CN105016379A - Method for preparing calcium metatitanate - Google Patents
Method for preparing calcium metatitanate Download PDFInfo
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- CN105016379A CN105016379A CN201510444456.1A CN201510444456A CN105016379A CN 105016379 A CN105016379 A CN 105016379A CN 201510444456 A CN201510444456 A CN 201510444456A CN 105016379 A CN105016379 A CN 105016379A
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- Prior art keywords
- solid
- calcium
- metatitanate
- chloride hydrate
- calcium chloride
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- 239000011575 calcium Substances 0.000 title claims abstract description 42
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 41
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 27
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007787 solid Substances 0.000 claims abstract description 26
- WMFHUUKYIUOHRA-UHFFFAOYSA-N (3-phenoxyphenyl)methanamine;hydrochloride Chemical compound Cl.NCC1=CC=CC(OC=2C=CC=CC=2)=C1 WMFHUUKYIUOHRA-UHFFFAOYSA-N 0.000 claims abstract description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 238000000926 separation method Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000002386 leaching Methods 0.000 claims abstract 2
- 239000012778 molding material Substances 0.000 claims description 14
- 241000370738 Chlorion Species 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 239000000047 product Substances 0.000 abstract description 16
- 239000000463 material Substances 0.000 abstract description 11
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000006227 byproduct Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 2
- WLQXPAUZYVXSNE-UHFFFAOYSA-N [Ca].O[N+]([O-])=O Chemical compound [Ca].O[N+]([O-])=O WLQXPAUZYVXSNE-UHFFFAOYSA-N 0.000 description 2
- 239000012620 biological material Substances 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 150000001669 calcium Chemical class 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000010303 mechanochemical reaction Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000012704 polymeric precursor Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method for preparing calcium metatitanate, and belongs to the technical field of material synthesis. The method comprises firstly uniformly mixing calcium chloride hydrate and titanium dioxide powder according to a mass ratio of 1:1-6:1 to obtain a mixture, then performing compacting molding on the mixture under a pressure of 2-15 MPa to obtain a molded material; sintering the molded material in air , controlling the heating speed to be 5-20 DEG C/min and keeping the temperature for 30-180 min when the temperature reaches to 800-1100 DEG C, so as to obtain a sintered product; adding a hydrochloric acid solution with the concentration of 3 wt%-5 wt% into the obtained sintered product according to the liquid-solid ratio of 15:1-40:1, leaching for 10-30 min, and then performing liquid-solid separation to obtain a solid; and repeatedly washing the solid by using deionized water until no chlorine ion is checked out, and drying the washed solid so as to obtain calcium metatitanate. The method has the characteristics of short flow, simple operation, easily supplied raw materials and auxiliary materials, low production cost, and recyclable by-products.
Description
Technical field
The present invention relates to a kind of method preparing calcium metatitanate, belong to field of material synthesis technology.
Background technology
Calcium metatitanate is a kind of titanate, and be the representative of the perovskite structure be found the earliest, its abundant raw material, is widely used at Material Field.Perovskite structure material has the character such as excellent thermostability, catalysis, magnetic, electroconductibility, sensing, makes it be used widely in the field such as electronics, catalysis.Calcium metatitanate is mainly used in the production of dielectric materials in the electronics industry, is the basic conductor original paper manufacturing monocrystalline and high frequency instrument, as coated material in biomaterial.At present, the main sol-gel method of method, coprecipitation method, mechanochemical reaction, polymeric precursor method etc. of calcium metatitanate is prepared.Samuel Holliday etc. have studied sol-gel method and prepares calcium metatitanate, with high pure nitric acid calcium, titanium isopropylate, ethylene glycol monomethyl ether for raw material, high pure nitric acid calcium and titanium isopropylate are dissolved in ethylene glycol monomethyl ether, then under 500-800 DEG C of condition, be incubated 30-180s and prepare calcium metatitanate, this method is strict to the control of temperature, and also relate to organism reaction, technical difficulty is large, expensive starting materials, is difficult to obtain comparatively ideal calcium metatitanate crystal.This calcium metatitanate will be used for the coated material of biomaterial, and can not meet industrial requirements.Fumio Saito and Suzuki etc. are by calcium oxide or calcium hydroxide and titanium dioxide mechanical mill 2-5 hour obtained calcium metatitanate under 700-900 DEG C of condition, and the simple but obtained calcium metatitanate of this method is impure.Hydrothermal method be by sodium hydroxide and titanium dioxide in autoclave, hydrothermal temperature is carry out liquid phase reaction under the condition of 150-250 DEG C, obtain white precipitate, add a certain amount of calcium chloride solution (Ca ∕ Ti mol ratio is slightly larger than 1) again, under certain pH, ion stirs for some time and just can obtain calcium metatitanate precipitation, through washing, dry obtained calcium metatitanate powder.Though this method process is simple, obtain and under high pressure carry out, equipment requirements is high, and it is poor that pH controls accuracy.Industrial main coprecipitation method produces calcium metatitanate, with oxalic acid react is precipitated after being mixed by a certain percentage by titanium dioxide with calcium oxide, through separation, washing, dry, calcining, obtains calcium metatitanate finished product powder.
In addition, Patent Office of the People's Republic of China (CN 102583514 A) discloses a kind of nanometer wire calcium metatitanate and synthetic method thereof, be dispersed in strong base solution by titania powder and heat, obtain calcium metatitanate precipitation, washing obtains nano level calcium metatitanate powder to neutral rear roasting.
Summary of the invention
For above-mentioned prior art Problems existing and deficiency, the present invention proposes a kind of method preparing calcium metatitanate, with calcium chloride hydrate and titanium dioxide for raw material, through mixing, shaping, sintering, leach, dry, obtain calcium metatitanate product.Compared with prior art, it is short that the present invention has flow process, simple to operate, and raw material, auxiliary material are easy to supply; Production cost is low, and the feature of by product reusable edible, the present invention is achieved through the following technical solutions.
Prepare a method for calcium metatitanate, its concrete steps comprise as follows:
(1) first calcium chloride hydrate and titanium dioxide powder are mixed according to mass ratio 1:1 ~ 6:1 and obtain mixture, then mixture is made type (making sheet, ball, rod etc.) at the pressure of 2 ~ 15Mpa and obtain molding materials;
(2) molding materials that step (1) obtains is sintered in atmosphere, control temperature rise rate be 5 ~ 20 DEG C/min rise to temperature be 800 ~ 1100 DEG C insulation 30 ~ 180min obtain sintered product;
(3) sintered product step (2) obtained is hydrochloric acid soln 10 ~ 30min that 15:1 ~ 40:1ml/g adds that concentration is 3wt% ~ 5wt% according to liquid-solid ratio, then the solid deionized water obtained after solid-liquor separation cleans to can't check chlorion repeatedly, can prepare calcium metatitanate by after the solid drying after washing.
Described calcium chloride hydrate is CaCl
22H
2o, CaCl
24H
2o or CaCl
26H
2o.
Obtain calcium chloride hydrate after the concentrating filter liquor drying obtained after described step (3) solid-liquor separation, return step (1) and use.
The invention has the beneficial effects as follows: compared with prior art, it is short that the present invention has flow process, simple to operate, and raw material, auxiliary material are easy to supply; Production cost is low, the feature of by product reusable edible.
Accompanying drawing explanation
Fig. 1 is present invention process schema;
Fig. 2 is the X-ray powder diffractogram (XRD figure) of the calcium metatitanate that the embodiment of the present invention 1 prepares.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1
As shown in Figure 1, this prepares the method for calcium metatitanate, and its concrete steps comprise as follows:
(1) first calcium chloride hydrate and titanium dioxide powder are mixed according to mass ratio 2:1 and obtain mixture, then mixture is made type (making sheet) at the pressure of 5Mpa and obtain molding materials; Wherein calcium chloride hydrate is CaCl
22H
2o;
(2) molding materials that step (1) obtains is sintered in atmosphere, control temperature rise rate be 10 DEG C/min rise to temperature be 900 DEG C insulation 60min obtain sintered product;
(3) sintered product step (2) obtained is the hydrochloric acid soln 15min that 30:1ml/g adds that concentration is 4wt% according to liquid-solid ratio, then the solid deionized water obtained after solid-liquor separation cleans to can't check chlorion repeatedly, calcium metatitanate can be prepared by after the solid drying (be placed in loft drier at 105 DEG C dry 24h) after washing, obtain calcium chloride hydrate after the concentrating filter liquor drying obtained after solid-liquor separation, return step (1) and use.
The calcium metatitanate XRD figure prepared as shown in Figure 2.
Embodiment 2
As shown in Figure 1, this prepares the method for calcium metatitanate, and its concrete steps comprise as follows:
(1) first calcium chloride hydrate and titanium dioxide powder are mixed according to mass ratio 4:1 and obtain mixture, then mixture is made type (making ball) at the pressure of 5Mpa and obtain molding materials; Wherein calcium chloride hydrate is CaCl
24H
2o;
(2) molding materials that step (1) obtains is sintered in atmosphere, control temperature rise rate be 15 DEG C/min rise to temperature be 900 DEG C insulation 180min obtain sintered product;
(3) sintered product step (2) obtained is the hydrochloric acid soln 30min that 20:1ml/g adds that concentration is 4wt% according to liquid-solid ratio, then the solid deionized water obtained after solid-liquor separation cleans to can't check chlorion repeatedly, calcium metatitanate can be prepared by after the solid drying (be placed in loft drier at 105 DEG C dry 24h) after washing, obtain calcium chloride hydrate after the concentrating filter liquor drying obtained after solid-liquor separation, return step (1) and use.
Embodiment 3
As shown in Figure 1, this prepares the method for calcium metatitanate, and its concrete steps comprise as follows:
(1) first calcium chloride hydrate and titanium dioxide powder are mixed according to mass ratio 3:1 and obtain mixture, then mixture is made type (making ball) at the pressure of 5Mpa and obtain molding materials; Wherein calcium chloride hydrate is CaCl
22H
2o;
(2) molding materials that step (1) obtains is sintered in atmosphere, control temperature rise rate be 5 DEG C/min rise to temperature be 1000 DEG C insulation 30min obtain sintered product;
(3) sintered product step (2) obtained is the hydrochloric acid soln 15min that 40:1ml/g adds that concentration is 3wt% according to liquid-solid ratio, then the solid deionized water obtained after solid-liquor separation cleans to can't check chlorion repeatedly, calcium metatitanate can be prepared by after the solid drying (be placed in loft drier at 105 DEG C dry 24h) after washing, obtain calcium chloride hydrate after the concentrating filter liquor drying obtained after solid-liquor separation, return step (1) and use.
Embodiment 4
As shown in Figure 1, this prepares the method for calcium metatitanate, and its concrete steps comprise as follows:
(1) first calcium chloride hydrate and titanium dioxide powder are mixed according to mass ratio 6:1 and obtain mixture, then mixture is made type (making rod) at the pressure of 15Mpa and obtain molding materials; Wherein calcium chloride hydrate is CaCl
26H
2o;
(2) molding materials that step (1) obtains is sintered in atmosphere, control temperature rise rate be 20 DEG C/min rise to temperature be 1100 DEG C insulation 60min obtain sintered product;
(3) sintered product step (2) obtained is the hydrochloric acid soln 15min that 30:1ml/g adds that concentration is 3wt% according to liquid-solid ratio, then the solid deionized water obtained after solid-liquor separation cleans to can't check chlorion repeatedly, calcium metatitanate can be prepared by after the solid drying (be placed in loft drier at 105 DEG C dry 24h) after washing, obtain calcium chloride hydrate after the concentrating filter liquor drying obtained after solid-liquor separation, return step (1) and use.
Embodiment 5
As shown in Figure 1, this prepares the method for calcium metatitanate, and its concrete steps comprise as follows:
(1) first calcium chloride hydrate and titanium dioxide powder are mixed according to mass ratio 1:1 and obtain mixture, then mixture is made type (making rod) at the pressure of 2Mpa and obtain molding materials; Wherein calcium chloride hydrate is CaCl
26H
2o;
(2) molding materials that step (1) obtains is sintered in atmosphere, control temperature rise rate be 18 DEG C/min rise to temperature be 800 DEG C insulation 50min obtain sintered product;
(3) sintered product step (2) obtained is the hydrochloric acid soln 10min that 15:1ml/g adds that concentration is 5wt% according to liquid-solid ratio, then the solid deionized water obtained after solid-liquor separation cleans to can't check chlorion repeatedly, calcium metatitanate can be prepared by after the solid drying (be placed in loft drier at 105 DEG C dry 24h) after washing, obtain calcium chloride hydrate after the concentrating filter liquor drying obtained after solid-liquor separation, return step (1) and use.
Below by reference to the accompanying drawings the specific embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, in the ken that those of ordinary skill in the art possess, various change can also be made under the prerequisite not departing from present inventive concept.
Claims (3)
1. prepare a method for calcium metatitanate, it is characterized in that concrete steps comprise as follows:
(1) first calcium chloride hydrate and titanium dioxide powder are mixed according to mass ratio 1:1 ~ 6:1 and obtain mixture, then mixture is made type at the pressure of 2 ~ 15Mpa and obtain molding materials;
(2) molding materials that step (1) obtains is sintered in atmosphere, control temperature rise rate be 5 ~ 20 DEG C/min rise to temperature be 800 ~ 1100 DEG C insulation 30 ~ 180min obtain sintered product;
(3) sintered product step (2) obtained is hydrochloric acid soln leaching 10 ~ 30min that 15:1 ~ 40:1ml/g adds that concentration is 3wt% ~ 5wt% according to liquid-solid ratio, then the solid deionized water obtained after solid-liquor separation cleans to can't check chlorion repeatedly, can prepare calcium metatitanate by after the solid drying after washing.
2. the method preparing calcium metatitanate according to claim 1, is characterized in that: described calcium chloride hydrate is CaCl
22H
2o, CaCl
24H
2o or CaCl
26H
2o.
3. the method preparing calcium metatitanate according to claim 1, is characterized in that: obtain calcium chloride hydrate after the concentrating filter liquor drying obtained after described step (3) solid-liquor separation, returns step (1) and uses.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510444456.1A CN105016379A (en) | 2015-07-27 | 2015-07-27 | Method for preparing calcium metatitanate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510444456.1A CN105016379A (en) | 2015-07-27 | 2015-07-27 | Method for preparing calcium metatitanate |
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| Publication Number | Publication Date |
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| CN105016379A true CN105016379A (en) | 2015-11-04 |
Family
ID=54406759
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|---|---|---|---|
| CN201510444456.1A Pending CN105016379A (en) | 2015-07-27 | 2015-07-27 | Method for preparing calcium metatitanate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106241859A (en) * | 2016-08-07 | 2016-12-21 | 淮安新能源材料技术研究院 | The method for preparing solid phase of porous calcium titanate micro-nano particle ball |
| CN107775011A (en) * | 2017-10-26 | 2018-03-09 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method for preparing titanium valve |
| CN109897984A (en) * | 2018-05-25 | 2019-06-18 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of titanium-based metal porous material |
| CN110029487A (en) * | 2019-04-23 | 2019-07-19 | 宁波江东碧辰环保科技有限公司 | A kind of preparation method of easy cleaning high strength industrial filter cloth |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106241859A (en) * | 2016-08-07 | 2016-12-21 | 淮安新能源材料技术研究院 | The method for preparing solid phase of porous calcium titanate micro-nano particle ball |
| CN106241859B (en) * | 2016-08-07 | 2018-07-20 | 淮安新能源材料技术研究院 | The method for preparing solid phase of porous calcium titanate micro-nano particle ball |
| CN107775011A (en) * | 2017-10-26 | 2018-03-09 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method for preparing titanium valve |
| CN107775011B (en) * | 2017-10-26 | 2020-08-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium powder |
| CN109897984A (en) * | 2018-05-25 | 2019-06-18 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of titanium-based metal porous material |
| CN110029487A (en) * | 2019-04-23 | 2019-07-19 | 宁波江东碧辰环保科技有限公司 | A kind of preparation method of easy cleaning high strength industrial filter cloth |
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Application publication date: 20151104 |
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