CN101837986B - Preparation method of hexagonal trumpet flower shape sodium hexafluorisilicate crystal - Google Patents
Preparation method of hexagonal trumpet flower shape sodium hexafluorisilicate crystal Download PDFInfo
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- CN101837986B CN101837986B CN2010102072468A CN201010207246A CN101837986B CN 101837986 B CN101837986 B CN 101837986B CN 2010102072468 A CN2010102072468 A CN 2010102072468A CN 201010207246 A CN201010207246 A CN 201010207246A CN 101837986 B CN101837986 B CN 101837986B
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Abstract
The invention relates to a preparation method of hexagonal trumpet flower shape sodium hexafluorisilicate crystal, relating to a preparation method of sodium hexafluorisilicate crystal. The invention solves the problem of single shape of the existing sodium hexafluorisilicate. The method of the invention comprises the following steps: erecting a clean glass substrate in ethanol emulsion of silicon dioxide, volatilizing ethanol after standing to obtain a silicon dioxide colloid crystal template; adding the polymer solution or melt on the template; removing the solvent or solidifying the melt to obtain a composite membrane; placing the composite membrane in hydrofluoric acid solution for 3-10min; and taking out of the composite membrane and washing to obtain the hexagonal trumpet flower shape sodium hexafluorisilicate crystal. The sodium hexafluorisilicate crystal prepared by the invention is of a hexagonal trumpet flower shape, has simple preparation method, easily obtained materials and low cost, and can be used as functional materials or used for water treatment.
Description
Technical field
The present invention relates to sodium hexafluorisilicate crystalline preparation method.
Background technology
The hexafluorosilicic acid sodium crystal is as a kind of inorganic crystal material
,Especially the crystalline material of micro-meter scale is widely used in functional materials, device and water treatment field.Because bionic reason, the crystal with flowers, plants and trees shape has been subjected to more concern.Existing control pH value is 2.5 ~ 3.5 by add yellow soda ash and hydrofluoric acid in hexafluorosilicic acid sodium salt crystallisation process, is that 25 ℃, magneticstrength are that the sodium hexafluorisilicate crystalline that reaction 45min prepares under the condition of 5T is shaped as hexagon in temperature; And be six rib tubuloses at the hexafluorosilicic acid sodium crystal of carbon mano-tube composite growth from solution, trumpet flower shape sodium hexafluorisilicate crystal report not at present.
Summary of the invention
The present invention is in order to solve the single problem of existing sodium hexafluorisilicate crystalline shape, and the preparation method of hexagonal trumpet flower shape sodium hexafluorisilicate crystal is provided.
The preparation method of hexagonal trumpet flower shape sodium hexafluorisilicate crystal of the present invention carries out according to the following steps: one, earlier glass substrate is placed on concentration 〉=98%(quality) the vitriol oil in soak 24h~48h, rinse well and dry with deionized water then, obtain clean glass substrate; Two, be 8%~12%(quality by concentration of silicon dioxide), be that the silicon dioxide granule of 380nm~450nm joins in the dehydrated alcohol with particle diameter, and be placed on and handle 5min~15min in the ultrasonic cleaner, obtain the silicon-dioxide emulsion; Three, will stand in the container that the silicon-dioxide emulsion is housed through the clean glass substrate that step 1 obtains, leave standstill, treat ethanol volatilization after, obtain silicon dioxide colloid crystal template; Four, the concentration by polymkeric substance is 8%~12%(quality) take by weighing polymkeric substance and solvent and obtain solution, polymers soln is dripped on the silicon dioxide colloid crystal template then, template is covered fully.Then silicon dioxide colloid crystal template is at room temperature kept 3min~10min, then put it in the vacuum drying oven, under being 50 ℃~80 ℃, the condition of vacuum tightness 0.25kPa ~ 0.6kPa, temperature keeps 2h~3h, under temperature is 100 ℃~130 ℃, the condition of vacuum tightness 0.25kPa ~ 0.6kPa, keep 0.8h~1.2h again, obtain composite membrane; Five, will be placed on concentration through the composite membrane that step 5 obtains is 18%~25%(quality) hydrofluoric acid solution in, be after keeping 3min~10min under 10 ℃~15 ℃ the condition in temperature, composite membrane is taken out, use distilled water wash, obtain hexagonal trumpet flower shape sodium hexafluorisilicate crystal; The polystyrene or the polymethylmethacrylate that are of the polymkeric substance described in the step 4 wherein; Solvent described in the step 4 is toluene or N, dinethylformamide.
The preparation method of hexagonal trumpet flower shape sodium hexafluorisilicate crystal of the present invention can also carry out according to the following steps: one, earlier glass substrate is placed on concentration 〉=98%(quality) the vitriol oil in soak 24h~48h, rinse well and dry with deionized water then, obtain clean glass substrate; Two, be 8%~12%(quality by concentration of silicon dioxide), be that the silicon dioxide granule of 380nm~450nm joins in the dehydrated alcohol with particle diameter, and be placed on and handle 5min~15min in the ultrasonic cleaner, obtain the silicon-dioxide emulsion; Three, will stand in the container that the silicon-dioxide emulsion is housed through the clean glass substrate that step 1 obtains, leave standstill, treat ethanol volatilization after, obtain silicon dioxide colloid crystal template; Four, polymer beads or powder evenly are placed on the silicon dioxide colloid crystal template, template is covered fully, then silicon dioxide colloid crystal template is put into baking oven, heating makes polymkeric substance be viscous state, keep taking out behind 3min~10min, reduce to normal temperature, obtain composite membrane; Five, will be placed on concentration through the composite membrane that step 5 obtains is 18%~25%(quality) hydrofluoric acid solution in, be after keeping 3min~10min under 10 ℃~15 ℃ the condition in temperature, composite membrane is taken out, use distilled water wash, obtain hexagonal trumpet flower shape sodium hexafluorisilicate crystal.
The present invention utilizes plate-making and lithographic technique, adopt method self-assembly from bottom to top, silicon dioxide granule is become the masterplate of control crystalline growth with polymer manufacture, after this template put into hydrofluoric acid solution, glass substrate begins dissolving, and the solute sodium hexafluorisilicate that obtains deposits on composite shuttering, after glass dissolves fully, silica spheres begins dissolving, and dissolving produces SiF
4Gas, the gas upper punch, sedimentary product produces the space before making, and the crystal continued growth obtains flower-shaped crystal.In in this process, polymkeric substance has kept the shape of silica spheres, and silica spheres provides shape and gas, and the glass substrate dissolving provides silicate.The hexafluorosilicic acid sodium crystal of the present invention's preparation is that the hexagonal loudspeaker are flower-shaped, and the preparation method is simple, and material is easy to get, and cost is low, can or be used for water treatment as functional materials.
Description of drawings
Fig. 1 is the low power sem photograph of the hexagonal trumpet flower shape sodium hexafluorisilicate crystal that obtains of embodiment 11; Fig. 2 is the high power sem photograph of the hexagonal trumpet flower shape sodium hexafluorisilicate crystal that obtains of embodiment 11; Fig. 3 is the X diffracting spectrum of the hexagonal trumpet flower shape sodium hexafluorisilicate crystal that obtains of embodiment 11; Fig. 4 is the sem photograph of the hexagonal trumpet flower shape sodium hexafluorisilicate crystal that obtains of embodiment 21.
Embodiment
Embodiment one: present embodiment the preparation method of hexagonal trumpet flower shape sodium hexafluorisilicate crystal carry out according to the following steps: one, earlier glass substrate is placed on concentration 〉=98%(quality) the vitriol oil in soak 24h~48h, rinse well and dry with deionized water then, obtain clean glass substrate; Two, be 8%~12%(quality by concentration of silicon dioxide), be that the silicon dioxide granule of 380nm~450nm joins in the dehydrated alcohol with particle diameter, and be placed on and handle 5min~15min in the ultrasonic cleaner, obtain the silicon-dioxide emulsion; Three, will stand in the container that the silicon-dioxide emulsion is housed through the clean glass substrate that step 1 obtains, leave standstill, treat ethanol volatilization after, obtain silicon dioxide colloid crystal template; Four, the concentration by polymkeric substance is 8%~12%(quality) take by weighing polymkeric substance and solvent and obtain solution, then polymers soln is dripped on the silicon dioxide colloid crystal template, template is covered fully, then silicon dioxide colloid crystal template is at room temperature placed 3min~10min, then put it in the vacuum drying oven, under being 50 ℃~80 ℃, the condition of vacuum tightness 0.25kPa ~ 0.6kPa, temperature keeps 2h~3h, under temperature is 100 ℃~130 ℃, the condition of vacuum tightness 0.25kPa ~ 0.6kPa, keep 0.8h~1.2h again, obtain composite membrane; Five, will be placed on concentration through the composite membrane that step 5 obtains is 18%~25%(quality) hydrofluoric acid solution in, be after keeping 3min~10min under 10 ℃~15 ℃ the condition in temperature, composite membrane is taken out, use distilled water wash, obtain hexagonal trumpet flower shape sodium hexafluorisilicate crystal; The polystyrene or the polymethylmethacrylate that are of the polymkeric substance described in the step 4 wherein; Solvent described in the step 4 is toluene or N, dinethylformamide.
Present embodiment utilization plate-making and lithographic technique, adopt method self-assembly from bottom to top, silicon dioxide granule is become the masterplate of control crystalline growth with polymer manufacture, after this template put into hydrofluoric acid solution, glass substrate begins dissolving, and the solute sodium hexafluorisilicate that obtains deposits on composite shuttering, after glass dissolves fully, silica spheres begins dissolving, and dissolving produces SiF
4Gas, the gas upper punch, sedimentary product produces the space before making, and the crystal continued growth obtains flower-shaped crystal.In in this process, polymkeric substance has kept the shape of silica spheres, and silica spheres provides shape and gas, and the glass substrate dissolving provides silicate.The hexafluorosilicic acid sodium crystal of present embodiment preparation is that the hexagonal loudspeaker are flower-shaped, and the preparation method is simple, and material is easy to get, and cost is low.
Embodiment two: what present embodiment and embodiment one were different is: glass substrate soaks 28h~45h in the step 1 in the vitriol oil.Other is identical with embodiment one.
Embodiment three: what present embodiment was different with embodiment one or two is: glass substrate soaks 36h in the step 1 in the vitriol oil.Other is identical with embodiment one or two.
Embodiment four: what present embodiment was different with one of embodiment one to three is: concentration of silicon dioxide is 9%~11.5%(quality in the step 2), particle diameter is 390nm~440nm, supersound process 6min~13min.Other is identical with one of embodiment one to three.
Embodiment five: what present embodiment was different with one of embodiment one to four is: concentration of silicon dioxide is the 10%(quality in the step 2), particle diameter is 420nm, supersound process 10min.。Other is identical with one of embodiment one to four.
Embodiment six: what present embodiment was different with one of embodiment one to five is: the concentration of polymkeric substance is 9%~11.5%(quality in the step 4).Other is identical with one of embodiment one to five.
Embodiment seven: what present embodiment was different with one of embodiment one to six is: the concentration of polymkeric substance is the 10%(quality in the step 4).Other is identical with one of embodiment one to six.
Embodiment eight: what present embodiment was different with one of embodiment one to seven is: the template that drips polymers soln in the step 4 at room temperature keeps 4min~9min, then put it in the vacuum drying oven, under temperature is 55 ℃~75 ℃, the condition of vacuum tightness 0.3kPa ~ 0.5kPa, keep 2.2h~2.8h, under temperature is 110 ℃~125 ℃, the condition of vacuum tightness 0.3kPa ~ 0.5kPa, keep 0.9h~1.1h again.Other is identical with one of embodiment one to seven.
Embodiment nine: what present embodiment was different with one of embodiment one to eight is: the template that drips polymers soln in the step 4 at room temperature keeps 6min, then put it in the vacuum drying oven, under temperature is 65 ℃, the condition of vacuum tightness 0.4kPa, keep 2.5h, under temperature is 118 ℃, the condition of vacuum tightness 0.4kPa, keep 1.0h again.Other is identical with one of embodiment one to eight.
Embodiment ten: what present embodiment was different with one of embodiment one to nine is: in the step 5 composite membrane being placed on concentration is 19%~24%(quality) hydrofluoric acid solution in, be after keeping 4min~9min under 11 ℃~14 ℃ the condition, composite membrane to be taken out in temperature.Other is identical with one of embodiment one to nine.
Embodiment 11: the preparation method of the hexagonal trumpet flower shape sodium hexafluorisilicate crystal of present embodiment carries out according to the following steps: one, earlier glass substrate is placed on concentration 〉=98%(quality) the vitriol oil in soak 24h, rinse well and dry with deionized water then, obtain clean glass substrate; Two, be the 10%(quality by concentration of silicon dioxide), be that the silicon dioxide granule of 400nm joins in the dehydrated alcohol with particle diameter, and be placed on and handle 10min in the ultrasonic cleaner, obtain the silicon-dioxide emulsion; Three, will stand in the container that the silicon-dioxide emulsion is housed through the clean glass substrate that step 1 obtains, leave standstill, treat ethanol volatilization after, obtain silicon dioxide colloid crystal template; Four, be the 10%(quality by polystyrene concentration) take by weighing polystyrene and toluene and obtain solution, polystyrene solution is dripped on the silicon dioxide colloid crystal template, template is covered fully.After then silicon dioxide colloid crystal template at room temperature being kept 5min, be placed in the vacuum drying oven, under temperature is 60 ℃, the condition of vacuum tightness 0.6kPa, keep 3h, and then under temperature is 120 ℃, the condition of vacuum tightness 0.6kPa, keep 1h to obtain composite membrane; Five, will be placed on concentration through the composite membrane that step 5 obtains is the 20%(quality) hydrofluoric acid solution in, be after keeping 10min under 15 ℃ the condition, composite membrane to be taken out in temperature, use distilled water wash, obtain hexagonal trumpet flower shape sodium hexafluorisilicate crystal.
The low power sem photograph of the hexagonal trumpet flower shape sodium hexafluorisilicate crystal that present embodiment obtains as shown in Figure 1, the high power sem photograph as shown in Figure 2, as can be seen from Figure 1, the trumpet flower shape sodium hexafluorisilicate crystal marshalling, diameter of each flower is 2 μ m ~ 3 μ m, can clearly be seen that from Fig. 2 the hexafluorosilicic acid sodium crystal is that the loudspeaker of hexagonal are flower-shaped.The X diffracting spectrum of the hexagonal trumpet flower shape sodium hexafluorisilicate crystal that present embodiment obtains as shown in Figure 3, as can be seen from Figure 3, present embodiment obtain for the hexafluorosilicic acid sodium crystal
The preparation method of present embodiment is simple, and material is easy to get, and cost is low.
Embodiment 12: the preparation method of the hexagonal trumpet flower shape sodium hexafluorisilicate crystal of present embodiment carries out according to the following steps: one, earlier glass substrate is placed on concentration 〉=98%(quality) the vitriol oil in soak 24h~48h, rinse well and dry with deionized water then, obtain clean glass substrate; Two, be 8%~12%(quality by concentration of silicon dioxide), be that the silicon dioxide granule of 380nm~450nm joins in the dehydrated alcohol with particle diameter, and be placed on and handle 5min~15min in the ultrasonic cleaner, obtain the silicon-dioxide emulsion; Three, will stand in the container that the silicon-dioxide emulsion is housed through the clean glass substrate that step 1 obtains, leave standstill, treat ethanol volatilization after, obtain silicon dioxide colloid crystal template; Four, polymer beads or powder evenly are placed on the silicon dioxide colloid crystal template, template is covered fully, then silicon dioxide colloid crystal template is put into baking oven, heating makes polymkeric substance be viscous state, keep taking out behind 3min~10min, reduce to normal temperature, obtain composite membrane; Five, will be placed on concentration through the composite membrane that step 5 obtains is 18%~25%(quality) hydrofluoric acid solution in, be after keeping 3min~10min under 10 ℃~15 ℃ the condition in temperature, composite membrane is taken out, use distilled water wash, promptly get hexagonal trumpet flower shape sodium hexafluorisilicate crystal.
Present embodiment utilization plate-making and lithographic technique, adopt method self-assembly from bottom to top, silicon dioxide granule is become the masterplate of control crystalline growth with polymer manufacture, after this template put into hydrofluoric acid solution, glass substrate begins dissolving, and the solute sodium hexafluorisilicate that obtains deposits on composite shuttering, after glass dissolves fully, silica spheres begins dissolving, and dissolving produces SiF
4Gas, the gas upper punch, sedimentary product produces the space before making, and the crystal continued growth obtains flower-shaped crystal.In in this process, polymkeric substance has kept the shape of silica spheres, and silica spheres provides shape and gas, and the glass substrate dissolving provides silicate.The hexafluorosilicic acid sodium crystal of present embodiment preparation is that the hexagonal loudspeaker are flower-shaped, and the preparation method is simple, and material is easy to get, and cost is low.
Embodiment 13: what present embodiment and embodiment 12 were different is: glass substrate soaks 28h~45h in the step 1 in the vitriol oil.Other is identical with embodiment 12.
Embodiment 14: what present embodiment was different with embodiment 12 or 13 is: glass substrate soaks 36h in the step 1 in the vitriol oil.Other is identical with embodiment 12 or 13.
Embodiment 15: what present embodiment was different with one of embodiment 12 to 14 is: concentration of silicon dioxide is 9%~11.5%(quality in the step 2), particle diameter is 390nm~440nm, supersound process 6min~13min.Other is identical with one of embodiment 12 to 14.
Embodiment 16: what present embodiment was different with one of embodiment 12 to 15 is: concentration of silicon dioxide is the 10%(quality in the step 2), particle diameter is 420nm, supersound process 10min.Other is identical with one of embodiment 12 to 15.
Embodiment 17: what present embodiment was different with one of embodiment 12 to 16 is: in the step 4 silicon dioxide colloid crystal template of overlie polymer is put into baking oven, heating makes and is viscous state, keeps taking out behind 4min~9min.Other is identical with one of embodiment 12 to 16.
Embodiment 18: what present embodiment was different with one of embodiment 12 to 17 is: in the step 4 silicon dioxide colloid crystal template of overlie polymer is put into baking oven, heating makes and is viscous state, keeps taking out behind the 5min.Other is identical with one of embodiment 12 to 17.
Embodiment 19: what present embodiment was different with one of embodiment 12 to 18 is: in the step 5 composite membrane being placed on concentration is 19%~24%(quality) hydrofluoric acid solution in, be to keep 4min~9min under 11 ℃~14 ℃ the condition in temperature.Other is identical with one of embodiment 12 to 18.
Embodiment 20: what present embodiment was different with one of embodiment 12 to 19 is: in the step 5 composite membrane being placed on concentration is the 20%(quality) hydrofluoric acid solution in, be to keep 5min under 13 ℃ the condition in temperature.Other is identical with one of embodiment 12 to 19.
Embodiment 21: the preparation method of the hexagonal trumpet flower shape sodium hexafluorisilicate crystal of present embodiment carries out according to the following steps: one, earlier glass substrate is placed on concentration 〉=98%(quality) the vitriol oil in soak 24h, rinse well and dry with deionized water then, obtain clean glass substrate; Two, be the 10%(quality by concentration of silicon dioxide), be that the silicon dioxide granule of 450nm joins in the dehydrated alcohol with particle diameter, and be placed on and handle 10min in the ultrasonic cleaner, obtain the silicon-dioxide emulsion; Three, will stand in the container that the silicon-dioxide emulsion is housed through the clean glass substrate that step 1 obtains, leave standstill, treat ethanol volatilization after, obtain silicon dioxide colloid crystal template; Four, polymer beads or powder evenly are placed on the silicon dioxide colloid crystal template, template is covered fully.Then silicon dioxide colloid crystal template is put into baking oven, heating makes polymkeric substance be viscous state, keeps taking out behind the 10min, reduces to normal temperature, obtains composite membrane; Five, will be placed on concentration through the composite membrane that step 5 obtains is the 20%(quality) hydrofluoric acid solution in, be after keeping 10min under 10 ℃~15 ℃ the condition, composite membrane to be taken out in temperature, use distilled water wash, obtain hexagonal trumpet flower shape sodium hexafluorisilicate crystal.
The sodium hexafluorisilicate crystalline sem photograph that present embodiment obtains as shown in Figure 2, as can be seen from Figure 2, the hexagonal trumpet flower shape sodium hexafluorisilicate crystal proper alignment, the diameter of hexagonal trumpet flower is 2 μ m ~ 3 μ m, the preparation method of present embodiment is simple, and material is easy to get, and cost is low.
Claims (6)
1. the preparation method of hexagonal trumpet flower shape sodium hexafluorisilicate crystal, the preparation method who it is characterized in that hexagonal trumpet flower shape sodium hexafluorisilicate crystal carries out according to the following steps: one, earlier glass substrate is placed on concentration 〉=98%(quality) the vitriol oil in soak 24h~48h, rinse well and dry with deionized water then, obtain clean glass substrate; Two, be 8%~12%(quality by concentration of silicon dioxide), be that the silicon dioxide granule of 380nm~450nm joins in the dehydrated alcohol with particle diameter, and be placed on and handle 5min~15min in the ultrasonic cleaner, obtain the silicon-dioxide emulsion; Three, will stand in the container that the silicon-dioxide emulsion is housed through the clean glass substrate that step 1 obtains, leave standstill, treat ethanol volatilization after, obtain silicon dioxide colloid crystal template; Four, the concentration by polymkeric substance is 8%~12%(quality) take by weighing polymkeric substance and solvent and obtain solution, polymers soln is dripped on the silicon dioxide colloid crystal template then, template is covered fully; Then silicon dioxide colloid crystal template is at room temperature kept 3min~10min, then put it in the vacuum drying oven, under being 50 ℃~80 ℃, the condition of vacuum tightness 0.25kPa~0.6kPa, temperature keeps 2h~3h, under temperature is 100 ℃~130 ℃, the condition of vacuum tightness 0.25kPa~0.6kPa, keep 0.8h~1.2h again, obtain composite membrane; Five, will be placed on concentration through the composite membrane that step 5 obtains is 18%~25%(quality) hydrofluoric acid solution in, be after keeping 3min~10min under 10 ℃~15 ℃ the condition in temperature, composite membrane is taken out, use distilled water wash, obtain hexagonal trumpet flower shape sodium hexafluorisilicate crystal; Wherein the polymkeric substance described in the step 4 is polystyrene or polymethylmethacrylate; Solvent described in the step 4 is toluene or N, dinethylformamide.
2. the preparation method of hexagonal trumpet flower shape sodium hexafluorisilicate crystal according to claim 1 is characterized in that glass substrate soaks 28h~45h in the step 1 in the vitriol oil.
3. the preparation method of hexagonal trumpet flower shape sodium hexafluorisilicate crystal according to claim 1 and 2 is characterized in that concentration of silicon dioxide is 9%~11.5%(quality in the step 2), particle diameter is 390nm~440nm, supersound process 6min~13min.
4. the preparation method of hexagonal trumpet flower shape sodium hexafluorisilicate crystal according to claim 3, the concentration that it is characterized in that polymkeric substance in the step 4 is 9%~11.5%(quality).
5. according to the preparation method of claim 1,2 or 4 described hexagonal trumpet flower shape sodium hexafluorisilicate crystals, it is characterized in that the template that drips polymers soln in the step 4 at room temperature keeps 4min~9min, then put it in the vacuum drying oven, under temperature is 55 ℃~75 ℃, the condition of vacuum tightness 0.3kPa~0.5kPa, keep 2.2h~2.8h, under temperature is 110 ℃~125 ℃, the condition of vacuum tightness 0.3kPa~0.5kPa, keep 0.9h~1.1h again.
6. the preparation method of hexagonal trumpet flower shape sodium hexafluorisilicate crystal according to claim 5, it is characterized in that in the step 5 composite membrane being placed on concentration is 19%~24%(quality) hydrofluoric acid solution in, be after keeping 4min~9min under 11 ℃~14 ℃ the condition, composite membrane to be taken out in temperature.
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Citations (2)
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CN1686842A (en) * | 2005-05-24 | 2005-10-26 | 南昌大学 | Technique for preparing sodium fluosilicate by using raffinate extracted from smelting columbite-tantalite ore |
CN101284669A (en) * | 2008-05-06 | 2008-10-15 | 西北大学 | Preparation process of prodan by sodium sulfate method |
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CN1686842A (en) * | 2005-05-24 | 2005-10-26 | 南昌大学 | Technique for preparing sodium fluosilicate by using raffinate extracted from smelting columbite-tantalite ore |
CN101284669A (en) * | 2008-05-06 | 2008-10-15 | 西北大学 | Preparation process of prodan by sodium sulfate method |
Non-Patent Citations (1)
Title |
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翁贤芬等.流沙状氟硅酸钠晶体的制备.《化肥工业》.2005,第32卷(第4期),28-30. * |
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