CN101363135B - Synthesis method of potassium hexatitanate whisker - Google Patents
Synthesis method of potassium hexatitanate whisker Download PDFInfo
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- CN101363135B CN101363135B CN2007100447706A CN200710044770A CN101363135B CN 101363135 B CN101363135 B CN 101363135B CN 2007100447706 A CN2007100447706 A CN 2007100447706A CN 200710044770 A CN200710044770 A CN 200710044770A CN 101363135 B CN101363135 B CN 101363135B
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Abstract
The invention discloses a preparation method of potassium hexatitanate crystal whiskers, which adopts a technique of melting and quenching for synthesis and has convenient and feasible process flow. First, raw materials containing titanium and gallium are mixed with fluxing agent, sintered in an elevated temperature vessel, taken out after being melted, and quenched on special quenching equipment, thereby producing well-proportioned fine powder with particle diameter less than 1mm. Then, the powder is put into a reactor with hot water; the quantity of potassium ion release is controlled by controlling the acidity of the solution. While the reaction is finished, the product is filtered, washed by deionized water at the temperature of 20 to 40 DEG C repeatedly, soaked by surface active agent, and sintered directly after being filtered, thereby obtaining the end product. There is no pollution throughout the process. The synthetic potassium hexatitanate crystal whiskers synthesized by the method have the advantages of few un-needle-shaped particles, low cost, low thermal conductivity, high infrared reflectivity and good sound-absorbing property at high temperature, with the average length of the crystal whiskers being 5 to 30um and the average diameter being 0.5-3um, can be used as reinforcing material, friction material, thermal insulation material and the like, and have a yield higher than 97%.
Description
Technical field
The invention belongs to a kind of method of manufacture of inorganic salt whisker, particularly the method for manufacture of crystal whisker of hexa potassium titanate.
Background technology
In the prior art, one Chinese patent application discloses a kind of method of producing crystal whisker of hexa potassium titanate for No. 200610029750.7, and its technology is: 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 mixed enters into 900～1300 ℃ High Temperature Furnaces Heating Apparatus after evenly, and the quenching of special-purpose quenching machine becomes the fine powder of particle diameter less than 1mm; Advance in the ratio of solid-to-liquid ratio 1:15 to 1:5 in 90～99 ℃ the hydrothermal reaction device; Solid-liquid separation, solid part are washed most sulfate ion (SO with 1～4 ℃ of deionized water repetitive scrubbing
4 2-), drying is sloughed surface water; Stopped 90～360 minutes down at 600～1000 ℃, accomplish the recrystallization conversion, be finished product after being cooled to room temperature.
The shortcoming of this crystal whisker of hexa potassium titanate compound method is:
1,1～4 ℃ of deionized water repetitive scrubbing, condition are a bit harsh, especially are difficult to summer realize.Temperature is low more in addition, and the filtering rate of basic soln is low more, the reduction of the efficient that causes producing.
2, caking phenomenon can be occurred in the recrystallization sintering process, crushing process need be carried out specially, sieve classification then, such Mechanical Crushing must cause the fracture of part whisker, has influenced the homogeneity of potassium titanate crystal whisker.
3, drying, the process of taking off surface water is the process of more complicated, and temperature rise rate can not be too fast, otherwise hard blocks can occur, and temperature rise rate is low excessively, has influence on the output of product, and in addition, this process is the bigger process of energy waste.
Summary of the invention
The chemical property of crystal whisker of hexa potassium titanate is more stable; Satisfactory mechanical property as strongthener and friction materials, is had many uses; Especially enjoying favor with low thermal conductivity, high infrared reflection rate and the sound absorption qualities under the high temperature, is very good insulating refractory.
The present invention uses scorification, is intended to improve some defectives of existing scorification, further shortened process; Reduce synthetic energy consumption; When improving this method yield, improve the quality of crystal whisker of hexa potassium titanate, and further reduce the synthetic cost of crystal whisker of hexa potassium titanate.
The present invention provides a kind of process synthetic method of new crystal whisker of hexa potassium titanate.
The synthetic route of crystal whisker of hexa potassium titanate
(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, fusing assistant is poured on load weighted raw material together by 1～3% weighing of gross weight, does not need special mixing;
(2) above-mentioned raw materials is entered into 900～1300 ℃ High Temperature Furnaces Heating Apparatus, stopped 30～90 minutes, make the raw material miscellany become molten mass;
(3) above-mentioned molten mass is taken out, quenching on the special-purpose quenching machine that runs up makes it be dispersed into the fine powder of evengranular diameter less than 1mm; What formed this moment is two potassium titanate crystal whisker groups;
(4) with the ratio of above-mentioned fine powder in solid-to-liquid ratio 1:15 to 1:5; Enter into 90～99 ℃ of hydrothermal reaction devices; Use liquid meter adding concentration is 1～15% sulfuric acid, the acidity of control solution, and the pH value that makes solution is between 10～12; Control the potassium ion stripping quantity with these means, reacted 90～240 minutes; Use sulfuric acid in the reaction process, the excessive alkali that neutralizes, the energy that this thermopositive reaction provides makes two potassium titanate crystal whiskers group be dispersed into single whisker more easily;
(5) solution in the above-mentioned reactor drum is entered into filter, carry out solid-liquid separation, liquid portion is accumulated separately, for pure alkaline potassium sulfate solution, waits until special disposal, is a kind of agricultural high-quality potash fertilizer;
(6), wash most sulfate ion (SO with the deionized water wash of above-mentioned solid part with 20～40 ℃
4 2-), do not have muddy with the check of 1% barium chloride solution; Washing water turn back in the reactor drum and recycle; Fully invade bubble after 5 minutes with the aqueous solution that contains 1～5% water soluble surfactant active again, the hydraulic pressure in the filter is done, the aqueous solution that contains promoting agent reclaims continued and uses;
(7) with the wet feed that draws off in the above-mentioned filter, directly get into tunnel, stopped 100～600 minutes down at 100～1000 ℃, accomplish the recrystallization conversion, be finished product after being cooled to room temperature.
Titaniferous materials is meant one or both the mixing in various model white titanium pigments, anatase octahedrite, the brookite etc.
Contain one or both the mixing that the potassium raw material is meant Anhydrous potassium carbonate, Carbon Dioxide hydrogen potassium, saltpetre, Pottasium Hydroxide etc.
In described (1) technology, with titaniferous materials with contain the ratio weighing in molar ratio of potassium raw material, it is mixed together evenly to add fusing assistant; Fusing assistant is pressed 1～3% weighing of titanium, potassium raw material and fusing assistant total amount;
Described fusing assistant is meant one or both the mixing of vitriolate of tartar, saltpetre, boric acid, borax, boric anhydride, Repone K, potassium silicate, silicon-dioxide.The effect that reduces material system miscellany fusing point is played in the adding of fusing assistant, simultaneously under the high temperature various containers being played corrosion inhibition, and is of value to the dispersion of the single whisker of potassium titanate.
Described tensio-active agent is meant like silane coupling agent class etc.; Can be dissolved in the water or be dissolved in the absolute ethyl alcohol; After the potassium titanate crystal whisker surface adsorption, enter into the recrystallization sintering during stage, tensio-active agent partly or entirely decomposes; Caking or agglomerating phenomenon do not occur after making recrystallization, and do not influence the performance of potassium titanate crystal whisker.
By synthetic crystal whisker of hexa potassium titanate of the present invention, non-elongated piece is few, and cost is low; Thermal conductivity is little, and the infrared reflection rate is higher, and the high temperature sound absorption qualities is good; The mean length of whisker is 5～30 microns, and 0.5～3 micron of mean diameter can be used as strongthener, friction materials, lagging material etc.The crystal whisker of hexa potassium titanate that is synthesized of method thus, its yield is greater than 97%.
Embodiment
Embodiment 1
(1) with anatase thpe white powder and Anhydrous potassium carbonate according to TiO
2: K
2The ratio weighing of O=1.9 mol ratio, and evenly mixed with fusing assistant boric acid, and fusing assistant boric acid is pressed 3% weighing of anatase thpe white powder and Anhydrous potassium carbonate and fusing assistant boric acid total amount, load weighted raw material is poured on mixed together;
(2) above-mentioned raw materials is entered into 1100 ℃ High Temperature Furnaces Heating Apparatus, stopped 60 minutes, make the raw material miscellany become molten mass;
(3) above-mentioned molten mass is taken out, quenching on the special-purpose quenching machine that runs up makes it be dispersed into the fine powder that evengranular particle diameter is 0.5mm; What formed this moment is two potassium titanate crystal whisker groups
(4) with the ratio of above-mentioned fine powder in solid-to-liquid ratio 1:10, enter into 90 ℃ hydrothermal reaction device, the pH value of the sulphuric acid soln control solution of use 5% is 10～12, reacts 180 minutes;
(5) solution in the above-mentioned reactor drum is entered into filter, carry out solid-liquid separation, liquid portion is accumulated separately, is alkaline potassium sulfate solution, waits until special disposal;
(6) with the deionized water repetitive scrubbing of above-mentioned solid part, wash most sulfate ion (SO with 40 ℃
4 2-), there is not muddiness with the check of 1% barium chloride solution, washing water turn back in the reactor drum and recycle; To contain 2% KH550 aqueous solution soaking 5 minutes, filter, and contain the KH560 aqueous solution and recycle;
(7) with the material that draws off in the above-mentioned filter, get into tunnel, stopped 400 minutes down at 100～800 ℃, accomplish the recrystallization conversion, be the crystal whisker of hexa potassium titanate finished product after being cooled to room temperature.Mean diameter 0.5～2.0 μ of crystal whisker of hexa potassium titanate, mean length 10～15 μ, yield 97%.
Embodiment 2:
(1) with anatase octahedrite and Carbon Dioxide hydrogen potassium according to TiO
2: K
2The ratio weighing of O=2.0 mol ratio and fusing assistant vitriolate of tartar are evenly mixed, and the fusing assistant vitriolate of tartar is pressed 2% weighing of anatase octahedrite and Carbon Dioxide hydrogen potassium and fusing assistant vitriolate of tartar total amount;
(2) above-mentioned mixed uniform raw material is entered into 1050 ℃ High Temperature Furnaces Heating Apparatus, stopped 40 minutes, make the raw material miscellany become molten mass;
(3) above-mentioned molten mass is taken out, quenching on the special-purpose quenching machine that runs up makes it be dispersed into the fine powder of evengranular particle diameter less than 0.3mm; What formed this moment is two potassium titanate crystal whisker groups;
(4) with the ratio of above-mentioned fine powder in solid-to-liquid ratio 1:8, enter into 95 ℃ hydrothermal reaction device, using 4% sulphuric acid soln control pH value of solution value is 10～12, reacts 160 minutes;
(5) solution in the above-mentioned reactor drum is entered into filter, carry out solid-liquid separation, liquid portion is accumulated separately, is pure alkaline potassium sulfate solution, waits until special disposal;
(6) with above-mentioned solid part with 30 ℃ of deionized water repetitive scrubbings, wash most sulfate ion (SO
4 2-), use 1%BaCl
2The solution check does not have muddy, and washing water turn back in the reactor drum and recycle; With containing 2% KH550 aqueous solution soaking 5 minutes, filter, contain the KH560 aqueous solution and recycle;
(7) with the material that draws off in the above-mentioned filter, get into tunnel, stopped 340 minutes down at 100～900 ℃, accomplish the recrystallization conversion, be the crystal whisker of hexa potassium titanate finished product after being cooled to room temperature.Mean diameter 0.6～1.5 μ of crystal whisker of hexa potassium titanate, mean length 5～10 μ, yield 97.4%.
Claims (5)
1. the compound method of a crystal whisker of hexa potassium titanate, technical process is following:
(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, the amount of fusing assistant is by 1～3% weighing of gross weight; Fusing assistant is selected one or both the mixing of vitriolate of tartar, saltpetre, boric acid, borax, boric anhydride, Repone K, potassium silicate, silicon-dioxide for use;
(2) above-mentioned raw materials is entered into 900～1300 ℃ High Temperature Furnaces Heating Apparatus, stopped 30～90 minutes, make the raw material miscellany 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 special-purpose quenching machine;
(4) with above-mentioned fine powder in 1: 15 to 1: 5 ratio of solid-to-liquid ratio, advance in 90～99 ℃ the hydrothermal reaction device, between the pH value 10～12 of sulphuric acid soln control solution, reacted 90～240 minutes with 1～15%;
(5) 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 above-mentioned solid part with 20～40 ℃ of deionized water repetitive scrubbings, wash most sulfate ion, washing water turn back in the reactor drum and recycle; After fully soaking 5 minutes with the aqueous solution that contains 1～5% water soluble surfactant active again, the hydraulic pressure in the filter is done, the aqueous solution that contains promoting agent reclaims continued and uses;
(7) with the material that draws off in the above-mentioned filter, directly advance tunnel, stopped 100～600 minutes down at 100～1000 ℃, accomplish the recrystallization conversion, be finished product after being cooled to room temperature.
2. by the compound method of the described a kind of crystal whisker of hexa potassium titanate of claim 1, it is characterized in that titaniferous materials is meant one or both the mixing in various model white titanium pigments, anatase octahedrite, the brookite.
3. by the compound method of claim 1 or 2 described crystal whisker of hexa potassium titanate, it is characterized in that containing one or both the mixing that the potassium raw material is meant Anhydrous potassium carbonate, Carbon Dioxide hydrogen potassium, saltpetre, Pottasium Hydroxide.
4. by the compound method of the described crystal whisker of hexa potassium titanate of claim 3, it is characterized in that, in described (1) technology, with titaniferous materials with contain the ratio weighing in molar ratio of potassium raw material, it is evenly mixed together to add fusing assistant; Fusing assistant is pressed 1～3% weighing of titanium, potassium raw material and fusing assistant total amount;
Described fusing assistant is meant one or both the mixing of vitriolate of tartar, saltpetre, boric acid, borax, boric anhydride, Repone K, potassium silicate, silicon-dioxide.
5. by the compound method of the described crystal whisker of hexa potassium titanate of claim 1, it is characterized in that in described (6) technology, described tensio-active agent is meant silane coupling agent.
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| CN2007100447706A CN101363135B (en) | 2007-08-10 | 2007-08-10 | Synthesis method of potassium hexatitanate whisker |
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| CN101363135B true CN101363135B (en) | 2012-07-11 |
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Families Citing this family (7)
| 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 |
| 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 |
| 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 |
| CN104894636B (en) * | 2015-04-29 | 2017-10-27 | 华东理工大学 | The preparation method of eight potassium titanate crystal whiskers |
| CN106637408A (en) * | 2016-12-23 | 2017-05-10 | 张家港大塚化学有限公司 | Preparation method of acicular short fiber composite potassium hexatitanate crystal whisker |
| CN108315822B (en) * | 2018-02-10 | 2020-12-18 | 罗旭 | Method for preparing potassium hexatitanate whisker by epoxy-driven one-step method and photocatalytic application thereof |
| CN108166051A (en) * | 2018-03-08 | 2018-06-15 | 合肥工业大学 | A kind of morphology controllable potassium hexatitanate powder crystal material and its low energy consumption preparation method |
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|---|---|---|---|---|
| US5407754A (en) * | 1991-06-20 | 1995-04-18 | Titan Kogyo Kabushiki Kaisha | Potassium hexatitanate fibers for use as reinforcement |
| 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 |
| CN1468805A (en) * | 2002-07-17 | 2004-01-21 | 上海秀普复合材料有限公司 | Potassium titanate whisker and its synthesis |
| CN1740408A (en) * | 2004-08-26 | 2006-03-01 | 上海捷晔复合材料有限公司 | Production process of serial potassium titanate whisker products |
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2007
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Patent Citations (4)
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|---|---|---|---|---|
| US5407754A (en) * | 1991-06-20 | 1995-04-18 | Titan Kogyo Kabushiki Kaisha | Potassium hexatitanate fibers for use as reinforcement |
| 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 |
| CN1468805A (en) * | 2002-07-17 | 2004-01-21 | 上海秀普复合材料有限公司 | Potassium titanate whisker and its synthesis |
| CN1740408A (en) * | 2004-08-26 | 2006-03-01 | 上海捷晔复合材料有限公司 | Production process of serial potassium titanate whisker products |
Non-Patent Citations (4)
| Title |
|---|
| JP特开平5-214117A 1993.08.24 |
| Ningzhong Bao等.High Quality and Yield in Potassium Titanate Wiskers Synthesized by Calcination from Hydrous Titania.《Journal of the American Ceramic Society》.2004,第87卷(第3期),326-330. * |
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Effective date of registration: 20201125 Address after: 201908 Shanghai city Baoshan District Luo Road No. 591 Patentee after: SHANGHAI JINGXU COMPOSITE MATERIAL Co.,Ltd. Patentee after: Nantong whisker Ceramic Manufacturing Co., Ltd Address before: 201908 Shanghai city Baoshan District Luo Road No. 591 Patentee before: SHANGHAI JINGXU COMPOSITE MATERIAL Co.,Ltd. |
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