CN102839424B - Method for preparing potassium hexatitanate whisker - Google Patents
Method for preparing potassium hexatitanate whisker Download PDFInfo
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- CN102839424B CN102839424B CN201210374730.9A CN201210374730A CN102839424B CN 102839424 B CN102839424 B CN 102839424B CN 201210374730 A CN201210374730 A CN 201210374730A CN 102839424 B CN102839424 B CN 102839424B
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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, transverse section is close to consistent, and external and internal compositions height is complete, and length-to-diameter ratio is generally more than 5 ~ 1000, diameter is usually between 200nm ~ 100 μm, but the diameter of whiskers with special property is generally between 1 ~ 10 μm.Potassium titanate crystal whisker is also potassium titanate fiber, is white needle-like crystals, and density is 3.2g/cm
3, there is excellent thermotolerance, chemical stability and chemical resistance, there is high surface strength (>700kg/mm
2) and high Young's modulus (>2800kg/mm
2).Be synthesized in the fifties by the E.I.Du Pont Company of the U.S. at first, first as heat-resisting, heat insulation starting material exploitation, be applied to universe and military aspect.At present, potassium titanate crystal whisker is mainly used as the absorbing material etc. of the strongthener of macromolecular material, high-temperature resistant coating, electro-conductive fiber and radioactive substance.Applying maximum in potassium titanate crystal whisker is crystal whisker of hexa potassium titanate (K
2ti
6o
13), it is the compound that potassium titanate crystal whisker series is the most stable, and whisker excellent property, does not react with diluted acid, diluted alkaline, salts solution and organic solvent.
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 only has sintering process can be widely used in the suitability for industrialized production of crystal whisker of hexa potassium titanate.By literature search, application number be 200610031042.7 Chinese patent disclose a kind of production method of crystal whisker of hexa potassium titanate, its main technique is: 1. by titaniferous materials and containing potassium raw material according to TiO
2: K
2the ratio of O=1.9 ~ 2.0 mol ratio weighs; 2. the above-mentioned raw material mixed is entered into the High Temperature Furnaces Heating Apparatus of 900 ~ 1300 DEG C, stop 30 ~ 90 minutes, make raw mixture become molten mass; 3. above-mentioned molten mass is taken out, in the quenching of professional quenching machine, the fine powder making it be dispersed into particle diameter to be less than 1mm; 4. by the ratio volume of above-mentioned fine powder in solid-to-liquid ratio 1:15 to 1:5, enter in the hydrothermal reaction device of 90 ~ 99 DEG C, the sulphuric acid soln with 1 ~ 15% controls, between the pH value 10 ~ 12 of solution, to react 90 ~ 360 minutes; 5. the solution in above-mentioned reactor is carried out solid-liquid separation, liquid portion is accumulated separately, is pure basic sulfate potassium solution; 6., by the deionized water repetitive scrubbing of above-mentioned solid part with 1 ~ 4 DEG C, wash most sulfate ion (SO
4 2+), washing water turn back in reactor and recycle; 7., by dry for the wet feed drawn off in above-mentioned filter, slough surface water; 8. by the above-mentioned material sloughing surface water, stop 90 ~ 360 minutes at 600 ~ 1000 DEG C, complete recrystallization conversion, be cooled to room temperature and be finished product.There is following shortcoming in the method: 1. processing step is complicated, is unfavorable for that industrialization is produced; 2. life cycle of the product is long; 3. need recrystallization to change, fuel expends height, and production cost is too high; 4. there will be caking phenomenon in recrystallization sintering process, need to carry out crushing process specially, then sieve classification, such Mechanical Crushing, the fracture of part whisker will inevitably be caused, have impact on the homogeneity of potassium titanate crystal whisker.5.1 ~ 4 DEG C of deionized water repetitive scrubbings, condition is harsher, is difficult to realize in Panzhihua Region.In addition temperature is lower, and the filtration of basic solution is lower, causes the efficiency of producing to reduce.
Application number be 03116985.6 Chinese patent disclose the preparation method of another kind of crystal whisker of hexa potassium titanate.Its main technique is:
1. preparation of raw material: TiO amounted to into by raw material
2with K
2o, by TiO
2∕ K
2o=2 ~ 6mol, preferably 4 ~ 6mol, add water mixing, and wherein the weight percent of water content is 50 ~ 95%; 2. precursor preparation: adopt spraying dry or rotary flashing drying, stock suspension is made the more uniform spherical precursors of size; 3. react: precursors loaded in crucible or be pre-formed as base substrate, sinter 0.5 ~ 12 hour at 1100 DEG C ~ 1300 DEG C; 4. separate fine: sintered product is soaked and 5 ~ 15 times, in the deionized water of 50 ~ 100 DEG C 2 ~ 10 hours and stir solution and knit; 5. filter, washing; 6: dry: by washed filter cake 150 DEG C of dryings 2 hours, obtained crystal whisker of hexa potassium titanate.There is following shortcoming in this technique: the production cycle is long; The preparation of presoma is more complicated, and production technique is more complicated.
Application number be 201110289501.2 Chinese patent disclose the preparation method of another kind of crystal whisker of hexa potassium titanate, its main technique is: by K
2cO
3with metatitanic acid (containing TiO
240wt%) in molar ratio [n(K2CO3) ∕ n(TiO2)] for 1:3.5 at room temperature mixes, put into 150 DEG C of loft drier, timing agitation, time of drying is 24h, obtains precursors; In 250ml crucible, put into 100g presoma, roasting at 150 DEG C, 400 DEG C, 600 DEG C, 800 DEG C, 1000 DEG C, 1150 DEG C in retort furnace, roasting time gets 2h respectively, 4h, 7h, 10h; Be that the different time products therefrom of 1000 DEG C, 1150 DEG C roastings carries out Soaking treatment 10h in azeotropic water-bath to temperature, product is suction filtration after Soaking treatment, puts into after 150 DEG C of loft drier dry 24h and obtains crystal whisker of hexa potassium titanate product.The main shortcoming of the method is: life cycle of the product is long; Complex manufacturing.
Application number be 01134183.1 Chinese patent be that the production of crystal whisker of hexa potassium titanate provides a kind of method, the Production Flow Chart of the method is: 1. mix, according to titanium source (TiO
2): potassium source (K
2the mol ratio of O)=1.9 ~ 2.5, puts into ball mill by titanium source and potassium source and mixes, make compound; 2. sinter, above-mentioned compound is put into box-type furnace or tunnel furnace that temperature is 900 ~ 1200 DEG C, sinter 0.5 ~ 4 hour, make it sinter molten mass into; 3. use twin rollers to carry out quick refrigeration to above-mentioned molten mass, its method is, in two rollers of twin rollers, pass into recirculated cooling water, is, after above-mentioned molten mass enters from twin rollers top, while quenching, be squeezed into thin slice by two rollers; 4. dispersion treatment, according to above-mentioned thin slice: the ratio of pure water=1:5 ~ 1:50, puts into reactor by above-mentioned thin slice and pure water, and is heated to 60 ~ 100 DEG C, and within every 10 ~ 20 minutes, adding the diluted acid that concentration is 3 ~ 20%, is pH value>=9 of solution; Meanwhile, stir 1 ~ 5 hour under 200 ~ 1000 turns of rotating speeds of ∕ minute, make suspension; 5. be separated, being separated suspension with whizzer, the moisture of going out wherein, is that it becomes meal; 6. wash, meal is put into whizzer, and adds pure water, meal is washed; 7. dry, appeal meal is put into the baking oven that temperature is 100 ~ 300 DEG C, toasts 3 ~ 5 hours, make it dry; 8. high temperature crystallization sintering, is placed in through dried meal the tunnel furnace that temperature is 900 ~ 1200 DEG C, sinters 1 ~ 5 hour, become the symptom xln of dispersion; 9. twice dispersing process, according to appeal acicular crystals: the ratio of pure water=1:5 ~ 1:50, puts into reactor by needle-like crystal and pure water, and is heated to 60 ~ 100 DEG C to it, stir 1 ~ 5 hour under 200 ~ 1000 turns of rotating speeds of ∕ minute; Then, slough moisture with whizzer, and with pure water to without negatively charged ion; 10. the acicular crystals through twice dispersing process is put into the baking oven baking 3 ~ 5 hours that temperature is 100 ~ 300 DEG C, make it dry; 11. screenings, with 200 ~ 400 object sieves, sieve to the acicular crystals through redrying process, obtain crystal whisker of hexa potassium titanate.Mainly there is following shortcoming in the 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, what facilitate industrial applications prepares crystal whisker of hexa potassium titanate novel method.
Summary of the invention
It is simple that technical problem to be solved by this invention is to provide a kind of technical process, and easy to operate, yield is high, and cost is low, is suitable for the industrial method 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, by-100 object titaniferous materials and containing potassium raw material according to TiO
2︰ K
2the mixed in molar ratio of O=3 ~ 6 is even;
B, step a is mixed after material be placed in sintering 1 ~ 5h under the temperature environment of 1100 ~ 1300 DEG C, material is fully reacted;
C, by step b sinter after material cool fast, then with water, cooled material fully dissociated under the isoperibol of 60 ~ 80 DEG C, finally filters, be drying to obtain product crystal whisker of hexa potassium titanate.
The present invention dissociates and refers to and to be dissolved by soluble alkali materials with water, then removes with water, improves the process of product purity.In order to energy efficient, in step c, the material after sintering being cooled the medium usually adopted fast is water coolant.
Wherein, the mol ratio of aforesaid method step a Raw is: TiO
2︰ K
2o=5.2 ~ 5.8.
Wherein, the temperature sintered in aforesaid method step b is 1150 ~ 1250 DEG C.
Wherein, dry in aforesaid method step c temperature is 85 ~ 95 DEG C.
Wherein, the titaniferous materials described in aforesaid method is at least one in anatase titanium dioxide, rutile titanium dioxide or metatitanic acid.
Wherein, containing potassium raw material described in aforesaid method is salt of wormwood.
The invention has the beneficial effects as follows: the granularity that the present invention controls raw material is conducive to batch mixing evenly, raw material is reacted fully, improves yield; Control material molar ratio, be conducive to the purity improving product; Strict control sintering temperature and time, make TiO
2potassium hexatitanate can be changed into as much as possible, thus improve yield; Sintered material is cooled fast, makes liquid phase lose crystallization ability completely, be all converted into the vitreum under low temperature, reduce crystal tiny in product simultaneously, make the thing of product purer mutually, ensure that product is potassium hexatitanate substantially, improve purity and yield; With water, cooled material is carried out dissociation, improve product purity; Under the comprehensive action of above measure, can fully improve product yield and purity, decrease the production process of presoma in art methods or the recrystallization switching process in later stage simultaneously, saved energy consumption, reduced production cost.The inventive method technical process is simple, with short production cycle, and suitability for industrialized is produced.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the crystal whisker of hexa potassium titanate that the embodiment of the present invention one prepares;
Fig. 2 is the SEM figure of the crystal whisker of hexa potassium titanate that the embodiment of the present invention two prepares;
Fig. 3 is the XRD figure of the crystal whisker of hexa potassium titanate that the embodiment of the present invention two prepares; X-coordinate 2 θ angle, unit °; Ordinate zou intensity, unit counts, the number of photons namely collected under 2 θ angles;
Fig. 4 is the SEM figure of the crystal whisker of hexa potassium titanate that the embodiment of the present invention three prepares;
Fig. 5 is the XRD figure of the crystal whisker of hexa potassium titanate that the embodiment of the present invention three prepares; X-coordinate 2 θ angle, unit °; Ordinate zou intensity, unit counts, the number of photons namely collected under 2 θ angles;
Fig. 6 is the SEM figure of the crystal whisker of hexa potassium titanate that the embodiment of the present invention four prepares.
Embodiment
Below by embodiment, the present invention is further illustrated.
The preparation method of crystal whisker of hexa potassium titanate of the present invention, comprises the steps:
A, by-100 object titaniferous materials and containing potassium raw material according to TiO
2︰ K
2the mixed in molar ratio of O=3 ~ 6 is even;
B, step a is mixed after material be placed in sintering 1 ~ 5h under the temperature environment of 1100 ~ 1300 DEG C, material is fully reacted;
C, by step b sinter after material cool fast, then with water, cooled material fully dissociated under the isoperibol of 60 ~ 80 DEG C, finally filters, be drying to obtain product crystal whisker of hexa potassium titanate.
Raw material granularity-100 order of the present invention, makes titaniferous materials and basically identical containing the bulk volume of potassium raw material, is conducive to batch mixing even, raw material is contacted fully.Raw material is according to TiO
2︰ K
2the mixed in molar ratio of O=3 ~ 6, proportioning is crossed young pathbreaker and is generated two potassium titanates or potassium tetratitanate, and product purity is reduced, and product proportioning is excessive, also can affect quality product.Sintering temperature of the present invention is too high, and crystal whisker products can fuse due to high temperature, reduces its length, and temperature of reaction is too low will produce potassium tetratitanate impurity.The present invention need carry out chilling to sintered material, if slow cooling, product will be transformed into potassium tetratitanate and two potassium titanates, and cooling can avoid the generation of impurity fast.Dissociate under the isoperibol of 60 ~ 80 DEG C, the dissolving of soluble impurity can be guaranteed.
Preferably, the mol ratio of aforesaid method step a Raw is: TiO
2︰ K
2o=5.2 ~ 5.8.
Preferably, the temperature sintered in aforesaid method step b is 1150 ~ 1250 DEG C.
Preferably, dry in aforesaid method step c temperature is 85 ~ 95 DEG C.
Preferably, the titaniferous materials described in aforesaid method is at least one in anatase titanium dioxide, rutile titanium dioxide or metatitanic acid.
Preferably, containing potassium raw material described in aforesaid method is salt of wormwood.
Below by embodiment, the specific embodiment of the present invention is further described, but not therefore by protection scope of the present invention restriction in one embodiment.
Embodiment one
By-100 object 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;
The above-mentioned raw material mixed is encased in the crucible of suitable size, and crucible is put in the high temperature box type resistance furnace of 1150 DEG C, stop 3h;
The above-mentioned product sintered is taken out, puts in water container immediately and cool;
After treating that product has cooled, from water, take out product, the product in crucible is put into the beaker containing 400ml water, and beaker to be put into set temperature be in the water-bath of 70 DEG C, the product stirred in beaker makes crystal whisker products fully dissociate, and Dissociation time is 2h;
After the above-mentioned product suction filtration dissociating later, after putting into the drying in oven of 90 DEG C, be finished product.
See SEM figure (Fig. 1) of the crystal whisker of hexa potassium titanate prepared, the length of crystal whisker of hexa potassium titanate is about 20 μm, and diameter is about 4 μm, and embodiment one adopts anatase titanium dioxide to be raw material, m(TiO
2)=9.57g, end product quality is 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 in product and raw material)
Embodiment two
By-100 object 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;
The above-mentioned raw material mixed is encased in the crucible of suitable size, and crucible is put in the high temperature box type resistance furnace of 1200 DEG C, stop 3h;
The above-mentioned product sintered is taken out, puts in water container immediately and cool;
After treating that product has cooled, from water, take out product, the product in crucible is put into the beaker containing 400ml water, and beaker to be put into set temperature be in the water-bath of 70 DEG C, the product stirred in beaker makes crystal whisker products fully dissociate, and Dissociation time is 2h;
After the above-mentioned product suction filtration dissociating later, after putting into the drying in oven of 90 DEG C, be finished product.
See SEM figure and the XRD figure (Fig. 2 and Fig. 3) of obtained crystal whisker of hexa potassium titanate, see from XRD assay, in product, main image is crystal whisker of hexa potassium titanate, there is not remaining image composition.From the display of SEM result, the length of crystal whisker of hexa potassium titanate is 25 ~ 45 μm, and diameter is lower than 7 μm, and embodiment two adopts anatase titanium dioxide to be raw material, m(TiO
2)=9.57g, end product quality is 9.54g, and product yield is 83.36%.
Embodiment three
By-100 object 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;
The above-mentioned raw material mixed is encased in the crucible of suitable size, and crucible is put in the high temperature box type resistance furnace of 1250 DEG C, stop 3h;
The above-mentioned product sintered is taken out, puts in water container immediately and cool;
After treating that product has cooled, from water, take out product, the product in crucible is put into the beaker containing 400ml water, and beaker to be put into set temperature be in the water-bath of 70 DEG C, the product stirred in beaker makes crystal whisker products fully dissociate, and Dissociation time is 2h;
After the above-mentioned product suction filtration dissociating later, after putting into the drying in oven of 90 DEG C, be finished product.
See SEM figure and the XRD figure (Fig. 4 and Fig. 5) of obtained crystal whisker of hexa potassium titanate, analyze from XDR and see, the image in this product is crystal whisker of hexa potassium titanate entirely, forms without other image.Whisker length is greater than 34 μm, and diameter is below 10 μm, and embodiment three adopts anatase titanium dioxide to be raw material, m(TiO
2)=9.57g, end product quality is 9.57g, and product yield is 83.62%.
Embodiment four
By-100 object 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;
The above-mentioned raw material mixed is encased in the crucible of suitable size, and crucible is put in the high temperature box type resistance furnace of 1200 DEG C, stop 3h.By greenhouse cooling 1150 DEG C, stop 2h;
The above-mentioned product sintered is taken out, puts in water container immediately and cool;
After treating that product has cooled, from water, take out product, the product in crucible is put into the beaker containing 400ml water, and beaker to be put into set temperature be in the water-bath of 70 DEG C, the product stirred in beaker makes crystal whisker products fully dissociate, and Dissociation time is 2h;
After the above-mentioned product suction filtration dissociating later, after putting into the drying in oven of 90 DEG C, be finished product.
See SEM figure (Fig. 6) of the crystal whisker of hexa potassium titanate prepared, observe from figure, the length of crystal whisker of hexa potassium titanate is 25 ~ 60 μm, and diameter is 1 ~ 5 μm, and embodiment four adopts anatase titanium dioxide to be raw material, m(TiO
2)=9.57g, end product quality is 9.66g, and product yield is 84.41%.
From embodiment, the present invention adopts the granularity of control raw material, controls material molar ratio, controls sintering temperature and time, water coolant is adopted to make sintered material cool fast, adopt water that cooled material is carried out the measures such as dissociation, abundant raising product yield and purity, decrease the production process of presoma in art methods or the recrystallization switching process in later stage simultaneously, saved energy consumption, reduced production cost.
Claims (5)
1. the preparation method of crystal whisker of hexa potassium titanate, is characterized in that comprising the steps:
A, by-100 object titaniferous materials and containing potassium raw material according to TiO
2︰ K
2the mixed in molar ratio of O=5.2 ~ 5.8 is even;
B, step a is mixed after material be placed in sintering 1 ~ 5h under the temperature environment of 1100 ~ 1300 DEG C, material is fully reacted;
C, by step b sinter after material cool fast, then with water, cooled material fully dissociated under the isoperibol of 60 ~ 80 DEG C, finally filters, be drying to obtain product crystal whisker of hexa potassium titanate.
2. the preparation method of crystal whisker of hexa potassium titanate according to claim 1, is characterized in that: the temperature sintered in step b is 1150 ~ 1250 DEG C.
3. the preparation method of crystal whisker of hexa potassium titanate according to claim 1, is characterized in that: temperature dry in step c is 85 ~ 95 DEG C.
4. the preparation method of crystal whisker of hexa potassium titanate according to any one of claim 1 to 3, is characterized in that: described titaniferous materials is at least one in anatase titanium dioxide, rutile titanium dioxide or metatitanic acid.
5. the preparation method of crystal whisker of hexa potassium titanate according to any one of claim 1 to 3, is characterized in that: described is salt of wormwood containing potassium raw material.
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| JP6329526B2 (en) | 2013-03-18 | 2018-05-23 | 東邦チタニウム株式会社 | Method for producing potassium titanate |
| CN103911664B (en) * | 2014-04-30 | 2016-06-29 | 潍坊中晶新材料科技有限公司 | A kind of synthetic method of lenticular potassium hexatitanate |
| 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 |
| CN106119950B (en) * | 2016-06-23 | 2018-08-17 | 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 |
| CN106119949B (en) * | 2016-06-23 | 2018-08-17 | 南通奥新电子科技有限公司 | A kind of preparation method and its magnetic modification application of high intensity potassium titanate crystal whisker |
| CN112779602B (en) * | 2020-12-09 | 2022-11-18 | 南京工业大学 | Two-step sintering preparation method of potassium hexatitanate whisker |
Citations (3)
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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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2012
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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