CN1472369A - Preparation of potassium hexatitanate whiskers - Google Patents
Preparation of potassium hexatitanate whiskers Download PDFInfo
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- CN1472369A CN1472369A CNA031169856A CN03116985A CN1472369A CN 1472369 A CN1472369 A CN 1472369A CN A031169856 A CNA031169856 A CN A031169856A CN 03116985 A CN03116985 A CN 03116985A CN 1472369 A CN1472369 A CN 1472369A
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Abstract
A process for preparing the crystal whiskers of potassium hexatitanate from titanium compound and potassium compound includes such steps as preparing spherical precursor from the crystal Ti compound and the K compound, sintering, hydrolyzing with deionized water, filtering, washing, and drying. Its advantages are high quality of crystal whisker, low cost and less discharged sewage.
Description
Technical field
That the present invention relates to is a kind of preparation method's of potassium titanate crystal whisker, particularly a kind of crystal whisker of hexa potassium titanate preparation method, belongs to the material field.
Background technology
Potassium titanate crystal whisker is because of its excellent mechanics and high-temperature physical property, good chemical stability and the processing performance and the high ratio of performance to price, be widely used in the toughness reinforcing enhancing of resin base and ceramic matric composite, especially in fields such as heatproof lagging material, friction materials, insulating material.Sintering process is to carry out the method that high temperature burns till behind the raw material blending, because cost is relatively low, industrial application is more.Find by literature search, China Patent No. is: 00112275.4, name is called: the manufacture method of crystal whisker of hexa potassium titanate, this patented technology is expressed as: a kind of crystal whisker of hexa potassium titanate manufacture method, with titanium compound and potassium compound is raw material, it is characterized in that: the reaction precursor body must contain the amorphous compound and the water of titanium, before synthesizing the raw material that mixes is piled into the thin layer of thick 0.1～3cm, the once sintered crystal whisker of hexa potassium titanate that promptly gets.Though this method has overcome the shortcoming that potassium ion stripping quantity in the multistep sintering process process is difficult to control, technology is numerous and diverse, the difficult control of whisker morphology, and, cause difficulty of scale operation because must control the raw material thickness of thin layer is 0.1～0.3cm; Whisker is separated and is produced a large amount of acid waste liquids in the fine process.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of preparation method of crystal whisker of hexa potassium titanate is provided, this method cost is low, technology controlling and process convenient, be convenient to large-scale commercial production and environmental friendliness, one step sintering promptly obtains the goodish crystal whisker of hexa potassium titanate of quality, makes it solve the problem that exists in the background technology.
The present invention is achieved by the following technical solutions, the present invention is a raw material with titanium compound and potassium compound, raw material is the crystalline compound that contains titanium, the crystalline compound of this titanium is Detitanium-ore-type hydrolyzed titanium dioxide or Detitanium-ore-type metatitanic acid, prepare spherical reaction precursor body by spraying drying or rotary flashing drying process, this spherical reaction precursor body is the coacervate that crystalline compound and the potassium compound by titanium forms; Pack into the reaction precursor body in the crucible or be pre-formed as blank sintering; Separate with deionized water and to knit whisker; By filtering, wash, drying finally makes crystal whisker of hexa potassium titanate again.
Below the invention will be further described, method steps is as follows:
(1) preparation of raw material: raw material is amounted to into TiO
2With K
2O presses TiO
2/ K
2O=2～6mol ratio, preferably 4～6mol ratio adds water and mixes, and the weight percent of total water content is 50～95%;
(2) presoma preparation: adopt spraying drying or rotary flashing drying, stock suspension is made the more uniform spherical reaction precursor body of size;
(3) reaction: will send out and answer presoma to pack in the crucible or be pre-formed as base substrate, 1100～1300 ℃ of following sintering 0.5～12 hour;
(4) separate fibre: sintered product is soaked in 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 (K 150 ℃ of dryings 2 hours
2O6TiO
2).
The present invention has substantive distinguishing features and marked improvement, the present invention has a fixed structure and composition by preparation, the more uniform spherical reaction precursor body of size, saved the long-pending gauge control of stockpile in potassium ion stripping step in the multistep processes technological process and the single stage method process, make that preparation technology is simple and be convenient to control, be fit to scale operation; The whisker quality better, production cost is low, helps applying; Do not need to separate and knit, promptly reduced cost, reduced discharging of waste liquid again, help environmental protection with acid treatment.The present invention's one step sintering promptly gets crystal whisker of hexa potassium titanate, and the crystal whisker of hexa potassium titanate diameter homogeneous of manufacturing (1～3um), fiber elongated (30～60um).Since earlier by drying process prepare have a certain size, more uniform spherical reacting precursor, it is lower to make that the present invention makes the cost of crystal whisker of hexa potassium titanate, the whisker quality is higher, preparation condition is loose, suitable large-scale industrial production and environmental.
Embodiment
Provide following examples in conjunction with content of the present invention:
Embodiment 1
1. preparation of raw material: Detitanium-ore-type industrial metatitanic acid, chemical pure salt of wormwood, wherein TiO
2/ K
2O=6mol, adding water, to make moisture be 50% suspension; 2. presoma preparation: stock suspension made by rotary flashing drying have a fixed structure and composition, the more uniform spherical reaction precursor body of size; 3. reaction: the reaction precursor body is packed in the crucible 1100 ℃ of following sintering 12 hours; 4. separate fibre: sintered product is soaked in 15 times, in 50 ℃ the deionized water 10 hours and stir to separate and knit; 5. filter washing; 6.150 ℃ drying 2 hours.
The crystal whisker of hexa potassium titanate that said process obtains, diameter 1～3um, length 30～60um, quality is even, structural integrity.
Embodiment 2
1. preparation of raw material: Detitanium-ore-type hydrolyzed titanium dioxide, chemical pure salt of wormwood, wherein TiO
2/ K
2O=5mol, adding water, to make moisture be 80% suspension; 2. presoma preparation: stock suspension made by spraying drying have a fixed structure and composition, the more uniform spherical reaction precursor body of size; 3. reaction: the reaction precursor body is packed in the crucible 1200 ℃ of following sintering 4 hours; 4. separate fibre: sintered product is soaked in 10 times, in 100 ℃ the deionized water 2 hours and stir to separate and knit; 5. filter washing; 6.150 ℃ drying 2 hours.
The crystal whisker of hexa potassium titanate that said process obtains, diameter 1～3um, length 30～60um, quality is even, structural integrity.
Embodiment 3
1. preparation of raw material: Detitanium-ore-type industrial metatitanic acid, industrial magnesium phosphate, wherein TiO
2/ K
2O=6mol, adding water, to make moisture be 95% suspension; 2. presoma preparation: stock suspension made by spraying drying have a fixed structure and composition, the more uniform spherical reaction precursor body of size; 3. reaction: with reaction precursor body pre-molding, 1300 ℃ of following sintering 0.5 hour; 4. separate fibre: sintered product is soaked in 5 times, in 100 ℃ the deionized water 5 hours and stir to separate and knit; 5. filter washing; 6.150 ℃ drying 2 hours.
The crystal whisker of hexa potassium titanate that said process obtains, diameter 1～3um, length 30～60um, quality is even, structural integrity.
Embodiment 4
1. preparation of raw material: Detitanium-ore-type industrial metatitanic acid, industrial magnesium phosphate, wherein TiO
2/ K
2O=4mol, adding water, to make moisture be 65% suspension; 2. presoma preparation: stock suspension made by rotary flashing drying have a fixed structure and composition, the more uniform spherical reaction precursor body of size; 3. reaction: with reaction precursor body pre-molding, 1150 ℃ of following sintering 1.5 hours; 4. separate fibre: sintered product is soaked in 15 times, in 80 ℃ the deionized water 2 hours and stir to separate and knit; 5. filter washing; 6.150 ℃ drying 2 hours.
The crystal whisker of hexa potassium titanate that said process obtains, diameter 1～3um, length 30～60um, quality is even, structural integrity.
Claims (3)
1, a kind of preparation method of crystal whisker of hexa potassium titanate, with titanium compound and potassium compound is raw material, it is characterized in that, raw material is the crystalline compound that contains titanium, the crystalline compound of this titanium is Detitanium-ore-type hydrolyzed titanium dioxide or Detitanium-ore-type metatitanic acid, prepare spherical reaction precursor body by spraying drying or rotary flashing drying process, this spherical reaction precursor body is the coacervate that crystalline compound and the potassium compound by titanium forms, pack into the reaction precursor body in the crucible or be pre-formed as blank sintering, separate with deionized water and to knit whisker, again by filtering washing, drying finally makes 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, method steps is as follows:
(1) preparation of raw material: with titanium compound and potassium compound is raw material, and raw material is amounted to into TiO
2With K
2O presses TiO
2/ K
2O=2～6mol ratio adds water and mixes, and the weight percent of total water content is 50～95%;
(2) presoma preparation: adopt spraying drying or rotary flashing drying, stock suspension is made the more uniform spherical reaction precursor body of size;
(3) reaction: will send out and answer presoma to pack in the crucible or be pre-formed as base substrate, 1100～1300 ℃ of following sintering 0.5～12 hour;
(4) separate fibre: sintered product is soaked in 5～15 times, in 50～100 ℃ the deionized water 2～10 hours and stir to separate and knit;
(5) filter washing;
(6) drying makes crystal whisker of hexa potassium titanate K
2O6TiO
2
3, the preparation method of crystal whisker of hexa potassium titanate according to claim 2 is characterized in that, raw material is amounted to into TiO
2With K
2O, preferred TiO
2/ K
2O=4～6mol ratio.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03116985 CN1232679C (en) | 2003-05-16 | 2003-05-16 | Preparation of potassium hexatitanate whiskers |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03116985 CN1232679C (en) | 2003-05-16 | 2003-05-16 | Preparation of potassium hexatitanate whiskers |
Publications (2)
| Publication Number | Publication Date |
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| CN1472369A true CN1472369A (en) | 2004-02-04 |
| CN1232679C CN1232679C (en) | 2005-12-21 |
Family
ID=34152645
Family Applications (1)
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|---|---|---|---|
| CN 03116985 Expired - Fee Related CN1232679C (en) | 2003-05-16 | 2003-05-16 | Preparation of potassium hexatitanate whiskers |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100439572C (en) * | 2005-12-09 | 2008-12-03 | 隗学礼 | Method for preparing titanate lamella |
| CN101148779B (en) * | 2007-07-24 | 2011-07-27 | 山东大学 | Preparation method for potassium titanate crystal whisker |
| CN102259910A (en) * | 2011-06-16 | 2011-11-30 | 申偲伯 | Method for producing potassium titanate in large scale by utilizing ore-grade titanium-containing compound |
| 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 |
| 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 |
| CN104843774A (en) * | 2015-04-14 | 2015-08-19 | 张家港大塚化学有限公司 | Preparation method of large-particle-size potassium titanate material |
| CN104846429A (en) * | 2015-04-14 | 2015-08-19 | 张家港大塚化学有限公司 | Preparation method of potassium hexatitanate crystal plates |
| 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 |
| CN106367810A (en) * | 2016-09-18 | 2017-02-01 | 唐山晶须复合材料制造有限公司 | Method for synthesizing potassium magnesium titanate lamellar crystals from lamellar raw material |
| CN107188593A (en) * | 2017-06-06 | 2017-09-22 | 广东工业大学 | A kind of process for dispersing of accuracy controlling alumina whisker draw ratio |
Families Citing this family (1)
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|---|---|---|---|---|
| CN101297826B (en) * | 2008-04-25 | 2010-11-03 | 天津生机集团股份有限公司 | Compound Bupleurum injection for curing common cold of dog and preparation thereof |
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2003
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100439572C (en) * | 2005-12-09 | 2008-12-03 | 隗学礼 | Method for preparing titanate lamella |
| CN101148779B (en) * | 2007-07-24 | 2011-07-27 | 山东大学 | Preparation method for potassium titanate crystal whisker |
| CN102259910A (en) * | 2011-06-16 | 2011-11-30 | 申偲伯 | Method for producing potassium titanate in large scale by utilizing ore-grade titanium-containing compound |
| CN102259910B (en) * | 2011-06-16 | 2014-03-12 | 申偲伯 | Method for producing potassium titanate in large scale by utilizing ore-grade titanium-containing compound |
| 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 |
| CN104846429B (en) * | 2015-04-14 | 2017-05-10 | 张家港大塚化学有限公司 | Preparation method of potassium hexatitanate crystal plates |
| CN104843774A (en) * | 2015-04-14 | 2015-08-19 | 张家港大塚化学有限公司 | Preparation method of large-particle-size potassium titanate material |
| CN104846429A (en) * | 2015-04-14 | 2015-08-19 | 张家港大塚化学有限公司 | Preparation method of potassium hexatitanate crystal plates |
| 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 |
| 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 |
| CN106367810A (en) * | 2016-09-18 | 2017-02-01 | 唐山晶须复合材料制造有限公司 | Method for synthesizing potassium magnesium titanate lamellar crystals from lamellar raw material |
| CN106367810B (en) * | 2016-09-18 | 2018-09-04 | 唐山晶须复合材料制造有限公司 | The synthetic method of magnesium titanate platelet is synthesized by sheet-shaped material |
| CN107188593A (en) * | 2017-06-06 | 2017-09-22 | 广东工业大学 | A kind of process for dispersing of accuracy controlling alumina whisker draw ratio |
| CN107188593B (en) * | 2017-06-06 | 2020-08-11 | 广东工业大学 | Dispersion method for accurately regulating and controlling length-diameter ratio of alumina whiskers |
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