CN101117728A - Method for synthesizing sodium titanate whisker - Google Patents
Method for synthesizing sodium titanate whisker Download PDFInfo
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- CN101117728A CN101117728A CNA2006100297494A CN200610029749A CN101117728A CN 101117728 A CN101117728 A CN 101117728A CN A2006100297494 A CNA2006100297494 A CN A2006100297494A CN 200610029749 A CN200610029749 A CN 200610029749A CN 101117728 A CN101117728 A CN 101117728A
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- 238000000034 method Methods 0.000 title claims abstract description 10
- GROMGGTZECPEKN-UHFFFAOYSA-N sodium metatitanate Chemical compound [Na+].[Na+].[O-][Ti](=O)O[Ti](=O)O[Ti]([O-])=O GROMGGTZECPEKN-UHFFFAOYSA-N 0.000 title description 3
- 230000002194 synthesizing effect Effects 0.000 title description 2
- 239000011734 sodium Substances 0.000 claims abstract description 32
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 28
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000010791 quenching Methods 0.000 claims abstract description 10
- 230000000171 quenching effect Effects 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000002352 surface water Substances 0.000 claims description 8
- 238000010189 synthetic method Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- WBZKQQHYRPRKNJ-UHFFFAOYSA-L disulfite Chemical compound [O-]S(=O)S([O-])(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-L 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000001953 recrystallisation Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- 229910052717 sulfur Inorganic materials 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 235000010338 boric acid Nutrition 0.000 claims description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 2
- 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
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 229940001516 sodium nitrate Drugs 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 235000010215 titanium dioxide Nutrition 0.000 claims description 2
- 239000002783 friction material Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000012774 insulation material Substances 0.000 abstract 1
- 238000002310 reflectometry Methods 0.000 abstract 1
- 229910001415 sodium ion Inorganic materials 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 229910052719 titanium Inorganic materials 0.000 abstract 1
- 239000010936 titanium Substances 0.000 abstract 1
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- BYRRPYMBVHTVKO-UHFFFAOYSA-N [Na].[Ti] Chemical compound [Na].[Ti] BYRRPYMBVHTVKO-UHFFFAOYSA-N 0.000 description 1
- 150000001257 actinium Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention discloses a manufacturing method for sodium hexa-titanate whiskers. Adopting the melting-quenching method of synthesis, the method comprises: mixing titanium-containing raw material, sodium-containing raw material and fluxing agents first; sintering in a high-temperature container until the mixture becomes molten; taking out the molten mixture and quenching on a special quenching device; dissolving part sodium ions in an acid solution; sintering after filtering, washing and drying, then finished product can be obtained; the technological flow is simple and feasible; and the whole process has no pollution. The sodium hexa-titanate whiskers synthesized with the method of the present invention has low cost, low thermal conductivity and high infrared-ray reflectivity. The sodium hexa-titanate whiskers are 10-50 micrometers in average length and 1-5 micrometers in average diameter and can be used as enhancing material, friction material, heat insulation material, etc.
Description
Technical field
The invention belongs to a kind of manufacture method of inorganic salt whisker, particularly the manufacture method of six titanium sodium titanate crystal whiskers.
Background technology
The performance of sodium hexatitanate whisker is highly stable, and physical strength is also higher, as strongthener and friction materials, has many uses, and especially with low thermal conductivity, high infrared reflection rate and enjoy attention, is very good lagging material.
In synthesizing of sodium hexatitanate whisker, mainly contain hydrothermal method, promptly the hydro-thermal under the High Temperature High Pressure is synthetic.The synthetic sodium hexatitanate whisker of sintering process is difficulty comparatively.The synthetic method that also has sodium titanate nanotubes and mix (mainly being actinium series and lanthanon) sodium titanate be difficult to realize industrialization, and cost is also very high.
The synthetic method of sodium hexatitanate powder is more, and on performance, sodium hexatitanate powder and sodium hexatitanate whisker have very big difference.The purposes of sodium hexatitanate whisker is more extensive.
Summary of the invention
The invention provides a kind of process synthetic method of new sodium hexatitanate whisker.
The synthetic route of sodium hexatitanate whisker
(1) with titaniferous materials and contain sodium raw materials according to TiO
2: Na
2The ratio weighing of O=2.0～3.0 mol ratios, fusing assistant are poured on load weighted raw material evenly mixed together by 1～5% weighing of gross weight; Because of being scorification, not very high to the requirement of raw material, as long as mixing simply;
(2) above-mentioned mixed uniform raw material is entered into 900～1300 ℃ High Temperature Furnaces Heating Apparatus, stopped 30～150 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 evengranular fine powder; What formed this moment is the sodium trititanate whisker;
(4) with above-mentioned fine powder in 1: 15 to 1: 5 ratio of solid-to-liquid ratio, enter into 90～99 ℃, sulfuric acid concentration is in 1～25% the reactor, to react 90～360 minutes;
(5) solution in the above-mentioned reactor is entered into filter, carry out solid-liquid separation, liquid portion is accumulated separately, is pure metabisulfite solution, waits until special disposal, is a kind of industrial chemicals saltcake;
(6), wash most sulfate ion (SO with above-mentioned solid part hot wash
4 2-), in filter, draw off; Washing water turn back in the reactor and recycle;
(7) with the wet feed drying that draws off in the above-mentioned filter, slough surface water;
(8) with the above-mentioned material of sloughing surface water, enter tunnel furnace, stopped 90～300 minutes down, finish the recrystallization conversion, be finished product after being cooled to room temperature at 600～1000 ℃.
Titaniferous materials is meant one or both the mixing in various model titanium dioxides, anatase octahedrite powder, the brookite powder etc.
Contain one or both the mixing that sodium raw materials is meant anhydrous sodium carbonate, anhydrous sodium bicarbonate, SODIUMNITRATE, sodium hydroxide etc.
Fusing assistant is meant zero kind, one or both mixing of sodium sulfate, salt of wormwood, boric acid, sodium-chlor, water glass etc.
By synthetic sodium hexatitanate whisker of the present invention, cost is low, and thermal conductivity is little, infrared reflection rate height, and the mean length of whisker is 10～50 microns, 1～5 micron of mean diameter can be used as strongthener, friction materials, lagging material etc.
Embodiment
Embodiment 1
(1) with anatase thpe white powder and anhydrous sodium carbonate according to TiO
2: Na
2The ratio weighing of O=2.9 mol ratio is poured on load weighted raw material evenly mixed together;
(2) above-mentioned mixed uniform raw material is entered into 1100 ℃ High Temperature Furnaces Heating Apparatus, stopped 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 evengranular fine powder; What formed this moment is the sodium trititanate whisker;
(4) with above-mentioned fine powder in 1: 10 ratio of solid-to-liquid ratio, enter into the reactor of 90 ℃ sulfur acid 5%, reacted 360 minutes;
(5) solution in the above-mentioned reactor is entered into filter, carry out solid-liquid separation, liquid portion is accumulated separately, is pure metabisulfite solution, waits until special disposal;
(6), wash most sulfate ion (SO with above-mentioned solid part hot wash
4 2-), use 1%BaCl
2The solution check does not have muddy, draws off in filter then; Washing water turn back in the reactor and recycle;
(7) with the wet feed drying that draws off in the above-mentioned filter, slough surface water;
(8) with the above-mentioned material of sloughing surface water, enter tunnel furnace, stopped 240 minutes down, finish the recrystallization conversion, be the sodium hexatitanate whisker finished product after being cooled to room temperature at 900 ℃.
Embodiment 2:
(1) with anatase octahedrite powder and anhydrous sodium bicarbonate according to TiO
2: Na
2The ratio weighing of O=2.5 mol ratio with 2% weighing of fusing assistant sodium sulfate by total amount, is poured on load weighted raw material evenly mixed together;
(2) above-mentioned mixed uniform raw material is entered into 1050 ℃ High Temperature Furnaces Heating Apparatus, stopped 100 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 evengranular fine powder; What formed this moment is the sodium trititanate whisker;
(4) with above-mentioned fine powder in 1: 8 ratio of solid-to-liquid ratio, enter into the reactor of 95 ℃ sulfur acid 14%, reacted 260 minutes;
(5) solution in the above-mentioned reactor is entered into filter, carry out solid-liquid separation, liquid portion is accumulated separately, is pure metabisulfite solution, waits until special disposal;
(6), wash most sulfate ion (SO with above-mentioned solid part hot wash
4 2-), use 1%BaCl
2The solution check does not have muddy, draws off in filter then; Washing water turn back in the reactor and recycle;
(7) with the wet feed drying that draws off in the above-mentioned filter, slough surface water;
(8) with the above-mentioned material of sloughing surface water, enter tunnel furnace, stopped 300 minutes down, finish the recrystallization conversion, be the sodium hexatitanate whisker finished product after being cooled to room temperature at 800 ℃.
Claims (4)
1. the synthetic method of a sodium hexatitanate whisker, technical process is as follows:
(1) with titaniferous materials and contain sodium raw materials according to TiO
2: Na
2The ratio weighing of O=2.0～3.0 mol ratios, fusing assistant are poured on load weighted raw material evenly mixed together by 1～5% weighing of total amount;
(2) above-mentioned mixed uniform raw material is entered into 900～1300 ℃ High Temperature Furnaces Heating Apparatus, stopped 30～150 minutes, make the raw material miscellany become molten mass;
(3) above-mentioned molten mass is taken out, carry out quenching, make it be dispersed into evengranular fine powder;
(4) with above-mentioned fine powder in 1: 15 to 1: 5 ratio of solid-to-liquid ratio, advance in 90～99 ℃ the reactor of sulfur acid 1～25%, reacted 90～360 minutes:
(5) solution in the above-mentioned reactor is carried out solid-liquid separation, liquid portion is accumulated separately, is pure metabisulfite solution;
(6), wash most sulfate ion (SO with above-mentioned solid part hot wash
4 2-), in filter, draw off; Washing water turn back in the reactor and recycle;
(7) with the wet feed drying that draws off in the above-mentioned filter, slough surface water;
(8) with the above-mentioned material of sloughing surface water, stopped 90～300 minutes down at 600～1000 ℃, finish the recrystallization conversion, be finished product after being cooled to room temperature.
2. by the synthetic method of the described a kind of sodium hexatitanate whisker of claim 1, it is characterized in that titaniferous materials is meant one or both the mixing in various model titanium dioxides, anatase octahedrite powder, the brookite powder etc.
3. by the synthetic method of claim 1 and 2 described a kind of sodium hexatitanate whiskers, it is characterized in that, contain one or both the mixing that sodium raw materials is meant anhydrous sodium carbonate, anhydrous sodium bicarbonate, SODIUMNITRATE, sodium hydroxide etc.
4. by the synthetic method of claim 1 and 2 described a kind of sodium hexatitanate whiskers, it is characterized in that fusing assistant is meant zero kind, one or both mixing of sodium sulfate, salt of wormwood, boric acid, sodium-chlor, water glass etc.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006100297494A CN101117728B (en) | 2006-08-04 | 2006-08-04 | Method for synthesizing sodium titanate whisker |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006100297494A CN101117728B (en) | 2006-08-04 | 2006-08-04 | Method for synthesizing sodium titanate whisker |
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| Publication Number | Publication Date |
|---|---|
| CN101117728A true CN101117728A (en) | 2008-02-06 |
| CN101117728B CN101117728B (en) | 2011-12-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2006100297494A Expired - Fee Related CN101117728B (en) | 2006-08-04 | 2006-08-04 | Method for synthesizing sodium titanate whisker |
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| Country | Link |
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| CN (1) | CN101117728B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502796A (en) * | 2011-10-09 | 2012-06-20 | 嵇天浩 | Direct and large-scale preparation of sodium hexatitanate without water washing |
| CN104192893A (en) * | 2014-09-01 | 2014-12-10 | 清远先导材料有限公司 | Preparation method of sodium 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 |
| CN107460545A (en) * | 2017-08-24 | 2017-12-12 | 台州学院 | A kind of preparation method of bar-shaped zirconium oxide whisker |
| CN110846717A (en) * | 2019-11-29 | 2020-02-28 | 南京科技职业学院 | Method for preparing sodium titanate whisker by using waste salt containing NaCl |
| CN111040730A (en) * | 2019-11-15 | 2020-04-21 | 鞍钢集团矿业有限公司 | Brake pad composite friction material and preparation method thereof |
Family Cites Families (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 |
| CN1270974C (en) * | 2002-07-17 | 2006-08-23 | 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 |
-
2006
- 2006-08-04 CN CN2006100297494A patent/CN101117728B/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502796A (en) * | 2011-10-09 | 2012-06-20 | 嵇天浩 | Direct and large-scale preparation of sodium hexatitanate without water washing |
| CN104192893A (en) * | 2014-09-01 | 2014-12-10 | 清远先导材料有限公司 | Preparation method of sodium hexatitanate |
| CN104192893B (en) * | 2014-09-01 | 2017-03-22 | 清远先导材料有限公司 | Preparation method of sodium 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 |
| 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 |
| CN107460545A (en) * | 2017-08-24 | 2017-12-12 | 台州学院 | A kind of preparation method of bar-shaped zirconium oxide whisker |
| CN107460545B (en) * | 2017-08-24 | 2019-07-26 | 台州学院 | A kind of preparation method of rodlike zirconium oxide whisker |
| CN111040730A (en) * | 2019-11-15 | 2020-04-21 | 鞍钢集团矿业有限公司 | Brake pad composite friction material and preparation method thereof |
| CN111040730B (en) * | 2019-11-15 | 2021-02-26 | 鞍钢集团矿业有限公司 | Brake pad composite friction material and preparation method thereof |
| CN110846717A (en) * | 2019-11-29 | 2020-02-28 | 南京科技职业学院 | Method for preparing sodium titanate whisker by using waste salt containing NaCl |
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|---|---|
| CN101117728B (en) | 2011-12-28 |
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