CN106967886B - A kind of method of on-line cleaning recycling noble metal in nitric acid plant - Google Patents

A kind of method of on-line cleaning recycling noble metal in nitric acid plant Download PDF

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Publication number
CN106967886B
CN106967886B CN201710150886.1A CN201710150886A CN106967886B CN 106967886 B CN106967886 B CN 106967886B CN 201710150886 A CN201710150886 A CN 201710150886A CN 106967886 B CN106967886 B CN 106967886B
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oxidation furnace
cleaning
water
nitric acid
noble metal
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CN106967886A (en
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赖龙龙
李卫国
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Taiyuan Rui Lin Precious Metals Recycling Co Ltd
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Taiyuan Rui Lin Precious Metals Recycling Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00Obtaining noble metals
    • C22B11/04Obtaining noble metals by wet processes
    • C22B11/042Recovery of noble metals from waste materials
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/20Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
    • C01B21/38Nitric acid
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • Y02P20/129Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Treating Waste Gases (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

The method that the present invention provides on-line cleaning recycling noble metal in a kind of nitric acid plant wherein needing the equipment cleaned based on oxidation furnace, and is carried out at the same time cleaning to the other equipment on production line, and institute's oxidizing stove is combined vertical structure, and inlet and outlet pipe lines connect;Clean range is:From catalyst frame lower part equipment shell body cleaning to oxidation furnace lower gas exit, between include evaporator, water-cooling wall, superheater whole heat exchanger tubes;Cleaning process is as follows:Water flushing → pickling → neutralization → secondary washing → passivation → hand inspection reset → pretreatment.The beneficial effects of the invention are as follows:By the on-line cleaning to oxidation furnace, so that boiler tubulation surface is reached the cleannes to meet the requirements, increase effectively the heat exchange efficiency of waste heat boiler, while also achieving to by the noble metal in impurity(Platinum, palladium)Extraction, significantly reduce the platinum consumption in nitric acid production, reduce production cost for enterprise's production, improve economic well-being of workers and staff.

Description

A kind of method of on-line cleaning recycling noble metal in nitric acid plant
Technical field
The present invention relates to a kind of method for recovering precious metals, and in particular to on-line cleaning recycles noble metal in a kind of nitric acid plant Method.
Background technology
The production technology of nitric acid is broadly divided into high-pressure process, non-pressure process in the world(Seldom)And double pressurized method.High-pressure process due to High energy consumption and low yield energy, and due to the requirement of environmental protection, it is domestic at present closely to eliminate.And the double pressurized method technique being a dark horse, with Its low energy consumption and high production capacity, it has also become the main force of nitric acid production, domestic pressurization process units double at present have to be covered more 100, is often covered Production capacity is 100,000 tons/year or more.It is counted according to national nitric acid salt made from earth containing a comparatively high percentage of sodium chloride association, domestic pressurized nitric acid process units double at present make extensively With functionality set net and install platinum recover additional, the yield in 2016 years, national nitric acid is 15,000,000 tons, is consumed with 0.15 g ton Platinum, 0.1 g ton palladium consumption calculate.The whole nation will be lost platinum porpezite for 1 year and distinguish 2.25 tons, 1.5 tons.Total value is in more than ten00000000 yuan of people People's coin(Now belong to history noble metal price most bottom position period).Again since noble metal belongs to national strategy goods and materials, social value It is huge.
Nitric acid production is to be catalyzed by platinum net using ammonia, oxygen as raw material and realize the two fully burning chemical combination.In nitric acid production In, the operating temperature of platinum-nickel alloys catalysis net is 850-880 DEG C, while under the constant impingement of high pressure draught, your gold such as platinum, palladium The loss of category also can gradually increase with the working time.Reducing the method that platinum consumes at present is mainly:Installation palldium alloy collecter ring, Use platinum-nickel alloys functional sleeve net, installation noble metal recover.It installs collecter ring additional or platinum consumption is reduced with bright using function network Effective fruit, but still have a considerable amount of platinum fine particles as high-temperature gas is lost in along process pipe, and due to just Often in production, the temperature in oxidation furnace is controlled at 850-880 DEG C, a large amount of high-temperature gas and evaporator section and overheat in waste heat boiler The tubulation of section is in direct contact, and a large amount of noble metal granule can be made to be adhered in the form of the oxide on the inner tubal wall of nitric acid system.
Key equipment oxidation furnace during dilute nitric acid production, for internal exchanger there are two types of form, one kind is domestic big " bar cloth cock " form that part company uses;Another kind is external advanced " La Mangte " boiler form.The country has two at present Company has bought the oxidation furnace of two sets of second-hand " La Mangte " boiler forms from foreign countries, is aoxidized in most of dilute nitric acid production device Using " bar cloth cock " boiler form in stove, and the oxidation furnace of " bar cloth cock " form has two big drawbacks:One, such boiler The evaporator section and superheat section of form are frequently present of booster problem, and the third of Shanxi Tian Ji coal chemical industries group covers 270,000 tons/year of production dresses It sets superheat section and multiple pipe explosion accident occurred in once 1 year, cause device cannot normal continuous and steady operation;Jinan chemical fertilizer factory 10 Ten thousand tons/year of production device evaporator sections have blocked up more than ten pipe because of booster.Similar device and similar pipe explosion accident are in China Double upper pressurizations production nitric acid producers it is commonplace;Two, waste heat boiler outlet at bottom NOx gas temperatures are up to 430-470 DEG C, all not up to design objectives(400 DEG C or so)Requirement, this temperature height illustrates that the heat transfer effect of waste heat boiler is bad, changes Thermal effect is bad to also mean that the impurity of tubulation adsorption is too many, and the heat exchange efficiency of boiler can be made to have a greatly reduced quality.
Since most of nitric acid producer is all the oxidation furnace of " bar cloth cock " boiler form at present in China, inside the oxidation furnace Boiler heat exchange pipe due to long-time use, be in direct contact with ammonia and air, cause tubulation surface corrosion deposition fouling it is serious, The heat exchange efficiency of waste heat boiler is set to be greatly reduced, not only the yield of byproduct steam declines in this way, also can be to the technique of whole system Control influences very big.
Invention content
For the above situation, the technical problem to be solved by the present invention is to:Oxidation furnace is general used in existing nitric acid production The store-through problem serious in tubulation surface corrosion deposition fouling, and waste heat boiler heat exchange efficiency is caused to decline, byproduct steam yield Decline.
In view of the above technical problems, the technical solution used in the present invention is:On-line cleaning in a kind of nitric acid plant is provided The method for recycling noble metal;It is the oxidation furnace of " bar cloth cock " boiler form wherein to need the equipment cleaned, this equipment is combination Vertical structure, inlet and outlet pipe lines connection;Clean range is:Go out from catalyst frame lower part equipment shell body cleaning to oxidation furnace lower gas Mouthful place, between including evaporator, water-cooling wall, superheater whole heat exchanger tubes.
The specific method is as follows for on-line cleaning recycling noble metal in nitric acid plant:
It is as follows according to the successful experience cleaning process of similar engineering:Water flushing → pickling → neutralization → secondary washing → Passivation → hand inspection reset → pretreatment;Specific operation process is as follows.
(1)Water rinses
Using during producer's parking maintenance, the big lid of oxidation furnace is dismantled, internal catalyst frame and platinum guaze are integrally hung out, and are beaten That opens the oxidation furnace that high temperature gas-gas heat exchanger is close to enters hole, and closely oxidation furnace exit installation is blind inside process gas pipeline Plate, blind plate lower part are reinforced with channel steel, are then connected to inside oxidation furnace with outside by the aperture among blind plate with wired hose The overflow tank in face;Then, clear water is constantly infused into oxidation furnace, the sewage after equipment is flowed into from the pipeline among blind plate Overflow tank lower layer;With being on the increase for outflow sewage, in the water meeting overflow to overflow tank upper layer container in lower layers of containers, then Start cleaning pump, the water in the container of upper layer is re-injected in oxidation furnace, form a closed circulatory system, cleaning 5-8 is small Shi Hou checks whether there is leak source.
(2)Pickling
Acid solution is allocated, with the continuous injection of acid solution, the solution of overflow tank lower layer will overflow in oxidation furnace Into upper layer, then the solution in upper layer is re-injected in oxidation furnace by pumping, is constantly recycled in this way;
The acid solution selects any one in the hydrochloric acid or phosphoric acid solution of volume a concentration of 10%.
(3)It neutralizes
After pickling, quantitative neutralizer is slowly added into oxidation furnace(Room temperature).Start cleaning pump to be recycled After 0.5-1 hours, after water sample pH value is 8 or so, clear water is replaced, until water sample is normal.
Dosing:Neutralizer adds a concentration of 100-150kg/T;
Process conditions:Room temperature, 0.5-1 hours;
The neutralizer selection sodium hydroxide or sodium bicarbonate solution.
(4)Secondary washing
It after neutralization, is rinsed inside oxidation furnace with a large amount of clear water, sewage draining valve should be opened in flushing process repeatedly Greatly;When inlet and outlet and the clarification of the water quality of each sewage draining exit, you can terminate cleaning.
(5)Passivation
Quantitative passivator is slowly added into overflow tank(Water temperature is kept for 95 ± 5 DEG C), start cleaning pump, by cleaning pump Passivator is injected in oxidation furnace, is turned again in overflow tank by oxidation furnace exit blind plate lower part wired hose, 8-12 is recycled After hour, clear water is replaced, until water sample is normal.
The passivator selects the phosphate of 0.1-0.5% concentration;Add a concentration of 150kg/T;Reaction temperature:95±5 ℃;Reaction time:8-12 hours(Note:Time, longer passivation effect was better).
(6)Manual cleaning resets
After cleaning completion, detailed inspection is carried out to oxidation furnace inside, thoroughly removes the dirt residue at local dead angle position, is closed It is resetted after lattice.
(7)Quality standard ensures
It should reach the set quota to equipment passivation or compound《Boiler Chemical directive/guide》In standard;
A, the metal surface after cleaning should be cleaned, basic noresidue dirt;The mistake that no apparent metal coarse-grain is precipitated washes phenomenon;
B, the metal average corrosion rate measured with corrosion indicator piece should be less than 6g/m2H, corrosion total amount are less than 60g/ m2
The overflow tank is divided into upper layer and lower layer, is connected to tubule between two layers, above one layer be used for recirculation solution, One layer is the impurity such as precipitate precious metals below.
It is wrapped up with stainless steel coil around the blind plate, to prevent the stainless steel tube line loss to oxidation furnace exit gas Evil.
During being cleaned to oxidation furnace, 1, my company can use the steel of stainless steel around blind plate when installing blind plate additional Circle is wrapped up, and any damage will not be caused to stainless steel tubing.It injects before solution, can be first noted into oxidation furnace when 2, cleaning Enter clear water and carry out cycle leak test, it is ensured that allocates cleaning solution after no leak source again, it includes boiler tubulation that can thus eliminate oxidation furnace Any leak source.3, cleaning solution is a kind of special solution, is the patented product of my company, by test of many times, which will not There is any corrosiveness to any iron and steel material quality.In conclusion during being cleaned to oxidation furnace, it will not be to equipment and pipe Line causes any harmful effect.On the contrary, also will increase the heat exchange efficiency of boiler in oxidation furnace after cleaning, nitric acid dress is substantially increased Set the yield of byproduct steam in normal productive process.
After passivation refers to the oxidized property media processes of metal, etch ratio it is original it is untreated before be decreased significantly show As.Passivation is the last one processing step in chemical cleaning, is a crucial step;Boiler heat exchange tubulation is rinsed through pickling, water, is rinsed Afterwards, metal surface is cleaned very much, is activated very much, it is easy to be corroded, so processing must be passivated immediately, after making cleaning Metal surface generates protective film, slows down corrosion.PASSIVATION MECHANISM:It can be explained with boundary-layer theory, that is, think that passivation is due to metal Acted on Oxidant, when effect metal surface generate it is a kind of it is very thin, fine and close, covering performance is good, in energy Admittedly attached passivating film on the metal surface.This tunic mutually exists at independent, typically the compound of oxygen and metal.It plays handle Metal and the completely separated effect of corrosive medium, prevent metal to be in direct contact with corrosive medium, molten to make metal stop substantially Solution.Its surface energy forms the passivating film for meeting above-mentioned requirements, but the passivating film after the oxidized property media processes of austenitic stainless steel Under the halide ions such as Cl-, Br-, the F- for playing activation, it is highly prone to destroy.Though this namely through acid wash passivation at If the austenitic stainless steel pressure vessels of reason cannot be removed totally after carrying out the water pressure test by water stain, but the Cl- that should control water contains Amount is no more than one of the reason of 25ppm.In addition the oxidation film for not being any metal all may be regarded as passivating film, if carbon steel is in high temperature oxygen The oxidation film formed after change is rigidly attached to the requirement of metal surface and cannot use passivating film as due to that cannot meet.
The beneficial effects of the invention are as follows:By the on-line cleaning to oxidation furnace, not only make boiler tubulation surface reach in accordance with It is required that cleannes, increase effectively the heat exchange efficiency of waste heat boiler, while also achieving to by the noble metal in impurity(Platinum, Palladium)Extraction, significantly reduce the platinum consumption in nitric acid production, reduce production cost for enterprise's production, improve economic well-being of workers and staff.
Description of the drawings
Fig. 1 is facilities and equipments transformation schematic diagram of the present invention;
In figure:1, the big lid of oxidation furnace;2, catalyst frame and platinum guaze;3, oxidation furnace;4, blind plate;5, channel steel;6, wired hose;7、 High temperature gas-gas heat exchanger;8, enter hole;9, overflow tank;10, cleaning pump.
Specific implementation mode
The present invention will be described by the following examples, and a kind of nitric acid plant on-line cleaning recycling is provided in the present invention The method of noble metal, cleaning process are as follows:Water flushing → pickling → neutralization → secondary washing → passivation → hand inspection is multiple Position → pretreatment.
(1)Water rinses:Using during producer's parking maintenance, the big lid of oxidation furnace 1 is dismantled, internal catalyst frame and platinum guaze 2 Entirety is hung out, and that opens that high temperature gas-gas heat exchanger 7 suffers oxidation furnace 3 enters hole 8, closely oxidation furnace 3 inside process gas pipeline Exit installs blind plate 4 additional, and 4 lower part of blind plate is reinforced with channel steel 5, then wired hose 6 is used to connect by the aperture among blind plate 4 The overflow tank 9 of logical oxidation furnace 3 inside and outside, as shown in Figure 1;Then clear water is constantly infused into oxidation furnace 3, by equipment Sewage afterwards flows into 9 lower layer of overflow tank from the pipeline among blind plate 4;With being on the increase for outflow sewage, in lower layers of containers In water meeting overflow to 9 upper layer container of overflow tank, then starts cleaning pump 10, the water in the container of upper layer is re-injected into oxidation furnace 3 It is interior, a closed circulatory system is formed, after cleaning 5-8 hours, checks whether there is leak source.
(2)Pickling:The hydrochloric acid solution of allotment 10%, with the continuous injection of hydrochloric acid solution, 9 lower layer of overflow tank in oxidation furnace 3 Solution then the solution in upper layer will be re-injected in oxidation furnace 3 by pumping in overflow to upper layer, so constantly into Row cycle.
(3)It neutralizes:After pickling, quantitative sodium bicarbonate solution is slowly added into oxidation furnace 3;It adds a concentration of 130kg/T;Start cleaning pump 10 and carry out cycle 0.5 hour, after water sample pH value is 8 or so, clear water is replaced, until water sample is normal.
(4)Secondary washing:After neutralization, is rinsed inside oxidation furnace 3 with a large amount of clear water, answered in flushing process repeatedly Sewage draining valve is opened greatly;When inlet and outlet and the clarification of the water quality of each sewage draining exit, you can terminate cleaning.
(5)Passivation:A concentration of 0.3% quantitative phosphate is slowly added into overflow tank 9(Water temperature keeps 95 ± 5 ℃), start cleaning pump 10, injected passivator in oxidation furnace 3 by cleaning pump 10, by 3 exit blind plate of oxidation furnace, 4 lower part steel wire Hose 6 turns again in overflow tank 9, and cycle replaces clear water, until water sample is normal after 10 hours.
(6)Manual cleaning resets:After cleaning completion, detailed inspection is carried out to 3 inside of oxidation furnace, thoroughly removes local dead angle The dirt residue at position resets after qualified.
(7)Quality standard ensures:It should reach the set quota to equipment passivation or compound《Boiler Chemical directive/guide》In Standard;
A, the metal surface after cleaning should be cleaned, basic noresidue dirt;The mistake that no apparent metal coarse-grain is precipitated washes phenomenon;
B, the metal average corrosion rate measured with corrosion indicator piece should be less than 6g/m2H, corrosion total amount are less than 60g/ m2
Cleaning and recovery method provided in the present invention will not be to equipment and pipeline during being cleaned to oxidation furnace Cause any harmful effect.On the contrary, also will increase the heat exchange efficiency of boiler in oxidation furnace after cleaning, nitric acid plant is substantially increased The yield of byproduct steam in normal productive process.

Claims (3)

1. a kind of method of on-line cleaning recycling noble metal in nitric acid plant, which is characterized in that using oxidation furnace as reaction vessel, Line cleans nitric acid plant, and recycles noble metal;Cleaning process includes:Water flushing → pickling → neutralization → secondary washing → blunt Change → hand inspection reset → pretreatment;Specific operation process is as follows:
(1)Water rinses
The big lid of oxidation furnace is dismantled, internal catalyst frame and platinum guaze are integrally hung out, and are opened high temperature gas-gas heat exchanger and suffered oxidation furnace Manhole, closely oxidation furnace exit installs blind plate additional inside process gas pipeline, and blind plate lower part reinforced with channel steel, then The overflow tank of oxidation furnace inside and outside is connected to by the aperture among blind plate with wired hose;Then constantly into oxidation furnace Injected clear water, the sewage after equipment flow into overflow tank lower layer from the pipeline among blind plate;With the continuous increasing of outflow sewage It is more, in the water meeting overflow to overflow tank upper layer container in lower layers of containers, then start cleaning pump, again by the water in the container of upper layer It injects in oxidation furnace, forms a closed circulatory system, after cleaning 5-8 hours, check whether there is leak source;
(2)Pickling:Acid solution is injected in oxidation furnace, with the continuous injection of acid solution, overflow tank lower layer in oxidation furnace Solution then the solution in upper layer will be re-injected in oxidation furnace by pumping, moved in circles in overflow to upper layer;
(3)It neutralizes:After pickling, quantitative neutralizer is slowly added into oxidation furnace at normal temperatures, start cleaning pump into Row cycle is after 0.5-1 hours, after water sample pH value is 8 or so, clear water is replaced, until water sample is normal;
(4)Secondary washing:It after neutralization, is rinsed inside oxidation furnace with a large amount of clear water, should will be arranged in flushing process repeatedly Dirty valve is opened greatly;When inlet and outlet and the clarification of the water quality of each sewage draining exit, that is, terminate to clean;
(5)Passivation:Quantitative passivator is slowly added into overflow tank, water temperature is kept for 95 ± 5 DEG C, starts cleaning pump, by clear It washes pump to inject passivator in oxidation furnace, be turned again in overflow tank by oxidation furnace exit blind plate lower part wired hose, recycled After 8-12 hours, clear water is replaced, until water sample is normal;
(6)Manual cleaning resets:After cleaning completion, detailed inspection is carried out to oxidation furnace inside, thoroughly removes local dead angle position Dirt residue, resetted after qualified;
Acid solution applied in the pickling selects any one in a concentration of 10% hydrochloric acid or phosphoric acid solution;
Used in the neutralization neutralizer selection sodium hydroxide or sodium bicarbonate solution in any one, add a concentration of 100-150kg/T;Neutral temperature is room temperature, and it is 0.5-1 hours to neutralize the time;
The passivator selects the phosphate of a concentration of 0.1-0.5%;Add a concentration of 150kg/T;Reaction temperature:95±5℃; Reaction time:8-12 hours.
2. the method for on-line cleaning recycling noble metal in a kind of nitric acid plant according to claim 1, which is characterized in that When closely oxidation furnace exit installs blind plate additional inside process gas pipeline, wrapped up with stainless steel coil around the blind plate.
3. the method for on-line cleaning recycling noble metal in a kind of nitric acid plant according to claim 1, which is characterized in that institute State overflow tank and be divided into upper layer and lower layer, be connected to tubule between two layers, above one layer be used for recirculation solution, below one layer be Precipitate precious metals impurity.
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