comprises sintering process, hydrothermal method, scorification, helps the method for melting and microwave process for synthesizing etc., and this wherein has only sintering process can be widely used in the suitability for industrialized production of crystal whisker of hexa potassium titanate.Through document retrieval, application number is the working method that 200610031042.7 Chinese patent discloses a kind of crystal whisker of hexa potassium titanate, and its main technology is: 1. with titaniferous materials with contain the potassium raw material according to TiO
2: K
2The ratio weighing of O=1.9 ~ 2.0 mol ratios; 2. the above-mentioned raw material that mixes is entered into 900 ~ 1300 ℃ High Temperature Furnaces Heating Apparatus, stopped 30 ~ 90 minutes, make raw mix become molten mass; 3. above-mentioned molten mass is taken out,, make it be dispersed into the fine powder of particle diameter less than 1mm in the quenching of professional quenching machine; 4. with the ratio volume of above-mentioned fine powder in solid-to-liquid ratio 1:15 to 1:5, advance in 90 ~ 99 ℃ the hydrothermal reaction device, between the pH value 10 ~ 12 of sulphuric acid soln control solution, reacted 90 ~ 360 minutes with 1 ~ 15%; 5. the solution in the above-mentioned reactor drum is carried out solid-liquid separation, liquid portion is accumulated separately, is pure alkaline potassium sulfate solution; 6. with the deionized water repetitive scrubbing of above-mentioned solid part, wash most sulfate ion (SO with 1 ~ 4 ℃
4 2+), washing water turn back in the reactor drum and recycle; The wet feed that draws off in the above-mentioned filter is dry 7., slough surface water; 8. with the above-mentioned material of sloughing surface water, stopped 90 ~ 360 minutes down, accomplish the recrystallization conversion, be cooled to room temperature and be finished product at 600 ~ 1000 ℃.There is following shortcoming in this method: 1. process step is complicated, is unfavorable for industrialization production; 2. life cycle of the product is long; 3. need the recrystallization conversion, fuel expends height, and production cost is too high; 4. caking phenomenon can be occurred in the recrystallization sintering process, crushing process need be carried out specially, sieve classification then, such Mechanical Crushing will inevitably cause the fracture of part whisker, has influenced the homogeneity of potassium titanate crystal whisker.5.1 ~ 4 ℃ of deionized water repetitive scrubbings, condition are harsh, are difficult to realize in Panzhihua Region.Temperature is low more in addition, and the filtration of basic soln is low more, and the efficient that causes producing reduces.
Application number is the preparation method that 03116985.6 Chinese patent discloses another kind of crystal whisker of hexa potassium titanate.Its main technique is:
1. preparation of raw material: raw material is amounted to into TiO
2With K
2O presses TiO
2∕ K
2O=2 ~ 6mol, preferably 4 ~ 6mol adds water and mixes, and wherein the weight percent of water cut is 50 ~ 95%; 2. precursor preparation: adopt spraying drying or rotary flashing drying, stock suspension is processed the more uniform spherical reaction precursor body of size; 3. reaction: the reaction precursor body is packed in the crucible or is pre-formed as base substrate, 1100 ℃ ~ 1300 ℃ sintering 0.5 ~ 12 hour; 4. separate fibre: sintered product is soaked and 5 ~ 15 times in 50 ~ 100 ℃ the deionized water 2 ~ 10 hours and stir to separate and knit; 5. filter washing; 6: drying: the filter cake that will wash makes crystal whisker of hexa potassium titanate 150 ℃ of dryings 2 hours.There is following shortcoming in this technology: the production cycle is long; The preparation of presoma is complicated, and production technique is complicated.
Application number is the preparation method that 201110289501.2 Chinese patent discloses another kind of crystal whisker of hexa potassium titanate, and its main technique is: with K
2CO
3(contain TiO with metatitanic acid
240wt%) in molar ratio [n (K2CO3) ∕ n (TiO2)] at room temperature mix for 1:3.5, put into 150 ℃ of loft drier, regularly to stir, be 24h time of drying, gets the reaction precursor body; In the 250ml crucible, put into the 100g presoma, in 150 ℃, 400 ℃, 600 ℃, 800 ℃, 1000 ℃, 1150 ℃ following roastings, roasting time is got 2h, 4h, 7h, 10h respectively in retort furnace; To temperature is that 1000 ℃, 1150 ℃ roasting different time products therefroms carry out water logging processing 10h in the azeotropic water-bath, and product is suction filtration after water logging is handled, and puts into to obtain the crystal whisker of hexa potassium titanate product after 150 ℃ of loft drier are dried 24h.The main shortcoming of this method is: life cycle of the product is long; Complex manufacturing.
Application number is that 01134183.1 Chinese patent is that the production of crystal whisker of hexa potassium titanate provides a kind of method, and the Production Flow Chart of this method is: 1. mix, according to titanium source (TiO
2): potassium source (K
2O)=1.9 ~ 2.5 mol ratio is put into ball mill with titanium source and potassium source and is mixed, and processes compound; 2. sintering, it is 900 ~ 1200 ℃ box-type furnace or tunnel that above-mentioned compound is put into temperature, sintering 0.5 ~ 4 hour makes it sinter molten mass into; 3. use twin rollers that above-mentioned molten mass is sharply cooled off, its method is, in two rollers of twin rollers, feeds recirculated cooling water, is after above-mentioned molten mass gets into from twin rollers top, in quenching, to be squeezed into thin slice by two rollers; 4. dispersion treatment according to the ratio of above-mentioned thin slice: pure water=1:5 ~ 1:50, is put into reactor drum with above-mentioned thin slice and pure water, and is heated to 60 ~ 100 ℃, and adding concentration was 3 ~ 20% diluted acid in per 10 ~ 20 minutes, was pH value>=9 of solution; Simultaneously, under 200 ~ 1000 Zhuan ∕ minutes rotating speed, stirred 1 ~ 5 hour, process suspension-s; 5. separating, with whizzer suspension-s is separated, go out wherein moisture, is that it becomes meal; 6. washing is put into whizzer with meal, and adds pure water, and meal is washed; 7. dry, will appealing meal, to put into temperature be 100 ~ 300 ℃ baking oven, toasted 3 ~ 5 hours, makes its drying; 8. high temperature crystallization sintering, will passing through meal that drying treatment crosses, to place temperature be 900 ~ 1200 ℃ tunnel, sintering 1 ~ 5 hour makes it become dispersive symptom xln; 9. the secondary dispersion treatment according to the ratio of appeal acicular crystals: pure water=1:5 ~ 1:50, is put into reactor drum with needle-like crystal and pure water, and it is heated to 60 ~ 100 ℃, under 200 ~ 1000 Zhuan ∕ minutes rotating speed, stirs 1 ~ 5 hour; Then, slough moisture with whizzer, and with pure water washing till do not have a negatively charged ion; 10. will passing through acicular crystals that the secondary dispersion treatment crosses, to put into temperature be 100 ~ 300 ℃ baking oven baking 3 ~ 5 hours, makes its drying; 11. screening with 200 ~ 400 purpose sieves, is sieved to the acicular crystals of handling through redrying, obtains crystal whisker of hexa potassium titanate.Mainly there is following shortcoming in this method: technical process is complicated, is difficult to operation, is unfavorable for suitability for industrialized production.
In sum, need a kind of technical process simple, easy to operate at present, make things convenient for the preparation crystal whisker of hexa potassium titanate novel method of industrial applications.
Summary of the invention
It is simple that technical problem to be solved by this invention provides a kind of technical process, easy to operate, and yield is high, and cost is low, is suitable for the industrial method for preparing crystal whisker of hexa potassium titanate.
The technical solution adopted for the present invention to solve the technical problems is: the preparation method of crystal whisker of hexa potassium titanate comprises the steps:
A, general-100 purpose titaniferous materials and contain the potassium raw material according to TiO
2︰ K
2The mixed in molar ratio of O=3～6 is even;
B, the material after step a mixed place sintering 1～5h under 1100～1300 ℃ the temperature environment, and material is fully reacted;
C, the material behind the step b sintering is cooled off fast, water fully dissociates cooled material under 60～80 ℃ isoperibol then, filters, is drying to obtain the product crystal whisker of hexa potassium titanate at last.
The present invention dissociates and is meant that water with solubility alkalescence substance dissolves, then with the water removal, improves the process of product purity.For energy efficient, among the step c material behind the sintering being cooled off the medium that adopts usually fast is water coolant.
Wherein, the mole proportioning of raw material is among the aforesaid method step a: TiO
2︰ K
2O=5.2～5.8.
Wherein, the agglomerating temperature is 1150～1250 ℃ among the aforesaid method step b.
Wherein, the exsiccant temperature is 85～95 ℃ among the aforesaid method step c.
Wherein, the described titaniferous materials of aforesaid method is at least a in anatase titanium dioxide, rutile titanium dioxide or the metatitanic acid.
Wherein, the said potassium raw material that contains of aforesaid method is a salt of wormwood.
The invention has the beneficial effects as follows: it is even that the granularity that the present invention controls raw material helps batch mixing, and raw material can be reacted fully, improves yield; The control material molar ratio helps improving product gas purity; Strict control sintering temperature and time, make TiO
2Can change six potassium titanates as much as possible into, thereby improve yield; Sintered material is cooled off fast, make liquid phase lose the crystallization ability fully, all be converted into the vitreum under the low temperature, reduce crystal tiny in the product simultaneously, make the thing of product purer mutually, guarantee that product is six potassium titanates basically, improve purity and yield; Water dissociates cooled material, improves product purity; Under the comprehensive action of above measure, can fully improve product yield and purity, reduced in the art methods production process of presoma or the recrystallization switching process in later stage simultaneously, practiced thrift energy consumption, reduced production cost.The inventive method technical process is simple, and is with short production cycle, suitability for industrialized production.
Description of drawings
The SEM figure of the crystal whisker of hexa potassium titanate that Fig. 1 prepares for the embodiment of the invention one;
The SEM figure of the crystal whisker of hexa potassium titanate that Fig. 2 prepares for the embodiment of the invention two;
The XRD figure of the crystal whisker of hexa potassium titanate that Fig. 3 prepares for the embodiment of the invention two; X-coordinate 2 θ angles, unit °; Ordinate zou intensity, the counts of unit, the number of photons of promptly under 2 θ angles, collecting;
The SEM figure of the crystal whisker of hexa potassium titanate that Fig. 4 prepares for the embodiment of the invention three;
The XRD figure of the crystal whisker of hexa potassium titanate that Fig. 5 prepares for the embodiment of the invention three; X-coordinate 2 θ angles, unit °; Ordinate zou intensity, the counts of unit, the number of photons of promptly under 2 θ angles, collecting;
The SEM figure of the crystal whisker of hexa potassium titanate that Fig. 6 prepares for the embodiment of the invention four.
Embodiment
Through embodiment the present invention is further described below.
The preparation method of crystal whisker of hexa potassium titanate of the present invention comprises the steps:
A, general-100 purpose titaniferous materials and contain the potassium raw material according to TiO
2︰ K
2The mixed in molar ratio of O=3～6 is even;
B, the material after step a mixed place sintering 1～5h under 1100～1300 ℃ the temperature environment, and material is fully reacted;
C, the material behind the step b sintering is cooled off fast, water fully dissociates cooled material under 60～80 ℃ isoperibol then, filters, is drying to obtain the product crystal whisker of hexa potassium titanate at last.
Raw material granularity of the present invention-100 order, make titaniferous materials with contain the bulk volume basically identical of potassium raw material, it is even to help batch mixing, and raw material can be contacted fully.Raw material is according to TiO
2︰ K
2The mixed in molar ratio of O=3～6, proportioning are crossed the young pathbreaker and are generated two potassium titanates or potassium tetratitanate, and product purity is reduced, and the product proportioning is excessive, also can influence quality product.Sintering temperature of the present invention is too high, and crystal whisker products can reduce its length owing to high temperature fuses, and reaction temperature is spent to hang down and will be produced potassium tetratitanate impurity.The present invention needs sintered material is carried out chilling, if slow cooling, product will be transformed into potassium tetratitanate and two potassium titanates, and cooling can be avoided the generation of impurity fast.Under 60～80 ℃ isoperibol, dissociate, can guarantee the dissolving of soluble impurity.
Preferably, the mole proportioning of raw material is among the aforesaid method step a: TiO
2︰ K
2O=5.2～5.8.
Preferably, the agglomerating temperature is 1150～1250 ℃ among the aforesaid method step b.
Preferably, the exsiccant temperature is 85～95 ℃ among the aforesaid method step c.
Preferably, the described titaniferous materials of aforesaid method is at least a in anatase titanium dioxide, rutile titanium dioxide or the metatitanic acid.
Preferably, the said potassium raw material that contains of aforesaid method is a salt of wormwood.
Be further described through the embodiment specific embodiments of the invention below, but therefore protection scope of the present invention be not limited among the embodiment.
Embodiment one
With-100 purpose anatase titanium dioxides and Anhydrous potassium carbonate according to TiO
2: K
2The molar ratio weighing of O=5.5, and the two is mixed;
Above-mentioned mixed raw materials is encased in the crucible of suitable size, and crucible is put in 1150 ℃ the high temperature box type resistance furnace, stop 3h;
The above-mentioned product that sinters is taken out, put in the water container immediately and cool off;
After treating that product cooling is accomplished, from water, take out product, the product in the crucible is put into the beaker that contains 400ml water, and beaker put into temperature is set is that the product that stirs in the beaker fully dissociates crystal whisker products in 70 ℃ the water-bath, the time of dissociating is 2h;
After the above-mentioned product suction filtration that dissociates later, be finished product after putting into 90 ℃ drying in oven.
See the SEM figure (Fig. 1) of the crystal whisker of hexa potassium titanate for preparing, the length of crystal whisker of hexa potassium titanate is about 20 μ m, and diameter is about 4 μ m, and it is raw material that embodiment one adopts anatase titanium dioxide, m (TiO
2)=9.57g, end product quality are 9.38g, and product yield is 81.96%.(product yield of the present invention is the ratio of content of titanium dioxide in content of titanium dioxide and the raw material in the product)
Embodiment two
With-100 purpose anatase titanium dioxides and Anhydrous potassium carbonate according to TiO
2: K
2The molar ratio weighing of O=5.5, and the two is mixed;
Above-mentioned mixed raw materials is encased in the crucible of suitable size, and crucible is put in 1200 ℃ the high temperature box type resistance furnace, stop 3h;
The above-mentioned product that sinters is taken out, put in the water container immediately and cool off;
After treating that product cooling is accomplished, from water, take out product, the product in the crucible is put into the beaker that contains 400ml water, and beaker put into temperature is set is that the product that stirs in the beaker fully dissociates crystal whisker products in 70 ℃ the water-bath, the time of dissociating is 2h;
After the above-mentioned product suction filtration that dissociates later, be finished product after putting into 90 ℃ drying in oven.
See the SEM figure and the XRD figure (Fig. 2 and Fig. 3) of the crystal whisker of hexa potassium titanate that makes, see that main image is a crystal whisker of hexa potassium titanate in the product, do not exist remaining image to form from the XRD assay.Show that from SEM result the length of crystal whisker of hexa potassium titanate is 25 ~ 45 μ m, diameter is lower than 7 μ m, and it is raw material that embodiment two adopts anatase titanium dioxide, m (TiO
2)=9.57g, end product quality are 9.54g, and product yield is 83.36%.
Embodiment three
With-100 purpose anatase titanium dioxides and Anhydrous potassium carbonate according to TiO
2: K
2The molar ratio weighing of O=5.5, and the two is mixed;
Above-mentioned mixed raw materials is encased in the crucible of suitable size, and crucible is put in 1250 ℃ the high temperature box type resistance furnace, stop 3h;
The above-mentioned product that sinters is taken out, put in the water container immediately and cool off;
After treating that product cooling is accomplished, from water, take out product, the product in the crucible is put into the beaker that contains 400ml water, and beaker put into temperature is set is that the product that stirs in the beaker fully dissociates crystal whisker products in 70 ℃ the water-bath, the time of dissociating is 2h;
After the above-mentioned product suction filtration that dissociates later, be finished product after putting into 90 ℃ drying in oven.
See the SEM figure and the XRD figure (Fig. 4 and Fig. 5) of the crystal whisker of hexa potassium titanate that makes, analyze from XDR and see that the image in this product is crystal whisker of hexa potassium titanate entirely, do not have other image and form.Whisker length is greater than 34 μ m, and diameter is below 10 μ m, and it is raw material that embodiment three adopts anatase titanium dioxide, m (TiO
2)=9.57g, end product quality are 9.57g, and product yield is 83.62%.
Embodiment four
With-100 purpose anatase titanium dioxides and Anhydrous potassium carbonate according to TiO
2: K
2The molar ratio weighing of O=5.5, and the two is mixed;
Above-mentioned mixed raw materials is encased in the crucible of suitable size, and crucible is put in 1200 ℃ the high temperature box type resistance furnace, stop 3h.With 1150 ℃ of greenhouse coolings, stop 2h;
The above-mentioned product that sinters is taken out, put in the water container immediately and cool off;
After treating that product cooling is accomplished, from water, take out product, the product in the crucible is put into the beaker that contains 400ml water, and beaker put into temperature is set is that the product that stirs in the beaker fully dissociates crystal whisker products in 70 ℃ the water-bath, the time of dissociating is 2h;
After the above-mentioned product suction filtration that dissociates later, be finished product after putting into 90 ℃ drying in oven.
See the SEM figure (Fig. 6) of the crystal whisker of hexa potassium titanate for preparing, from figure, observe that the length of crystal whisker of hexa potassium titanate is 25 ~ 60 μ m, diameter is 1 ~ 5 μ m, and it is raw material that embodiment four adopts anatase titanium dioxide, m (TiO
2)=9.57g, end product quality are 9.66g, and product yield is 84.41%.
Can know from embodiment; The present invention adopts granularity, control material molar ratio, control sintering temperature and the time of control raw material, adopts water coolant to make the sintered material cooling fast, adopts water with measures such as cooled material dissociate; Fully improve product yield and purity; Reduce in the art methods production process of presoma or the recrystallization switching process in later stage simultaneously, practiced thrift energy consumption, reduced production cost.
Claims (6)
1. the preparation method of crystal whisker of hexa potassium titanate is characterized in that comprising the steps:
A, general-100 purpose titaniferous materials and contain the potassium raw material according to TiO
2︰ K
2The mixed in molar ratio of O=3～6 is even;
B, the material after step a mixed place sintering 1～5h under 1100～1300 ℃ the temperature environment, and material is fully reacted;
C, the material behind the step b sintering is cooled off fast, water fully dissociates cooled material under 60～80 ℃ isoperibol then, filters, is drying to obtain the product crystal whisker of hexa potassium titanate at last.
2. the preparation method of crystal whisker of hexa potassium titanate according to claim 1, it is characterized in that: the mole proportioning of raw material is among the step a: TiO
2︰ K
2O=5.2～5.8.
3. the preparation method of crystal whisker of hexa potassium titanate according to claim 1, it is characterized in that: the agglomerating temperature is 1150～1250 ℃ among the step b.
4. the preparation method of crystal whisker of hexa potassium titanate according to claim 1, it is characterized in that: the exsiccant temperature is 85～95 ℃ among the step c.
5. according to the preparation method of each described crystal whisker of hexa potassium titanate in the claim 1 to 4, it is characterized in that: described titaniferous materials is at least a in anatase titanium dioxide, rutile titanium dioxide or the metatitanic acid.
6. according to the preparation method of each described crystal whisker of hexa potassium titanate in the claim 1 to 4, it is characterized in that: the said potassium raw material that contains is a salt of wormwood.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103911664A (en) * | 2014-04-30 | 2014-07-09 | 潍坊赛富特汽车配件有限公司 | Synthesis method of crystal potassium hexatitanate |
| CN105040102A (en) * | 2015-05-15 | 2015-11-11 | 南通奥新电子科技有限公司 | Preparation method of potassium titanate whisker used in friction materials |
| EP2977353A4 (en) * | 2013-03-18 | 2016-11-16 | Toho Titanium Co Ltd | Method for producing potassium titanate |
| CN106119949A (en) * | 2016-06-23 | 2016-11-16 | 南通奥新电子科技有限公司 | The preparation method of a kind of high intensity potassium titanate crystal whisker and magnetic modification application thereof |
| CN106119950A (en) * | 2016-06-23 | 2016-11-16 | 南通奥新电子科技有限公司 | A kind of preparation method and applications of high intensity potassium titanate crystal whisker |
| CN112779602A (en) * | 2020-12-09 | 2021-05-11 | 南京工业大学 | Two-step sintering preparation method of potassium hexatitanate whisker |
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| CN1346803A (en) * | 2001-11-16 | 2002-05-01 | 无锡市宏杰轻工有限公司 | Process for preparing crystal wisker of potassium hexatitanate |
| CN101144186A (en) * | 2006-09-12 | 2008-03-19 | 上海秀普复合材料有限公司 | Method for synthesizing potassium hexatitanate crystal whisker |
| CN102304762A (en) * | 2011-09-21 | 2012-01-04 | 镇江忆诺唯记忆合金有限公司 | Preparation method of potassium hexatitanate whiskers |
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| CN1346803A (en) * | 2001-11-16 | 2002-05-01 | 无锡市宏杰轻工有限公司 | Process for preparing crystal wisker of potassium hexatitanate |
| CN101144186A (en) * | 2006-09-12 | 2008-03-19 | 上海秀普复合材料有限公司 | Method for synthesizing potassium hexatitanate crystal whisker |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2977353A4 (en) * | 2013-03-18 | 2016-11-16 | Toho Titanium Co Ltd | Method for producing potassium titanate |
| US9796598B2 (en) | 2013-03-18 | 2017-10-24 | Toho Titanium Co., Ltd. | Method for producing potassium titanate |
| CN103911664A (en) * | 2014-04-30 | 2014-07-09 | 潍坊赛富特汽车配件有限公司 | Synthesis method of crystal potassium hexatitanate |
| CN105040102A (en) * | 2015-05-15 | 2015-11-11 | 南通奥新电子科技有限公司 | Preparation method of potassium titanate whisker used in friction materials |
| CN105040102B (en) * | 2015-05-15 | 2018-03-27 | 南通奥新电子科技有限公司 | A kind of manufacture method of friction material potassium titanate crystal whisker |
| CN106119949A (en) * | 2016-06-23 | 2016-11-16 | 南通奥新电子科技有限公司 | The preparation method of a kind of high intensity potassium titanate crystal whisker and magnetic modification application thereof |
| CN106119950A (en) * | 2016-06-23 | 2016-11-16 | 南通奥新电子科技有限公司 | A kind of preparation method and applications of high intensity potassium titanate crystal whisker |
| CN112779602A (en) * | 2020-12-09 | 2021-05-11 | 南京工业大学 | Two-step sintering preparation method of potassium hexatitanate whisker |
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| CN102839424B (en) | 2015-06-17 |
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