CN100575264C - A kind of method for preparing magnesium titanate from carnallitite - Google Patents
A kind of method for preparing magnesium titanate from carnallitite Download PDFInfo
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- CN100575264C CN100575264C CN200810023312A CN200810023312A CN100575264C CN 100575264 C CN100575264 C CN 100575264C CN 200810023312 A CN200810023312 A CN 200810023312A CN 200810023312 A CN200810023312 A CN 200810023312A CN 100575264 C CN100575264 C CN 100575264C
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- Prior art keywords
- magnesium titanate
- carnallitite
- containing compound
- potassium
- titanium
- Prior art date
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- 239000011777 magnesium Substances 0.000 title claims abstract description 64
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 49
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000010936 titanium Substances 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 150000001875 compounds Chemical class 0.000 claims abstract description 17
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011591 potassium Substances 0.000 claims abstract description 10
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000005245 sintering Methods 0.000 claims abstract description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 17
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 7
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 2
- 235000015320 potassium carbonate Nutrition 0.000 claims description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 2
- 235000010333 potassium nitrate Nutrition 0.000 claims description 2
- 239000004323 potassium nitrate Substances 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 229910052736 halogen Inorganic materials 0.000 abstract description 3
- 150000002367 halogens Chemical class 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 15
- 238000002360 preparation method Methods 0.000 description 12
- 238000007669 thermal treatment Methods 0.000 description 9
- 239000000126 substance Substances 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000002783 friction material Substances 0.000 description 4
- 238000005342 ion exchange Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 3
- 241000446313 Lamella Species 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- SWHAQEYMVUEVNF-UHFFFAOYSA-N magnesium potassium Chemical compound [Mg].[K] SWHAQEYMVUEVNF-UHFFFAOYSA-N 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 229910017682 MgTi Inorganic materials 0.000 description 1
- 241000276425 Xiphophorus maculatus Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical group [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical class [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 235000012254 magnesium hydroxide Nutrition 0.000 description 1
- -1 oxonium ion Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses and a kind ofly prepare the method for magnesium titanate from carnallitite, is raw material with carnallitite, titanium-containing compound and potassium-containing compound earlier, mixes; Again with mixture 800～1100 ℃ of following sintering 30 minutes～12 hours, sintered product through pulverize, washing, filter after, heat-treat again, obtain magnesium titanate.Natural light halogen masonry is a reaction raw materials, has reduced the raw materials cost of magnesium titanate.By regulating whisker or the platelet that proportioning raw materials is produced different purposes easily, simplified technical process, improved production efficiency, be more suitable for large-scale production.
Description
Technical field
The invention belongs to field of inorganic materials, be specifically related to a kind of from carnallitite preparation magnesium titanate, the particularly method of magnesium titanate platelet or whisker.
Background technology
Magnesium titanate is with sheet K
0.8Mg
0.4Ti
1.6O
4For representative, be a kind of novel high-performance inorganic material, can be used as uses such as friction materials, strongthener, ion-exchange material, therefore more and more be subjected to people and pay close attention to.Japanese patent laid-open 5-221795 once described layered titanic acid potassium magnesium (K
0.8Mg
0.4Ti
1.6O
4) preparation method of platelet, Japanese patent gazette 2000-230618 described its friction control agent as friction materials, and prepared friction materials all has stable friction and wear performance at low temperature to high temperature; While magnesium titanate (K
0.8Mg
0.4Ti
1.6O
4) laminate structure give it again and have good ion-exchange performance, usually as the presoma of other material of preparation, US6677041 has mentioned with K as patent
0.8Mg
0.4Ti
1.6O
4Be reaction raw materials, prepare flaky four titaniums, six titaniums, eight potassium titanate lamella crystals by ion-exchange and double sintering; Patent CN1543437 adopts K
0.8Mg
0.4Ti
1.6O
4Be reaction raw materials, successfully prepared flaky TiO
2Patent ZL01813460.2 K
0.8Mg
0.4Ti
1.6O
4Be reaction raw materials, prepared magnesium titanate platelet by the double sintering after the ion-exchange with lepidocrocite structure.
The preparation method of existing magnesium titanate platelet often needs to add as NaCl, KCl, Na
2MoO
4, K
2WO
4Deng fusing assistant,, improve the quality of products to reduce temperature of reaction; Need add a certain amount of magnesium-containing compound in addition, as MgCl
2, MgCO
3, Mg (NO
3)
2, MgF
2Deng, even pure substance such as simple substance magnesium powder provides the magnesium source.Higher just because of preparation cost, make the costing an arm and a leg of magnesium titanate, thereby limited the application of magnesium titanate.
Carnallitite is the final product that occurring in nature contains magnesium, sylvite lake Evaporation formation, and its molecular formula is KMgCl
36H
2O, the CA registration number is 1318-27-0.It is cheap, often as the raw materials for production of potassium-containing compound, magnesium-containing compound and simple substance magnesium.If substitute above-mentioned fusing assistant and magnesium source with carnallitite, directly use as the magnesium titanate raw materials for production, must make the cost of raw material reduce, also shortened the preparation technology of magnesium titanate simultaneously.But do not appear in the newspapers as yet as the method that raw material or fusing assistant prepare magnesium titanate platelet or whisker at present with carnallitite.
Summary of the invention
The objective of the invention is provides the low cost of a kind of magnesium titanate platelet or whisker, high-quality preparation method at the shortcoming among the existing magnesium titanate preparation method.
Purpose of the present invention can reach by following measure:
A kind ofly prepare the method for magnesium titanate, comprise the steps: from carnallitite
(1) is raw material with carnallitite, titanium-containing compound and potassium-containing compound, mixes;
Wherein carnallitite, titanium-containing compound and potassium-containing compound are respectively with KMgCl
3, TiO
2, K
2The O meter (is promptly amounted to into KMgCl
3, TiO
2, K
2O), its mol ratio is: KMgCl
3: TiO
2: K
2O=1: (3.5～4.5): (1.0～2.5).
(2) with mixture 800～1100 ℃ of following sintering 30 minutes～12 hours.
(3) with after sintered product pulverizing, washing, filtering, heat-treat again, obtain magnesium titanate.
Wherein titanium-containing compound is selected from one or more of titanium dioxide, Titanium Dioxide (Rutile) Top grade, anatase-type titanium oxide, hydrous titanium oxide, rutile-type perovskite powder or Detitanium-ore-type perovskite powder; Potassium-containing compound is selected from one or more of salt of wormwood, saltpetre, potassium hydroxide, Potassium monofluoride; The magnesium titanate that finally obtains is K
0.6-0.8Mg
0.4Ti
1.6O
(3.8-4)Or K
1.54-2Mg
0.77-1Ti
7-7.23O
16Platelet or whisker.Wherein the arithmetical av of the equivalent length of platelet and equivalent width is 0.1～50 μ m, equivalent length and when to measure wide ratio be 1～3, and its mean thickness is 0.05～5 μ m; The length of whisker is 5～50 μ m, and diameter is 0.2～2.5 μ m.Filtration product can be dried before the thermal treatment.
The heat treatment step of present method after sintered product filters can be removed the oxonium ion that enters interlayer when washing, thereby improves the degree of crystallinity of magnesium titanate platelet or whisker, improves the quality of products; Wherein thermal treatment temp is 300～700 ℃.
The thermal treatment process of this law has improved the degree of crystallinity of magnesium titanate platelet or whisker, has improved quality product.The magnesium titanate product of this law preparation can be used as strongthener, friction materials, high temperature material etc.
The invention has the advantages that:
1. natural light halogen masonry is a reaction raw materials, has reduced the raw materials cost of magnesium titanate.
2. can simplify technical process by regulating whisker or the platelet that proportioning raw materials is produced different purposes easily, improve production efficiency, be more suitable for large-scale production.
Description of drawings
Fig. 1 is existing technology of the magnesium titanate technological process of production and comparison diagram of the present invention.
Fig. 2 is K of the present invention
0.8Mg
0.4Ti
1.6O
4Scanning electronic microscope (SEM) figure.
Fig. 3 is K of the present invention
1.54Mg
0.77Ti
7.23O
16Scanning electronic microscope (SEM) figure.
Fig. 4 is K before and after the thermal treatment
0.8Mg
0.4Ti
1.6O
4The strong comparison diagram in x-ray peak of platelet.
Before A is thermal treatment among the figure, after B is thermal treatment.
Embodiment
According to embodiment the present invention is described further below:
Embodiment 1
With carnallitite, TiO
2(Detitanium-ore-type), KOH and KNO
3Press KMgCl
3: TiO
2: K
2O=1: 4.5: 1.5 ratio uniform mixing, place High Temperature Furnaces Heating Apparatus to sinter to 1000 ℃ in mixture, be incubated 1 hour, then furnace cooling; Sintered product is pulverized, and washing is filtered, and oven dry is then 700 ℃ of following thermal treatments.Products therefrom is that the arithmetical av of equivalent length and equivalent width is 1～5 μ m, equivalent length and when to measure wide ratio be 1～3, and mean thickness is the magnesium titanate platelet of 0.05～1 μ m; Adopt fundamental parameters method, by the fluorescent X-ray diffraction analysis, its chemical formula is K
0.8Mg
0.4Ti
1.6O
4(as shown in Figure 2).Fig. 4 is K before and after the thermal treatment
0.8Mg
0.4Ti
1.6O
4The contrast of the strong comparison diagram in x-ray peak of platelet as seen, it is relatively poor relatively not pass through heat treated product crystallinity.
With carnallitite, TiO
2(rutile-type) and K
2CO
3Press KMgCl
3: TiO
2: K
2O=1: 4.5: 2.5 ratio uniform mixing, place High Temperature Furnaces Heating Apparatus to sinter to 1100 ℃ in mixture, be incubated 30 minutes, then furnace cooling; Sintered product is pulverized, and washing is filtered; Then 300 ℃ of thermal treatments.Products therefrom is that the arithmetical av of equivalent length and equivalent width is 50 μ m, equivalent length and when to measure wide ratio be 1.5, and mean thickness is the magnesium titanate platelet of 2～5 μ m; Adopt fundamental parameters method, by the fluorescent X-ray diffraction analysis, its chemical formula is K
0.6Mg
0.4Ti
1.6O
4
Embodiment 3
With carnallitite, hydrous titanium oxide and KNO
3Press KMgCl
3: TiO
2: K
2O=1: 3.5: 1 ratio uniform mixing, place High Temperature Furnaces Heating Apparatus to sinter to 800 ℃ in mixture, be incubated 6 hours, then furnace cooling; All the other operations are with embodiment 1.Products therefrom is that length is 10～20 μ m, and diameter is the magnesium titanate whisker of 0.5 μ m; Use the X-ray diffraction analysis, its chemical formula is K
2MgTi
7O
16(as shown in Figure 3).
Embodiment 4
Carnallitite, hydrous titanium oxide and Detitanium-ore-type perovskite powder, KOH are pressed KMgCl
3: TiO
2: K
2O=1: 3.5: 2 ratio uniform mixing, place High Temperature Furnaces Heating Apparatus to sinter to 900 ℃ in mixture, be incubated 10 hours, then furnace cooling; All the other operations are with embodiment 1.Products therefrom is that length is 20～50 μ m, and diameter is the magnesium titanate whisker of 2.5 μ m; Use the X-ray diffraction analysis, its chemical formula is K
1.54Mg
0.77Ti
7.23O
16
Comparative example 1
1473 gram titanium dioxide, 638 gram potassium titanates, 1003 gram Repone K, 279 gram magnesium hydroxides and 200 ml waters are mixed as tackiness agent.Use water pressure engine to be blended in and be pressed into brick shape under the 14.7Mpa pressure.With this brick in electric furnace 1050 ℃ the calcining 1 hour, then gradually the cooling.The acquisition white powder is pulverized, washes, filters, dried to the incinerating product, and the arithmetical av of its long diameter and weak point diameter is 3 μ m, and mean thickness is 300nm, and long diameter is 1.5 with the weak point diameter ratio.By fluorescent X-ray analysis, determine the K that consists of of this white powder
0.8Mg
0.4Ti
1.6O
4
Compare with embodiment 1, this method technical process complexity has increased production cost (production cost be approximately embodiment 1 150%), has strengthened unnecessary facility investment again.
The present invention is a reaction raw materials with natural light halogen masonry, has reduced the raw materials cost of magnesium titanate.The present invention can simplify technical process by regulating platelet or the whisker that proportioning raw materials is produced different purposes easily, has improved production efficiency, is more suitable for large-scale production.
Reference:
[1] the dog volt is clear good, and Song Yongzhi is intelligent, light Tian Liangyi, multilayer metatitanic acid, layered titanic acid, laminar titanium oxide, and the preparation method of layered titanic acid, CN1543437.
[2]Hrioshi?Ogawa，Tokushima，Shigeo?Takahashi?etl，Platy?potassium?titanate，Process?froproducling?the?same，and?friction?material，US6677041。
[3] coulee is rich, and high bridge is grown the man, is that well is stretched tree, Lepidocrosite type potassium magnesium titanate and preparation method thereof, ZL01813460.2.
[4] Huai gift, Zhao Kuanfang, a kind of preparation method of titanate lamella, CN1978715.
Claims (6)
1, a kind ofly prepares the method for magnesium titanate, it is characterized in that comprising the steps: from carnallitite
(1) is raw material with carnallitite, titanium-containing compound and potassium-containing compound, mixes;
Wherein carnallitite, titanium-containing compound and potassium-containing compound are respectively with KMgCl
3, TiO
2, K
2The O meter, mol ratio is: KMgCl
3: TiO
2: K
2O=1: (3.5～4.5): (1.0～2.5);
(2) with mixture 800～1100 ℃ of following sintering 30 minutes～12 hours;
(3) with after sintered product pulverizing, washing, filtering, heat-treat again, obtain magnesium titanate.
2, according to claim 1ly prepare the method for magnesium titanate, it is characterized in that described titanium-containing compound is selected from one or more of Titanium Dioxide (Rutile) Top grade, anatase-type titanium oxide, hydrous titanium oxide, rutile-type perovskite powder or Detitanium-ore-type perovskite powder from carnallitite.
3, according to claim 1ly prepare the method for magnesium titanate, it is characterized in that described potassium-containing compound is selected from one or more of salt of wormwood, saltpetre, potassium hydroxide, Potassium monofluoride from carnallitite.
4, according to claim 1ly prepare the method for magnesium titanate, it is characterized in that described heat treated temperature is 300～700 ℃ from carnallitite.
5, according to claim 1ly prepare the method for magnesium titanate, it is characterized in that described magnesium titanate is K from carnallitite
0.6-0.8Mg
0.4Ti
1.6O
(3.8-4)Or K
1.54-2Mg
0.77-1Ti
7-7.23O
16Platelet or whisker.
6, the method for preparing magnesium titanate from carnallitite according to claim 5, it is characterized in that the equivalent length of described platelet and the arithmetical av of equivalent width are 0.1～50 μ m, its mean thickness is 0.05～5 μ m, equivalent length and when to measure wide ratio be 1～3; The length of described whisker is 5～50 μ m, and diameter is 0.2～2.5 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810023312A CN100575264C (en) | 2008-04-08 | 2008-04-08 | A kind of method for preparing magnesium titanate from carnallitite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810023312A CN100575264C (en) | 2008-04-08 | 2008-04-08 | A kind of method for preparing magnesium titanate from carnallitite |
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| Publication Number | Publication Date |
|---|---|
| CN101254945A CN101254945A (en) | 2008-09-03 |
| CN100575264C true CN100575264C (en) | 2009-12-30 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102230223B (en) * | 2011-06-16 | 2013-12-18 | 申偲伯 | Method for preparing magnesium potassium titanate by directly utilizing magnesium oxide |
| CN104947176B (en) * | 2015-06-23 | 2017-09-22 | 武汉科技大学 | A kind of hollow-core construction magnesium titanate potassium crystal whisker materials and preparation method thereof |
| 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 |
| CN106830926B (en) * | 2017-01-10 | 2020-07-14 | 南通奥新电子科技有限公司 | Preparation method of potassium magnesium titanate |
| CN113004866A (en) * | 2021-02-04 | 2021-06-22 | 张家港大塚化学有限公司 | Preparation method of environment-friendly friction material |
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