CN103184349B - High purity zinc preparation device and method - Google Patents
High purity zinc preparation device and method Download PDFInfo
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- CN103184349B CN103184349B CN201110456181.5A CN201110456181A CN103184349B CN 103184349 B CN103184349 B CN 103184349B CN 201110456181 A CN201110456181 A CN 201110456181A CN 103184349 B CN103184349 B CN 103184349B
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- raw material
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- column plate
- purity zinc
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Abstract
The invention provides a high purity zinc preparation device and a method. The high purity zinc preparation device comprises a three-segment tower plate distillation apparatus, a temperature control apparatus and a vacuum system. The three-segment tower plate distillation apparatus comprises a raw material kettle used for filling a zinc raw material; a condenser which comprises a lower condenser placed over the raw material kettle and an upper condenser placed over the lower condenser and having a gas port; a lower tower plate placed between the raw material kettle and the lower condenser, which has a gas port for communicating the raw material kettle and the lower condenser; an upper tower plate placed between the lower condenser and the upper condenser, which has the gas port for communicating the lower condenser and the upper condenser; and a quartz tube with the raw material kettle and the condenser, which has an opening at upper end. The provided high purity zinc preparation device and the method can remove the hazardness impurity and impurity which is difficult to be removed, so that high purity (5N) zinc can be prepared.
Description
Technical field
The present invention relates to a kind of Preparation equipment and method of high pure metal, relate in particular to a kind of Preparation equipment and method of high purity zinc.
Background technology
High purity zinc is widely used in the fields such as ZTO material, infrared detecting materials, material of infrared window, piezoelectric.Along with the development of new high-tech industry, the Application Areas of high purity zinc is increasingly extensive in recent years.
Therefore, the Preparation equipment of high purity zinc and method, as gordian technique, need to be developed, to realize the preparation of high purity zinc.
Summary of the invention
For the object of background technology, the invention provides a kind of Preparation equipment and method of high purity zinc, it can make high-purity (5N) zinc.
In order to realize object of the present invention, aspect first, the Preparation equipment that the invention provides a kind of high purity zinc comprises: three sections of column plate water distilling apparatus, temperature control unit, vacuum system.
Three sections of column plate water distilling apparatus comprise: raw material still, for splendid attire zinc raw material; Condenser, comprises and is placed in the lower condenser of raw material still top and is placed in lower condenser top and comprises the upper condenser of gas port; Lower column plate, is placed between raw material still and lower condenser, and has the pore that raw material still and lower condenser are communicated with; Upper column plate, is placed between lower condenser and upper condenser, and has the aperture that lower condenser and upper condenser are communicated with; And silica tube, in it, hold raw material still and condenser, there is upper end open.
Temperature control unit is around silica tube setting.
Vacuum system comprises: vacuum gland, is communicated with the upper end open sealing of silica tube and the gas port of and upper condenser inner with silica tube; Vacuum pump, is connected in vacuum gland and passes through vacuum gland and silica tube internal communication.
In order to realize object of the present invention, aspect second, the invention provides a kind of preparation method of high purity zinc, adopt the Preparation equipment according to the high purity zinc described in first aspect present invention, the preparation method of described high purity zinc comprises step: zinc raw material is encased in raw material still; Lower column plate, lower condenser, upper column plate and upper condenser are installed successively; Pack the assembly of mounted raw material still, lower column plate, lower condenser, upper column plate, upper condenser into silica tube; With vacuum gland sealed silica envelope; Open vacuum system, silica tube is evacuated to specified vacuum degree; Start temperature control unit, the raw material still to three sections of column plate water distilling apparatus, lower condenser, upper condenser carry out temperature control, and distill the scheduled time; After to be distilled, close and finish vacuum system and temperature control unit, take out condenser and pour out product.
Beneficial effect of the present invention is as follows.
By Preparation equipment and the method for high purity zinc provided by the invention, can remove hazardness impurity and troublesome impurity, high-purity to make (5N) zinc.
Brief description of the drawings
Fig. 1 is according to the structural representation of the Preparation equipment of high purity zinc of the present invention.
Wherein, description of reference numerals is as follows:
1 three sections of column plate water distilling apparatus 2 temperature control unit 3 vacuum systems
4 base 5 housing 6 thermal insulator
11 raw material still 13 condenser 15 silica tubes
Column plate 21 silicon carbide heating tubes on 17 times column plates 18
131 times condensers of 31 vacuum gland 33 vacuum pumps
Condenser 151 upper end open 171 pores on 133
181 aperture 1331 gas ports
Embodiment
Below in conjunction with brief description of the drawings according to the Preparation equipment of high purity zinc of the present invention and method.
First illustrate according to the Preparation equipment of high purity zinc of the present invention in conjunction with Fig. 1.
As shown in Figure 1, comprise three sections of column plate water distilling apparatus 1, temperature control unit 2 and vacuum system 3 according to the Preparation equipment of high purity zinc of the present invention.
Three sections of column plate water distilling apparatus 1, comprising: raw material still 11, for splendid attire zinc raw material; Condenser 13, comprises the lower condenser 131 that is placed in raw material still 11 tops and the upper condenser 13 that is placed in lower condenser 131 tops, and upper condenser 133 comprises gas port 1331; Lower column plate 17, is placed between raw material still 11 and lower condenser 131, and has the pore 171 that raw material still 11 and lower condenser 131 are communicated with; Upper column plate 18, is placed between lower condenser 131 and upper condenser 133, and has the aperture 181 that lower condenser 131 and upper condenser 133 are communicated with; And silica tube 15, in it, hold raw material still 11, lower column plate 17, upper column plate 18 and condenser 13, and there is upper end open 151.
Temperature control unit 2 arranges around silica tube 15.
Vacuum system 3 comprises: vacuum gland 31, seals the upper end open of silica tube 15 151 and be communicated with silica tube 15 gas port 1331 inner and upper condenser 133; And vacuum pump 33, be connected in vacuum gland 31 and pass through vacuum gland 31 and silica tube 15 internal communication.
In addition, also can comprise according to the Preparation equipment of high purity zinc of the present invention: housing 5, arranges around temperature control unit 1.
In addition, also can comprise according to the Preparation equipment of high purity zinc of the present invention: thermal insulator 6, is arranged in housing 5 and surrounds temperature control unit 1.Thermal insulator 6 can be insulating cotton.
According in the Preparation equipment of high purity zinc of the present invention, preferably, temperature control unit 2 can comprise silicon carbide heating tube 21.
According in the Preparation equipment of high purity zinc of the present invention, preferably, lower column plate 17 can be graphite cake.
According in the Preparation equipment of high purity zinc of the present invention, preferably, upper column plate 18 can be graphite cake.
According in the Preparation equipment of high purity zinc of the present invention, preferably, also can comprise: base 4, supports three sections of column plate water distilling apparatus 1, temperature control unit 2 and vacuum systems 3.
Then illustrate according to the preparation method of high purity zinc of the present invention in conjunction with Fig. 1.
Comprise step according to the preparation method of high purity zinc of the present invention: zinc raw material is encased in the raw material still 11 of three sections of column plate water distilling apparatus 1; Lower column plate 17, lower condenser 131, upper column plate 18 and upper condenser 133 are installed successively; Pack the assembly of mounted raw material still 11, lower column plate 17, lower condenser 131, upper column plate 18, upper condenser 133 into silica tube 15; With vacuum gland 31 sealed silica envelopes 15; Open vacuum system 3 silica tube 15 is evacuated to specified vacuum degree; Start temperature control unit 2, the raw material still 11 to three sections of column plate water distilling apparatus 1, lower condenser 131, upper condenser 133 carry out temperature control, and distill the scheduled time; After to be distilled, close and finish vacuum system 3 and temperature control unit 2, take out condenser 13 and pour out product from condenser 13.
According in the preparation method of high purity zinc of the present invention, preferably, the distilling period temperature of raw material still 11 correspondences is 400～700 DEG C, and the hypomere condensing temperature of lower condenser 131 correspondences is 400～300 DEG C; The epimere condensing temperature of upper condenser 133 is 300～200 DEG C.
According in the preparation method of high purity zinc of the present invention, preferably, specified vacuum degree is 10
-3pa～10
-2pa.
According in the preparation method of high purity zinc of the present invention, preferably, the distillation scheduled time is 5～20h.
According in the preparation method of high purity zinc of the present invention, preferably, zinc raw material is 4N zinc raw material.
The following describes the preparation method's of high purity zinc of the present invention embodiment.
Embodiment 1
Zinc raw material is 4N zinc raw material, and distilling period temperature is 400 DEG C, and hypomere condensing temperature is 300 DEG C, and epimere condensing temperature is 200 DEG C, and vacuum tightness is 10
-3pa, distillation time is 20h.
Embodiment 2
Zinc raw material is 4N zinc raw material, and distilling period temperature is 680 DEG C, and hypomere condensing temperature is 370 DEG C, and epimere condensing temperature is 230 DEG C, and vacuum tightness is 8 × 10
-3pa, distillation time is 13h.
Embodiment 3
Zinc raw material is 4N zinc raw material, and distilling period temperature is 550 DEG C, and hypomere condensing temperature is 320 DEG C, and epimere condensing temperature is 260 DEG C, and vacuum tightness is 2 × 10
-3pa, distillation time is 16h.
Embodiment 4
Zinc raw material is 4N zinc raw material, and distilling period temperature is 620 DEG C, and hypomere condensing temperature is 400 DEG C, and epimere condensing temperature is 300 DEG C, and vacuum tightness is 5 × 10
-3pa, distillation time is 7h.
Embodiment 5
Zinc raw material is 4N zinc raw material, and distilling period temperature is 700 DEG C, and hypomere condensing temperature is 400 DEG C, and epimere condensing temperature is 280 DEG C, and vacuum tightness is 10
-2pa, distillation time is 13h.
Finally provide the detected result of embodiment 1-5.
Detect and adopt icp ms (ICP-MS) to detect (manufacturer is PE company, and model is: DRC-II), the testing conditions of this equipment is: temperature is 18 DEG C～28 DEG C, and relative humidity is 30～70%, and cleanliness factor is 1000 grades.Detect principle: icp ms detection mode: element to be measured, after plasma high-temperature ionization, enters mass analyzer with positive charge form, according to the difference of mass/charge ratio, is received by detector, produces signal.Signal and this element signal ratio of reference material that element to be measured produces draw constituent content to be measured.
Table 1 has provided the detected result of embodiment 1-5.As can be seen from Table 1, foreign matter content is low, and the zinc product of embodiment 1-5 all reaches 5N purity.
The detected result (unit: ppm) of table 1 embodiment 1-5
Claims (10)
1. a Preparation equipment for high purity zinc, is characterized in that, comprising:
Three sections of column plate water distilling apparatus (1), comprising:
Raw material still (11), for splendid attire zinc raw material;
Condenser (13), comprising:
Lower condenser (131), is placed in raw material still (11) top; And
Upper condenser (133), is placed in lower condenser (131) top and comprises gas port (1331);
Lower column plate (17), is placed between raw material still (11) and lower condenser (131), and has the pore (171) that raw material still (11) and lower condenser (131) are communicated with;
Upper column plate (18), is placed between lower condenser (131) and upper condenser (133), and has the aperture (181) that lower condenser (131) and upper condenser (133) are communicated with; And
Silica tube (15), holds raw material still (11) and condenser (13) in it, have upper end
Opening (151);
Temperature control unit (2), arranges around silica tube (15);
Vacuum system (3), comprising:
Vacuum gland (31), is communicated with the gas port (1331) of the upper end open of silica tube (15) (151) sealing and and upper condenser (131) inner with silica tube (15);
Vacuum pump (33), is connected in vacuum gland (31) and passes through vacuum gland (31) and silica tube (15) internal communication.
2. the Preparation equipment of high purity zinc according to claim 1, is characterized in that, also comprises:
Housing (5), arranges around temperature control unit (2); And
Base (4), supports three sections of column plate water distilling apparatus (1), temperature control unit (2) and vacuum system (3);
Wherein, temperature control unit (2) comprises silicon carbide heating tube (21).
3. the Preparation equipment of high purity zinc according to claim 2, is characterized in that, also comprises:
Thermal insulator (6), is arranged in housing (5).
4. the Preparation equipment of high purity zinc according to claim 1, is characterized in that, lower column plate (17) is graphite cake.
5. the Preparation equipment of high purity zinc according to claim 1, is characterized in that, upper column plate (18) is graphite cake.
6. a preparation method for high purity zinc, is characterized in that, adopts the Preparation equipment according to the high purity zinc described in any one in claim 1-5, and the preparation method of described high purity zinc comprises step:
Zinc raw material is encased in raw material still (11);
Lower column plate (17), lower condenser (131), upper column plate (18) and upper condenser (133) are installed successively;
Pack the assembly of mounted raw material still (11), lower column plate (17), lower condenser (131), upper column plate (18), upper condenser (133) into silica tube (15);
With vacuum gland (31) sealed silica envelope (15);
Open vacuum system (3), silica tube (15) is evacuated to specified vacuum degree;
Start temperature control unit (2), the raw material still (11) of three sections of column plate water distilling apparatus (1), lower condenser (131), upper condenser (133) are carried out temperature control, and distilled the scheduled time;
After to be distilled, close and finish vacuum system (3) and temperature control unit (2), take out condenser (13) and pour out product.
7. the preparation method of high purity zinc according to claim 6, is characterized in that, the distilling period temperature that raw material still (11) is corresponding is 400～700 DEG C, and the hypomere condensing temperature that lower condenser (131) is corresponding is 400～300 DEG C; The epimere condensing temperature of upper condenser (133) is 300～200 DEG C.
8. the preparation method of high purity zinc according to claim 6, is characterized in that, specified vacuum degree is 10
-3pa.
9. the preparation method of high purity zinc according to claim 6, is characterized in that, the distillation scheduled time is 5～20h.
10. the preparation method of high purity zinc according to claim 6, is characterized in that, zinc raw material is 4N zinc raw material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110456181.5A CN103184349B (en) | 2011-12-29 | 2011-12-29 | High purity zinc preparation device and method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110456181.5A CN103184349B (en) | 2011-12-29 | 2011-12-29 | High purity zinc preparation device and method |
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|---|---|
| CN103184349A CN103184349A (en) | 2013-07-03 |
| CN103184349B true CN103184349B (en) | 2014-07-23 |
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|---|---|---|---|
| CN201110456181.5A Active CN103184349B (en) | 2011-12-29 | 2011-12-29 | High purity zinc preparation device and method |
Country Status (1)
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107389664A (en) * | 2017-07-31 | 2017-11-24 | 成都中建材光电材料有限公司 | The assay method of impurity content in a kind of high purity zinc |
| CN108950242B (en) * | 2018-07-10 | 2021-04-06 | 成都中建材光电材料有限公司 | Preparation device of high-purity zinc |
| CN117025969A (en) * | 2018-08-20 | 2023-11-10 | 昆明理工大学 | Vacuum furnace and method for extracting lead from waste CRT cone glass |
| CN109095767A (en) * | 2018-08-20 | 2018-12-28 | 昆明理工大学 | A kind of method of vacuum heat treatment CRT cone glass removing lead oxide |
| CN113649531B (en) * | 2021-08-16 | 2023-07-14 | 江西中晶新材料有限公司 | Production method of 5N zinc ingot |
Citations (8)
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|---|---|---|---|---|
| CN1031565A (en) * | 1988-07-21 | 1989-03-08 | 昆明工学院 | Bismuth-silver-zinc-containing shell vacuum extraction silver, bismuth and zinc |
| CN1051202A (en) * | 1989-10-21 | 1991-05-08 | 昆明工学院 | Separation of zn-cd alloy by vacuum distillation |
| JPH08188837A (en) * | 1995-01-09 | 1996-07-23 | Sumitomo Metal Mining Co Ltd | Lead splash condenser equipment |
| CN2602853Y (en) * | 2003-01-24 | 2004-02-11 | 翟国华 | Zinc powder preparation device |
| CN2804119Y (en) * | 2005-07-14 | 2006-08-09 | 刘水海 | Fast cold condensating metal molten purification furnace |
| CN2811904Y (en) * | 2005-06-13 | 2006-08-30 | 罗文洲 | Non-ferrous metal vacuum distillation and separation furnace with external electromagnetic induction heater |
| EP1335032B1 (en) * | 2002-01-30 | 2007-06-27 | Dowa Mining Co., Ltd. | Vacuum distillation method and apparatus for enhanced purification of high-purity metals like indium |
| CN201040765Y (en) * | 2007-05-24 | 2008-03-26 | 汤素蝶 | Vacuum distillation furnace for crude zinc |
-
2011
- 2011-12-29 CN CN201110456181.5A patent/CN103184349B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1031565A (en) * | 1988-07-21 | 1989-03-08 | 昆明工学院 | Bismuth-silver-zinc-containing shell vacuum extraction silver, bismuth and zinc |
| CN1051202A (en) * | 1989-10-21 | 1991-05-08 | 昆明工学院 | Separation of zn-cd alloy by vacuum distillation |
| JPH08188837A (en) * | 1995-01-09 | 1996-07-23 | Sumitomo Metal Mining Co Ltd | Lead splash condenser equipment |
| EP1335032B1 (en) * | 2002-01-30 | 2007-06-27 | Dowa Mining Co., Ltd. | Vacuum distillation method and apparatus for enhanced purification of high-purity metals like indium |
| CN2602853Y (en) * | 2003-01-24 | 2004-02-11 | 翟国华 | Zinc powder preparation device |
| CN2811904Y (en) * | 2005-06-13 | 2006-08-30 | 罗文洲 | Non-ferrous metal vacuum distillation and separation furnace with external electromagnetic induction heater |
| CN2804119Y (en) * | 2005-07-14 | 2006-08-09 | 刘水海 | Fast cold condensating metal molten purification furnace |
| CN201040765Y (en) * | 2007-05-24 | 2008-03-26 | 汤素蝶 | Vacuum distillation furnace for crude zinc |
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|---|---|
| CN103184349A (en) | 2013-07-03 |
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Effective date of registration: 20210628 Address after: 239000 100 Nanjing Road, Langya Economic Development Zone, Chuzhou City, Anhui Province Patentee after: Anhui Zhongfei Technology Co.,Ltd. Address before: 511500 Industrial Zone, wo Yun town, Qingxin County, Qingyuan, Guangdong (beside the fish dam road) Patentee before: FIRST RARE MATERIALS Co.,Ltd. |
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Application publication date: 20130703 Assignee: FIRST SEMICONDUCTOR MATERIALS Co.,Ltd. Assignor: Anhui Zhongfei Technology Co.,Ltd. Contract record no.: X2022980007179 Denomination of invention: Preparation equipment and method of high purity zinc Granted publication date: 20140723 License type: Common License Record date: 20220608 |
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Assignee: FIRST SEMICONDUCTOR MATERIALS Co.,Ltd. Assignor: Anhui Zhongfei Technology Co.,Ltd. Contract record no.: X2022980007179 Date of cancellation: 20230103 |
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