Preparation method of high purity zinc by vacuum distillation

A high-purity, vacuum technology, used in the improvement of process efficiency, crucible furnaces, furnaces, etc., can solve the problems that the product quality cannot be guaranteed, the temperature and volatilization conditions of the distillation furnace cannot be accurately controlled, and the process conditions are easy to control and separate. Good effect and easy to operate effect

Inactive Publication Date: 2012-07-25
HULUDAO ZINC IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most fire processes use single-zone or double-zone heating technology, which cannot accurately control the temp

Method used

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  • Preparation method of high purity zinc by vacuum distillation
  • Preparation method of high purity zinc by vacuum distillation

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Zinc raw material is 99.99% refined zinc, main impurity content: Pb: 0.005%, Cd: 0.003%, Fe: 0.003%, Cu: 0.002%, Sn: 0.001%, Al: 0.002%. The sum of impurities is 0.01%.

[0046] The process conditions are:

[0047] Crucible feeding 18Kg, distillation time 16h, distillation furnace upper temperature 360°C, lower temperature 460°C, silicon carbide rod heating voltage regulator output voltage 85V, vacuum degree ≤ -0.1Mpa.

[0048] The situation after operating according to this condition:

[0049] Volatile matter 0.3Kg, carbon residue 2.3Kg, 5N semi-finished product 15.4Kg.

[0050] The semi-finished product is sampled at the upper, middle and lower points to make a mixed sample, and then the impurities are detected by ICP-MS mass spectrometer as follows: Pb: 0.00015%, Cd: 0.00015%, Fe: 0.0001%, Cu: 0.00003%, Sn: 0.00001%, Al: 0.00005%, Ni: 0.00005%, Bi: 0.00001%, Mg: 0.00005%, As: 0.00005%, Cr: 0.00005%, Sb: 0.00005%. The sum of impurities is 0.0008%, meeting the requ...

Embodiment 2

[0052]Zinc raw material is 99.995% refined zinc, main impurity content: Pb: 0.003%, Cd: 0.002%, Fe: 0.001%, Cu: 0.001%, Sn: 0.001%, Al: 0.001%. The sum of impurities is 0.005%.

[0053] The process conditions are:

[0054] Crucible feeding 18Kg, distillation time 16h, distillation furnace upper temperature 370°C, lower temperature 470°C, silicon carbide rod heating voltage regulator output voltage 85V, vacuum degree ≤ -0.1Mpa.

[0055] The situation after operating according to this condition:

[0056] Volatile matter 0.3Kg, carbon residue 1.7Kg, 5N semi-finished product 16Kg.

[0057] The semi-finished product is sampled at the upper, middle and lower points to make a mixed sample, and then the impurities are detected by ICP-MS mass spectrometer as follows: Pb: 0.00015%, Cd: 0.00015%, Fe: 0.0001%, Cu: 0.00003%, Sn: 0.00001%, Al: 0.00005%, Ni: 0.00005%, Bi: 0.00001%, Mg: 0.00005%, As: 0.00005%, Cr: 0.00005%, Sb: 0.00005%. The sum of impurities is 0.0008%, meeting the requi...

Embodiment 3

[0059] Zinc raw material is 5N high-purity zinc semi-finished product.

[0060] The process conditions are:

[0061] Crucible feeding 18Kg, distillation time 16h, distillation furnace upper temperature 360°C, lower temperature 460°C, silicon carbide rod heating voltage regulator output voltage 85V, vacuum degree ≤ -0.1Mpa.

[0062] After operating according to this condition, the output situation: volatile matter 0.1Kg, carbon residue 2.4Kg, 6N semi-finished product 15.5Kg.

[0063] The product is made into a mixed sample by sampling at the upper, middle and lower points, and the impurities are detected by ICP-MS mass spectrometer as follows: Pb: 0.000025%, Cd: 0.000025%, Fe: 0.00001%, Cu: 0.000003%, Sn: 0.000001%, Al: 0.000005 % Ni: 0.000005%, Bi: 0.000002%, Mg: 0.000005%, As: 0.000001%, Cr: 0.000002%, Sb: 0.000005%. , the sum of impurities is 0.000089%, meeting the requirements of the standard Q / HX02.07-2007.

[0064] The mass percentage content of the 5N zinc zinc is: ≥9...

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Abstract

The invention provides a preparation method of high purity zinc by vacuum distillation, which includes: subjecting zinc material to acid leaching, washing and drying in a distillation furnace, filling a graphite crucible with the zinc material, subjecting the zinc material to vacuum distillation, discharging high purity zinc, and processing high purity zinc products. The preparation method using the zinc material to produce high purity zinc has the advantages that equipment is simple, operation is easy, separation is effective, process conditions are easy to control and impurity index is low, and is applicable to using zinc materials to produce high purity zinc.

Description

technical field [0001] The invention belongs to the field of nonferrous metal metallurgy, and in particular relates to a method for preparing high-purity zinc by vacuum distillation. Background technique [0002] High-purity zinc is used in the preparation of semiconductor compounds, infrared luminescent materials, advanced alloys, etc. Granules and powders of high-purity zinc can be used as chemical reagents. In recent years, granular and powdery products of high-purity zinc have been widely used in medicine, chemical industry, powder metallurgy, electroplating, spraying, scientific research and other fields. Since the refined zinc water process cannot obtain high-purity zinc with a purity of 5N and 6N through electrolysis, in order to further obtain high-purity zinc products, a fire process is used—that is, the vacuum distillation method is used to produce 5N and 6N high-purity zinc products. Most of the pyrotechnics adopt single-zone or double-zone heating technology, w...

Claims

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Application Information

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IPC IPC(8): C22B19/32C22B19/12C22B19/04
CPCY02P10/20
Inventor 李逸贾乙东李良董兆顺
Owner HULUDAO ZINC IND CO LTD
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