CN1042654C - Adsorptive palladium-alloy net - Google Patents
Adsorptive palladium-alloy net Download PDFInfo
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- CN1042654C CN1042654C CN95108021A CN95108021A CN1042654C CN 1042654 C CN1042654 C CN 1042654C CN 95108021 A CN95108021 A CN 95108021A CN 95108021 A CN95108021 A CN 95108021A CN 1042654 C CN1042654 C CN 1042654C
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Abstract
The present invention relates to a palladium alloy adsorbing net which is characterized in that (1), the palladium alloy adsorbing net is made of three kinds of alloy comprising 85% to 97% of palladium, 1 to 10% of nickel and 0.0001 to 5% of cerium; (2) the diameter of net wires of the palladium alloy adsorbing net ranges from 0.098mm to 0.132mm, and meshes of the net ranges from 40 meshes to 60 meshes. With the advantages of high recovery rate, high intensity, little airflow resistance and long service life, the palladium alloy adsorbing net is mainly used for recovering noble metal platinum in the processing of producing nitric acid.
Description
The invention belongs to a kind of absorption net that reclaims precious metal, relate in particular to a kind of adsorptive palladium-alloy net.
When producing nitric acid, the precious metal in the oxidized still is recycled, be the problem that scientific and technical personnel paid close attention to always, makes great efforts to have developed the method for platinum in the various recovery oxidized stills through people.As the mechanical filter method of filtration medium, be characterized in that pressure drop is big with frit or Ceramic Balls, be only applicable to high-pressure process and produce nitric acid.
Austria's nitrogen company (OSW) method is the CaO absorption method, and it is to establish a stainless steel basket behind platinum guaze, and built-in 3-5mm marble chip resolves into CaO and absorbs the PtO of voloxidation when temperature is raised to 600 ℃
2Become jade-green XCaO, YPtO
2And reaching the purpose that reclaims platinum, this method rate of recovery is higher, but resistance is big, the use temperature narrow range.
The sixties, untapped collecter ring reclaimed platinum, the porpezite net was arranged, palladium rhodium web, palladium nickel screen.Germany Degussa company has developed the porpezite collecter ring as nineteen sixty-eight, and the porpezite collecter ring is placed under the platinum guaze, is set off by the heat-resistance stainless steel silk screen, and use temperature 750-850 ℃, this net rate of recovery is low, and cost is too high.The palladium rhodium collecter ring that Beijing 621 is developed is by being that palladium rhodium collecter ring and two-layer up and down heat-resisting separation net combine, and subassembly places under the platinum guaze, and it is not high that this method also has the rate of recovery, and the cost height, the shortcoming of complex manufacturing technology.
The Ergelhard company of the U.S. is in order to overcome the shortcoming of above-mentioned collecter ring, research and develop the palladium nickel screen and reclaimed net, this net is to be combined by palladium nickel screen and two-layer up and down heat-resisting separation net, subassembly is put under the platinum guaze, have rate of recovery height, high temperature resistant, cost is low, gas-flow resistance is little, but it is low that its shortcoming is an intensity, and work-ing life is short.
The objective of the invention is to develop that a kind of intensity is big, the adsorptive palladium-alloy net of long service life.
The object of the present invention is achieved like this, platinum guaze is to be under the condition of high temperature and oxidizing reaction in converter for ammonia oxidation, oxidation along with ammonia, the form that the platinum guaze surface is more volatile oxide compound loses from network, and the platinum oxide of gas phase combines with palladium metal, form the loose material of a kind of non-crystalline state, be adsorbed on the net, play the effect of reclaiming precious metal.
Adsorptive palladium-alloy net is made up of palladium, nickel, three kinds of metals of cerium, and its alloy composition (weight percent) is as follows:
Pd 85-97％
Ni 1-10％
Ce 0.0001-5％
The physical and mechanical properties of adsorptive palladium-alloy net is as follows;
Mesh wire diameter is: 0.098-0.132mm
Mesh: 248 holes/cm
2～558 holes/cm
2
Tensile strength: greater than 343MPa
Unit elongation: greater than 7%
Its making method is as follows:
1.Pa, Ni, Ce be by the above-mentioned composition solid ingredient intermediate frequency vacuum oven of packing into, 1400-1600 ℃ of melting;
2. under 1000 ℃ of-1200 ℃ of temperature hot rolling 20-40 minute;
3. under 1000 ℃ of-1200 ℃ of temperature, carried out one time thermal treatment 20-40 minute;
4. carried out second heat treatment 20-40 minute under 1000 ℃ of-1200 ℃ of temperature cold rolling back;
5. wire drawing, making its diameter is φ 0.098-0.132mm;
Under 780-900 ℃ of temperature to finished silk thermal treatment, 2-5 promptly produces the finished silk of adsorptive palladium-alloy net second;
7. finished silk is made into mesh 248 holes/cm through netting machine
2～558 holes/cm
2
When adsorptive palladium-alloy net when the normal pressure unit uses, palldium alloy net flanging bag be welded into a molectron get final product with heat-resistance stainless steel is two-layer on the net down.When adsorptive palladium-alloy net when Pressure Unit is used, with three layers of heat-resistance stainless steel net two-layer palldium alloy net is separated bag and is welded into a molectron and gets final product.
It is as follows that adsorptive palladium-alloy net of the present invention is installed and used condition:
1. the above-mentioned adsorptive palladium-alloy net finished product that is processed into is installed under the interior platinum guaze of oxidized still;
2. service temperature was installed behind the adsorptive palladium-alloy net within 7 days, and temperature remains on 850 ℃ in the oxidized still, and Controllable Temperature is built in the normal running temperature of producing nitric acid afterwards;
3, the purity requirement of using ammonia does not contain mechanical impuritys such as grease and iron, magnesium greater than 98.5%;
5. prevent that the platinum guaze poisoning from influencing the rate of recovery of adsorptive palladium-alloy net;
6. oxidized still when maintenance, adsorptive palladium-alloy net is pulled down and will be kept flat, forbid complications and extruding;
7. be the 5-8 month duration of service.
Adsorptive palladium-alloy net of the present invention uses the separation and recovery method of back metal platinum as follows:
(1) the molten filtration of adsorptive palladium-alloy net acid after using, obtains precipitation chloroazotic acid thermosol;
(2) adding of the liquid the first step behind above-mentioned thermosol hydrochloric acid, second step added sodium-chlor, and the 3rd step added entry and contains the filtration afterwards of hydrazine reduction precious metal, with filtrate base metal was removed.
(3) after the precipitation that (2) filtration is obtained is used the chloroazotic acid thermosol, add hydrochloric acid and add sodium-chlor again.
(4) behind heating (3) solution, add chloride precipitation platinum, filtrate and precipitate and separate, undertaken by following two steps: the first step: 1. precipitation adds entry and contains hydrazine pulp reduction, filters.2. filter the precipitation obtain with aqua regia dissolution after, add hydrochloric acid reaction intact after, add sodium-chlor again.3. heated solution adds NH
4Cl precipitates platinum, filters, and the oven dry precipitation sinters purity into and be 99.95% extra large bright and beautiful platinum.
Second step: 1. filtrate adds the ammoniacal liquor complexing.2. complex liquid adds the filtration of HCl precipitation palladium.3. filter the precipitation that obtains and add hydrazine hydrate reduction, refilter.4. the throw out flushing chlorine root that obtains, oven dry, sintering.5. alcohol is reduced to purity greater than 99.95% extra large bright and beautiful palladium.
Advantage of the present invention is as follows:
1. little 4. long service life of high 3. gas-flow resistances of high 2. intensity of the rate of recovery
Most preferred embodiment of the present invention is as follows:
Embodiment one
1. palldium alloy composition content is:
Pd:2550g Ni:300g Ce:150g
2. making method is as follows:
(1) Pd, Ni, Ce three metals by the above-mentioned weight solid ingredient intermediate frequency vacuum oven of packing into, melting under 1500 ℃ of temperature;
(2) heat was pricked 30 minutes under 1200 ℃ of temperature;
(3) under 1080 ℃ of temperature, carry out a thermal treatment 30 minutes;
(4) under 1010 ℃ of temperature, carried out second heat treatment 30 minutes after the cold bundle;
(5) wire drawing, making filament diameter is 0.13mm;
(6) under 840 ℃ of temperature, the alloy silk of dialling was heat-treated for 3 seconds, produces the finished silk of adsorptive palladium-alloy net:
(7) finished silk is made into 558 holes/cm
2Net;
(8) with two-layer below the heat-resistance stainless steel net palldium alloy net flanging bag is welded into a molectron, is used to produce the normal pressure unit use of nitric acid.
3. the separation and recovery method after using is as follows:
(1) the folding vat of putting into of the adsorptive palladium-alloy net after using, adds 50 liters of Hcl, after complete reaction, filter, in precipitation, add chloroazotic acid and till flooding precipitation, carried out thermosol.
(2) add Hcl in the solution behind the thermosol and overflow, add the water-soluble filtration of 1.35Kg NaCl again up to no tobacco, in filtrate the adding hydrazine hydrate up to liquid be colourless till, refilter.
(3) filter in above-mentioned second time and obtain adding in the precipitation chloroazotic acid till flooded precipitation, carry out thermosol after adding Hcl overflow up to no tobacco, add 1.35Kg NaCl again.
(4) behind the solution that heating (3) obtains, add ammonium chloride and do not separate out, filter filtrate and precipitation were undertaken by following two steps up to there being precipitation.The first step: 1. precipitation adds hydrazine hydrate up to becoming thick paste, and reduction is filtered.2. filter and add chloroazotic acid in the precipitation obtain till flooded precipitation, adding Hcl in dissolving back overflows up to no tobacco, adds 1.35kg NaCl again.3. behind the solution that heating obtains, add NH
4Cl does not separate out up to there being precipitation, filters, and the oven dry precipitation sinters purity into and be 99.95% spongy platinum.Second step: 1. add the ammoniacal liquor complexing in the filtrate till solution is the straw yellow.2. in solution, add HCl and do not generate, filter up to there being precipitation.3. in the precipitation that filtration obtains, add hydrazine hydrate and become the thick paste reduction, refilter up to liquid.4. the precipitation flushing chlorine root that filtration is obtained is dried sintering.5. burn palladium with alcohol, obtain purity greater than 99.95% sponge palladium.
Embodiment two
1. palldium alloy is formed content with embodiment one.
2. making method just changes into (8) in the making method of embodiment one with three layers of heat-resistance stainless steel net two-layer palldium alloy net separation bag is welded into a molectron, uses for producing the nitric acid Pressure Unit.
3. separation and recovery method is with embodiment one.
Embodiment three
1. palldium alloy composition content is:
Pd:2700g Ni:240g Ce:60g2. making method and separation and recovery method are with embodiment one.Embodiment 4 1. palldium alloys are formed content:
Pd:2835g Ni:150g Ce:15g2. making method and separation and recovery method are with embodiment one.Embodiment 5 1. palldium alloys are formed content:
Pd:2910g Ni:60g Ce:30g2. making method and separation and recovery method are with embodiment one.
Claims (2)
1. adsorptive palladium-alloy net is characterized in that:
(1) it is that its alloy composition is by palladium, nickel, three kinds of alloy compositions of cerium:
Palladium: 85-97% nickel: 1-10% cerium: 0.0001-5%
(2) diameter of adsorptive palladium-alloy net silk is 0.098-0.132mm, and the mesh of being knitted is 248 holes/cm
2～558 holes/cm
2
2. adsorptive palladium-alloy net according to claim 1, the tensile strength that it is characterized in that the adsorptive palladium-alloy net silk is greater than 343MPa, and unit elongation is greater than 7%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95108021A CN1042654C (en) | 1995-06-28 | 1995-06-28 | Adsorptive palladium-alloy net |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95108021A CN1042654C (en) | 1995-06-28 | 1995-06-28 | Adsorptive palladium-alloy net |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1139156A CN1139156A (en) | 1997-01-01 |
| CN1042654C true CN1042654C (en) | 1999-03-24 |
Family
ID=5076597
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95108021A Expired - Fee Related CN1042654C (en) | 1995-06-28 | 1995-06-28 | Adsorptive palladium-alloy net |
Country Status (1)
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| CN (1) | CN1042654C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100457935C (en) * | 2005-11-09 | 2009-02-04 | 贵研铂业股份有限公司 | Palladium-base alloy for recovering platinum catalyst and recovering net |
| CN101906550B (en) * | 2010-07-09 | 2012-07-18 | 深圳市吉盟珠宝股份有限公司 | Palladium alloy and production method thereof |
| JP6368247B2 (en) * | 2011-12-21 | 2018-08-01 | スタムフォード・ディバイセズ・リミテッド | Aerosol generator |
| CN110983094B (en) * | 2019-11-22 | 2021-11-30 | 重庆材料研究院有限公司 | High-strength platinum material for resisting high-temperature deformation and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039448A (en) * | 1988-07-11 | 1990-02-07 | 挪威海德罗公司 | Ductile alloy |
-
1995
- 1995-06-28 CN CN95108021A patent/CN1042654C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039448A (en) * | 1988-07-11 | 1990-02-07 | 挪威海德罗公司 | Ductile alloy |
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| CN1139156A (en) | 1997-01-01 |
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