CN103184349A - High purity zinc preparation device and method - Google Patents
High purity zinc preparation device and method Download PDFInfo
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- CN103184349A CN103184349A CN2011104561815A CN201110456181A CN103184349A CN 103184349 A CN103184349 A CN 103184349A CN 2011104561815 A CN2011104561815 A CN 2011104561815A CN 201110456181 A CN201110456181 A CN 201110456181A CN 103184349 A CN103184349 A CN 103184349A
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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 Apparatus and method for of high pure metal, relate in particular to a kind of preparation Apparatus and method for of high purity zinc.
Background technology
High purity zinc is widely used in fields such as ZTO material, infrared acquisition material, 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 Apparatus and method for of high purity zinc need be developed as gordian technique, to realize the preparation of high purity zinc.
Summary of the invention
At the purpose of background technology, the invention provides a kind of preparation Apparatus and method for of high purity zinc, it can make high-purity (5N) zinc.
In order to realize purpose of the present invention, aspect first, the preparation equipment that the invention provides a kind of high purity zinc comprises: three sections column plate water distilling apparatus, temperature control unit, vacuum system.
Three sections column plate water distilling apparatus comprise: the raw material still is used for splendid attire zinc raw material; Condenser comprises the following condenser that places raw material still top and places down above the condenser and comprise the last condenser of gas port; Following column plate places between raw material still and the following condenser, and has the pore that raw material still and following condenser are communicated with; Last column plate places down between condenser and the last condenser, and has the aperture that condenser and last condenser are communicated with; And silica tube, hold raw material still and condenser in it, have upper end open.
Temperature control unit is around the silica tube setting.
Vacuum system comprises: the vacuum gland is communicated with the upper end open sealing of silica tube and with the gas port of the inner and last condenser of silica tube; Vacuum pump is connected in the vacuum gland and passes through vacuum gland and silica tube internal communication.
In order to realize purpose 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 described high purity zinc of first aspect present invention, the preparation method of described high purity zinc comprises step: the zinc raw material is encased in the raw material still; Following column plate, following condenser are installed successively, are gone up column plate and last condenser; With mounted raw material still, down column plate, down condenser, go up column plate, the assembly of going up condenser is packed silica tube into; With vacuum gland seal silica tube; Open vacuum system, silica tube is evacuated to the specified vacuum degree; Start temperature control unit, to the raw material still of three sections column plate vacuum distillation plants, down condenser, go up condenser and carry out temperature control, and distillation scheduled time; Behind to be distilled the finishing, 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 the preparation Apparatus and method for of high purity zinc provided by the invention, can remove hazardness impurity and troublesome impurity, high-purity to make (5N) zinc.
Description of drawings
Fig. 1 is the structural representation according to the preparation equipment of high purity zinc of the present invention.
Wherein, description of reference numerals is as follows:
1 three sections column plate water distilling apparatus 2 temperature control units 3 vacuum systems
4 bases, 5 housings, 6 thermal insulator
11 raw material stills, 13 condensers, 15 silica tubes
Column plate 21 silicon carbide heating tubes on 17 times column plates 18
131 times condensers of 31 vacuum glands, 33 vacuum pumps
Condenser 151 upper end open 171 pores on 133
181 apertures, 1331 gas ports
Embodiment
Below in conjunction with the preparation Apparatus and method for of description of drawings according to high purity zinc of the present invention.
At first in conjunction with the preparation equipment of Fig. 1 explanation according to high purity zinc of the present invention.
As shown in Figure 1, the preparation equipment according to high purity zinc of the present invention comprises three sections column plate water distilling apparatus 1, temperature control unit 2 and vacuum system 3.
Three sections column plate water distilling apparatus 1 comprise: raw material still 11 is used for splendid attire zinc raw material; Condenser 13 comprises the following condenser 131 that places raw material still 11 tops and the last condenser 13 that places down condenser 131 tops, and last condenser 133 comprises gas port 1331; Following column plate 17 places between raw material still 11 and the following condenser 13, and has the pore 171 that raw material still 11 and following condenser 131 are communicated with; Last column plate 18 places down between condenser 131 and the last condenser 133, and has the aperture 181 that condenser 131 and last condenser 133 are communicated with; And silica tube 15, hold raw material still 11, following column plate 17 in it, go up column plate 18 and condenser 13, and have upper end open 151.
Temperature control unit 2 arranges around silica tube 15.
Vacuum system 3 comprises: vacuum gland 31 is communicated with upper end open 151 sealings of silica tube 15 and with silica tube 15 gas ports 1331 inner and upward 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, the preparation equipment according to high purity zinc of the present invention also can comprise: 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 the housing 5 and surrounds temperature control unit 1.Thermal insulator 6 can be insulating cotton.
In the preparation equipment according to high purity zinc of the present invention, preferably, temperature control unit 2 can comprise silicon carbide heating tube 21.
In the preparation equipment according to high purity zinc of the present invention, preferably, following column plate 17 can be graphite cake.
In the preparation equipment according to high purity zinc of the present invention, preferably, last column plate 18 can be graphite cake.
In the preparation equipment according to high purity zinc of the present invention, preferably, also can comprise: base 4, support three sections column plate water distilling apparatus 1, temperature control unit 2 and vacuum systems 3.
Then in conjunction with the preparation method of Fig. 1 explanation according to high purity zinc of the present invention.
Preparation method according to high purity zinc of the present invention comprises step: the zinc raw material is encased in the raw material still 11 of three sections column plate vacuum distillation plants 1; Following column plate 17, following condenser 131 are installed successively, are gone up column plate 18 and last condenser 133; With mounted raw material still 11, down column plate 17, down condenser 131, go up column plate 18, the assembly of going up condenser 133 is packed silica tube 15 into; With vacuum gland 31 sealed silica envelopes 15; Open vacuum system 3 silica tube 15 is evacuated to the specified vacuum degree; Start temperature control unit 2, to the raw material still 11 of three sections column plate vacuum distillation plants 1, down condenser 131, go up condenser 133 and carry out temperature control, and distillation scheduled time; Behind to be distilled the finishing, close and finish vacuum system 3 and temperature control unit 2, take out condenser 13 and from condenser 13, pour out product.
In the preparation method according to high purity zinc of the present invention, preferably, the distilling period temperature of raw material still 11 correspondences is 400～700 ℃, and the hypomere condensing temperature of following condenser 131 correspondences is 400～300 ℃; The epimere condensing temperature of last condenser 133 is 300～200 ℃.
In the preparation method according to high purity zinc of the present invention, preferably, the specified vacuum degree is 10
-3Pa～10
-2Pa.
In the preparation method according to high purity zinc of the present invention, preferably, the distillation scheduled time is 5～20h.
In the preparation method according to high purity zinc of the present invention, preferably, the 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
The zinc raw material is 4N zinc raw material, and the distilling period temperature is 400 ℃, and the hypomere condensing temperature is 300 ℃, and the epimere condensing temperature is 200 ℃, and vacuum tightness is 10
-3Pa, distillation time are 20h.
Embodiment 2
The zinc raw material is 4N zinc raw material, and the distilling period temperature is 680 ℃, and the hypomere condensing temperature is 370 ℃, and the epimere condensing temperature is 230 ℃, and vacuum tightness is 8 * 10
-3Pa, distillation time are 13h.
Embodiment 3
The zinc raw material is 4N zinc raw material, and the distilling period temperature is 550 ℃, and the hypomere condensing temperature is 320 ℃, and the epimere condensing temperature is 260 ℃, and vacuum tightness is 2 * 10
-3Pa, distillation time are 16h.
Embodiment 4
The zinc raw material is 4N zinc raw material, and the distilling period temperature is 620 ℃, and the hypomere condensing temperature is 400 ℃, and the epimere condensing temperature is 300 ℃, and vacuum tightness is 5 * 10
-3Pa, distillation time are 7h.
Embodiment 5
The zinc raw material is 4N zinc raw material, and the distilling period temperature is 700 ℃, and the hypomere condensing temperature is 400 ℃, and the epimere condensing temperature is 280 ℃, and vacuum tightness is 10
-2Pa, distillation time are 13h.
Provide the detected result of embodiment 1-5 at last.
Detect to adopt icp ms (ICP-MS) to detect that (manufacturer is PE company, and model is: DRC-II), the testing conditions of this equipment is: temperature is 18 ℃～28 ℃, and relative humidity is 30～70%, and cleanliness factor is 1000 grades.Detect principle: the icp ms detection mode: after the element process plasma high-temperature to be measured ionization, enter mass analyzer with the positive charge form, the difference according to the mass 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.
Detected result (the unit: ppm) of table 1 embodiment 1-5
Claims (10)
1. the preparation equipment of a high purity zinc is characterized in that, comprising:
Three sections column plate water distilling apparatus (1) comprising:
Raw material still (11) is used for splendid attire zinc raw material;
Condenser (13) comprising:
Following condenser (131) places raw material still (11) top; And
Last condenser (133) places down condenser (131) top and comprises gas port (1331);
Following column plate (17) places between raw material still (11) and the following condenser (131), and has the pore (171) that raw material still (11) and following condenser (131) are communicated with;
Last column plate (18) places down between condenser (131) and the last condenser (133), and has the aperture (181) that condenser (131) and last condenser (133) are communicated with; And
Silica tube (15) holds raw material still (11) and condenser (13) in it, have upper end open (151);
Temperature control unit (2) arranges around silica tube (15);
Vacuum system (3) comprising:
Vacuum gland (31) is communicated with upper end open (151) sealing of silica tube (15) and with the gas port (1331) of the inner and last condenser (131) of 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 (6) supports three sections 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 the housing (5).
4. the preparation equipment of high purity zinc according to claim 1 is characterized in that, following column plate (17) is graphite cake.
5. the preparation equipment of high purity zinc according to claim 1 is characterized in that, following column plate (18) is graphite cake.
6. the preparation method of a high purity zinc is characterized in that, adopts the preparation equipment according to each described high purity zinc among the claim 1-5, and the preparation method of described high purity zinc comprises step:
The zinc raw material is encased in the raw material still (11);
Following column plate (17), following condenser (131) are installed successively, are gone up column plate (18) and last condenser (133);
With mounted raw material still (11), down column plate (17), down condenser (13), go up column plate (18), the assembly of going up condenser (18) is packed silica tube (15) into;
With vacuum gland (31) sealed silica envelope (15);
Open vacuum system (3), silica tube (15) is evacuated to the specified vacuum degree;
Start temperature control unit (2), to the raw material still (13) of three sections column plate vacuum distillation plants (1), down condenser (131), go up condenser (133) and carry out temperature control, and distillation scheduled time;
Behind to be distilled the finishing, 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 ℃, and the hypomere condensing temperature that following condenser (131) is corresponding is 400～300 ℃; The epimere condensing temperature of last condenser (133) is 300～200 ℃.
8. the preparation method of high purity zinc according to claim 6 is characterized in that, the 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, the 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 |
Applications Claiming Priority (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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| Publication Number | Publication Date |
|---|---|
| CN103184349A true CN103184349A (en) | 2013-07-03 |
| CN103184349B CN103184349B (en) | 2014-07-23 |
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ID=48675794
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110456181.5A Active CN103184349B (en) | 2011-12-29 | 2011-12-29 | High purity zinc preparation device and method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103184349B (en) |
Cited By (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 |
| CN108950242A (en) * | 2018-07-10 | 2018-12-07 | 成都中建材光电材料有限公司 | A kind of preparation facilities of high purity zinc |
| 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 |
| CN109182778A (en) * | 2018-08-20 | 2019-01-11 | 昆明理工大学 | A method of extracting lead from discarded CRT cone glass |
| CN113649531A (en) * | 2021-08-16 | 2021-11-16 | 江西中晶新材料有限公司 | Production method of 5N zinc ingot |
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Cited By (6)
| 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 |
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| 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 |
| 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 |
| CN109182778A (en) * | 2018-08-20 | 2019-01-11 | 昆明理工大学 | A method of extracting lead from discarded CRT cone glass |
| CN113649531A (en) * | 2021-08-16 | 2021-11-16 | 江西中晶新材料有限公司 | Production method of 5N zinc ingot |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103184349B (en) | 2014-07-23 |
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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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