CN203370367U - Filtering device used for recycling solid catalyst particles in water-containing inorganic process liquid - Google Patents
Filtering device used for recycling solid catalyst particles in water-containing inorganic process liquid Download PDFInfo
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- CN203370367U CN203370367U CN201220746000.2U CN201220746000U CN203370367U CN 203370367 U CN203370367 U CN 203370367U CN 201220746000 U CN201220746000 U CN 201220746000U CN 203370367 U CN203370367 U CN 203370367U
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- filter
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- process liquid
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Abstract
Provided is a filtering device used for recycling solid catalyst particles in a water-containing inorganic process liquid. The filtering device is a leaf-shaped filtering machine which contains at least 1 to 30 filtering blades, wherein at least one filtering blade is covered by a filtering cloth.
Description
Technical field
The utility model belongs to the chemical device field.The utility model relates to a kind of filter apparatus that reclaims solid catalyst particle from moisture inorganic process liquid, and this moisture inorganic process liquid is used for the production of hydroxylammonium by leaf filter.Described leaf filter contains 30 filter leaves altogether.Described filter leaf covers with filter cloth.The utility model relates in particular to a kind of filter apparatus that reclaims different types of solid catalyst particle from the moisture nitrate that contains inorganic process liquid, and this inorganic process liquid once was used to prepare in the production of hydroxylammonium by the method for hydrogenation nitrate or nitrogen oxide.
Background technology
The important use of hydroxyl ammonium salt is for preparing oxime from ketone or aldehyde, particularly by cyclohexanone, preparing cyclohexanone oxime.With regard to the preparation of this oxime, in known round-robin method, moisture acidic buffer reaction medium keeps circulation in the synthetic district of hydroxyl ammonium salt and the synthetic district of oxime.The buffer salt that reaction medium is derived by for example phosphoric acid and/or sulfuric acid and these acid, for example basic salt and/or ammonium salt acidic buffer.In the synthetic district of hydroxyl ammonium salt, with hydrogen, nitrate ion or oxynitrides are transformed into to azanol.Azanol reacts with free buffering acid and forms corresponding hydroxyl ammonium salt, and by this synthetic district of hydroxyl ammonium salt input oxime, it generates corresponding oxime with reactive ketone there, discharges sour simultaneously subsequently.Isolate oxime from reaction medium after, reaction medium is recycled to the synthetic district of hydroxyl ammonium salt and adds new nitrate ion or oxynitrides in reaction medium.
In the situation that synthesize hydroxyl ammonium salt with phosphoric acid and nitrate solution, above-mentioned chemical reaction is expressed as follows:
Reaction 1) prepare hydroxylammonium in the synthetic district of hydroxyl ammonium salt;
2H
3PO
4+NO
3-+3H
2→NH
3OH++2H
2PO
4-+2H
2O
Reaction 2) prepare oxime in the synthetic district of oxime:
Reaction 3), after isolating the oxime of formation, with the form of HNO3, supplement new nitrate ion:
H
3PO
4+H
2PO
4-+HNO
3+3H
2O→2H
3PO
4+NO
3-+3H
2O
First reaction is heterogeneous catalysis.Preferably, catalyst is usingd the form of homodisperse solid and is existed as the decentralized photo in liquid reaction mixture.
The mixture of reaction products of the first step is to contain the moisture inorganic process liquid of solid catalyst particle suspended substance in hydroxylammonium salt solution.
This moisture inorganic process liquid being input to the synthetic district's (reacting 2) of oxime before, preferably from this moisture inorganic process liquid, isolate solid catalyst particle.After filtration, this inorganic process liquid is hydroxylammonium salt solution filtrate.
The catalyst used in hydroxyl ammonium salt in preparation mainly is comprised of the metal that is selected from platinum family, such as being positioned at, on carbon carrier for example, usings palladium or (palladium+platinum) catalyst as active component.Can activate this catalyst by there being one or more catalyst activators.Catalyst activator can be to be selected from copper, silver, cadmium, mercury, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony and bismuth.Most preferably, this catalyst activator is germanium.Containing the compound of described element, for example oxide, nitrate, phosphate, sulfate, halide and acetate also can be used as catalyst activator.Element described in US3767758 or their compound, can be directly as catalyst or be added in reaction medium.
The catalyst that (reacts 1) use in preparing hydroxylammonium salt solution, preferably contain the heavy metal be positioned on carrier, is preferably placed at the platinum (Pt) on carrier, palladium (Pd) or platinum and palladium composition.
Although usually tend to use pure palladium, pure palladium may contain certain platinum impurity, palladium in pure palladium: the part by weight of platinum can be different.Preferably palladium contains the platinum lower than 25wt%, more preferably less than 5wt%, further preferably lower than 2wt%, particularly preferably lower than the platinum of 1wt%.
Preferably, carrier comprises carbon (for example graphite, carbon black, or activated carbon) or alumina support, is more preferably graphite or activated carbon.The catalyst used in the synthetic district of hydroxyl ammonium salt preferably contains the heavy metal of 1-25wt%, and the more preferably heavy metal of 5-15wt%, with respect to the gross weight of carrier and catalyst.
As a rule, the consumption of the catalyst in the synthetic district of hydroxyl ammonium salt is 0.05-25wt%, is preferably 0.2-15wt%, is more preferably 0.5-5wt%, with respect to the inorganic process liquid gross weight in the synthetic district of hydroxyl ammonium salt.
The particle mean size of catalyst granules is generally 1-150 μ m, and preferably 5-100 μ m, be more preferably 5-60 μ m, especially 5-40 μ m.The particle that so-called " particle mean size " refers to 50vol% is greater than nominal diameter.
Preferably, the content of this catalyst activator is the 0.01-100mg/g catalyst, and preferably the 0.05-50mg/g catalyst, be more preferably the 0.1-10mg/g catalyst, is most preferably the 1-7mg/g catalyst.
In fact, although this technique is a continuous process, catalyst loss it is selective and/or active, and need regular update.
Optionally definition is the mol ratio of hydroxylammonium output and proton (H+) consumption, and one of them hydroxylammonium needs two protons (H+).' hydroxylammonium is selective ' used herein (to product of hydroxylammonium selective) is defined as: 2 times of the amount of hydroxyl ammonium that reaction zone produces consume the mol ratios of H+ amount with reaction zone.Low selectively meaning can produce more undesirable accessory substances.
The activity of catalyst per hour is defined as the grams that every gram catalyst produces hydroxylammonium herein.In other words, the generation velocity correlation of activity and hydroxylammonium.
Catalyst weight used herein refers to the dry weight of catalyst, the weight of any carrier that comprises the active catalytic species useful place.
The replacing of catalyst needs every 4 weeks to every 3 years once.In general, by filtering all used catalysts, then change fresh catalyst into, or often a part of used catalyst is removed to the also fresh catalyst of regular replenishment and reclaimed used catalyst.
Yet the difficult problem of a known reclaimer is to be difficult to effectively reclaim catalyst, and can lose a large amount of catalyst the process that reclaims catalyst from filter, need the plant operations work more to keep an eye on simultaneously, this is a job consuming time.So valuable catalyst can be lost and need to more operative employee.
The utility model content
Therefore, the purpose of this utility model is to provide a kind of filter apparatus, no matter be to reclaim all catalyst or recovery section catalyst only, the method has higher efficiency and shirtsleeve operation technique.
Typical leaf filter, Niagara filter for example, comprise the shell of the filter leaf that contains maximum 30 dismountable bottom margins that are fixed on shell.Preferably, filter leaf is to make lower than the stainless steel of 110 microns mesh by having preferably.Leaf filter comprises a lot of levels or vertical blade, also comprises the commercially available Niagara filter with vertical filter leaf.
JP07275614 describe a kind of lobate filter wherein by the filter leaf radial arrangement to raise the efficiency.
In general, filter vane is to consist of rib, and covers with the rove net, and rove is on the net with the metal filter screen of meticulousr establishment, and this metal filter screen can be held back for example filtering particle filter cake of catalyst granules.
If use typical Niagara filter, spray filter and collect washing lotion suspension by flushing or water, realize reclaiming catalyst from filter.But, still need to process to reduce the content of salt content, especially nitrate with rear suspension liquid, and need dry the processing to remove moisture to guarantee the recovery in arbitrary heavy metal later stage in solid catalyst particle.
In the utility model, adopt the leaf filter with the filter leaf covered with filter cloth to reclaim catalyst, the rate of recovery of catalyst has improved at least 15%, and reclaims catalyst and again start the time shorten of reaction needed from filter.
Therefore, according to the utility model, it provides a kind of filter apparatus that reclaims solid catalyst particle from moisture inorganic process liquid, it is the leaf filter that contains at least 1 to 30 filter leaf, wherein at least one filter leaf covers with filter cloth, and moisture inorganic process liquid is used for the production of azanol by filter plant.
As everyone knows, a series of steel can be used for producing container, pipeline and the reactor for the preparation of azanol.This comprises steel 304,316,304L or 316L steel grade difference, and the content of molybdenum and other metals is also different.In addition, the content of carbon and other elements also can have influence on the corrosion resistance of reactor.
The scope maximum of steel 304 and 316 carbon content is 0.08wt%, steel 304L and 316L, and the scope maximum of carbon content is 0.030wt%.
Every other elemental range substantially the same (for example, for steel 304, the scope of nickel is 8.00-10.50wt%, and for steel 304L, the scope of nickel is 8.00-12.00wt%).
For the risk (welding decay) of the intercrystalline corrosion that overcomes the application initial stage, lower carbon content ' variant ' (316L) is developed out the steel (316) that have " standard " carbon content for substituting.Conclusion is the 450-850 ℃ of temperature whether steel can bear a few minutes, depends on temperature and the severe corrosive environment exposed subsequently.Subsequently, corrosion occurs at crystal grain boundary.
Most of steel contain certain molybdenum, well-known, and molybdenum has damaged the selective of hydroxylammonium reaction, and for example in reaction medium, the 1ppm molybdenum can cause the hydroxylammonium elective reduction to surpass 2%.Liquid property and mesh fineness that rely on to use, the mesh solubilized also for example discharges molybdenum in the solution that will filter.
Preferably the filter leaf of filter apparatus of the present utility model contains
I) there is the stainless (steel) wire lower than 110 microns mesh; With
Ii) described stainless steel contains 0-0.08wt% carbon and 0-0.03wt% molybdenum.
More preferably the carbon content of steel is 0-0.03wt% carbon.If carbon content lower than 0.030wt%, is exposed under said temperature, especially ' thick ' section at steel normally exposes a period of time by the heat affected area of pad, so just the corrosion of intergranular can not occur.Low carbon type is also easier than the welding of standard carbon type.
Steel also can be annealed.Annealing is the heat treatment that for example intensity and hardness change of a kind of performance that causes material.The production process of annealing conditions is that heating surpasses above-mentioned recrystallization temperature, keeps applicable temperature, cooling subsequently.For steel, this process be fully heating material a period of time (generally being heated to aglow) then cooling.But annealing can not reduce carbon content can make element be more evenly distributed, thereby has improved corrosion resistance.
What more preferably, the utility model was used is that austenitic steel is as filter leaf.
Austenite, be also referred to as γ phase iron, be a kind of nonmagnetic metal iron or iron solid solution allotrope and contain alloying element.In ordinary carbon steel, austenite is present in above-mentioned critical eutectoid temperature 1, in 000K (1,340 °F); Other steel alloys have different eutectoid temperatures.
Preferably described steel basically comprises the following steel formed and forms by being selected from:
Quenching annealed steel A comprises 0 – 0.08wt% carbon, 0 – 2.0wt% manganese, 0 – 2.0wt% silicon, 0 – 0.045wt% phosphorus, 0 – 0.03wt% sulphur, 17 – 21wt% chromium, 0 – 0.03wt% molybdenum, 8.0 – 13wt% nickel;
Mild steel B comprises 0 – 0.03wt% carbon, 0 – 2.0wt% manganese, 0 – 1.0wt% silicon, 0 – 0.045wt% phosphorus, 0 – 0.03wt% sulphur, 17 – 21wt% chromium, 0 – 0.03wt% molybdenum, 8.0 – 13.0wt% nickel;
Stabilized steel C comprises 0 – 0.08wt% carbon, 0 – 2.0wt% manganese, 0 – 2.0wt% silicon, 0 – 0.045wt% phosphorus, 0 – 0.04wt% sulphur, 17 – 21wt% chromium, 0 – 0.03wt% molybdenum, 9.0 – 13.0wt% nickel and or titanium (minimum: 5 times of wt% Tan – maximums: 0.8wt%) or niobium+tantalum (minimum: 8 times of wt% Tan – maximums: 1.1wt%).
In a specific embodiments, according to the utility model, it provides the filter apparatus that reclaims different types of solid catalyst particle the moisture nitrate from containing inorganic process liquid, and this inorganic process liquid once was used to the production for preparing hydroxylammonium by hydrogenation nitrate or oxynitrides.
The side that filter cloth can only be positioned at filter leaf also can be positioned at the both sides of filter leaf.
Preferably, in the utility model, with filter cloth, cover the filter leaf both sides.This makes filter efficiency higher.Preferably, filter cloth is a kind of cloth that is easy to dismounting.Filter cloth is applied to filter leaf and can includes but not limited to by any method use the cloth frame with clip, cloth is sewn on filter leaf, encase filter leaf (as socks) with the cloth bag of an end opening, perhaps for example, with (: cloth bag VelcroTM) being with zipper accessory or hook eye accessory, after perhaps being applied in filter leaf, by the cloth overseam.
Preferred filter cloth comprises a kind of cloth of polymer, is more preferably a kind of polypropylene cloth.Preferably, polypropylene cloth is knitting.Preferably, filter cloth has the mesh lower than 70 microns.
Before the filtration of being reclaimed catalyst granules, can add the independent suspension that contains silicon or carbon granule in process liquid, form filter cake thereby be applied to one deck particle on the woven wire of filter leaf.This is also referred to as the pre-coating step.Due to the size of woven wire, implementing this step on filter leaf needs 24 hours at most according to the size difference of metal twine.Start subsequently to filter solid catalyst particle from moisture inorganic process liquid.Due to any particle added in the pre-coating process for example silicon or carbon granule can and the catalyst granules mixing, the removal process of heavy metal is had a negative impact.
Therefore, preferably with catalyst material itself as the precoating layer of cloth and in by the filter apparatus filter process catalyst granules form filtering layer on filter cloth.Owing to having used filter cloth, carry out the time of pre-coating and reduced widely, and owing to having used catalyst itself, make particle for example silicon or carbon granule and catalyst do not blend together mutually for may, also simplified the removal process of heavy metal.
Reclaim the purpose of dry as far as possible catalyst in order fully to reclaim heavy metal (wherein).In addition, for security consideration, the catalyst of recovery should not contain nitrate.
Therefore, for reclaiming catalyst, need in leaf filter, carry out following step, i.e. water rinsing step and drying steps.
After drying, remove the catalyst that filter cake is collected with recovery.
Catalyst (filter cake) is scraped from filter cloth, thereby burn filter cake, reclaim the cloth that heavy metal or burning cover on filter cake and also make cloth decompose and make the heavy metal in catalyst be reclaimed.
If scrape catalyst (normal is mechanical) from filter cloth, filter cloth can reuse repeatedly, and, in a filtration cycle, catalyst recovery is improved.Removing filter cloth and applying new filter cloth is easy to many than the cleaning filter leaf.
The production equipment for preparing moisture hydroxylammonium salt solution can be any applicable reactor, for example there is the reactor of mechanical agitator or there is the reactor of operation post, and be more preferably the reactor with bubble column.NL6908934 has described the example of suitable bubble column.
Typical reactor configurations for the preparation of moisture hydroxylammonium salt solution is the hydrogenation steam bubble column type reactor with cooling section.Reactor configurations usually comprises the gas separator tube of a lot of groups and, for separating of the screen pipe of solid catalyst particle, this screen pipe contains at least one Niagara filter.
Inorganic process liquid is input to the screen pipe containing the filter element that is useful on first step filtration from the bubble column reactor by the gas separator tube.A certain amount of hydroxylammonium salt solution filtrate (usually in the 3-10% left and right) is input to filtrate pipe from screen pipe, is input to the filtrate separator tube from filtrate pipe afterwards again, then from the filtrate separator tube, is input to the synthetic district of oxime.Hydrogenation bubble column cooling at cooling section is got back in remaining hydroxylammonium salt solution filtrate (usually in the 97-90% left and right) input.Last in filtration cycle, reclaim dead catalyst.
Preferably, contain<3ppm of hydroxylammonium salt solution filtrate molybdenum, more preferably<2.5ppm molybdenum, most preferably<2.0ppm molybdenum, especially<1.5ppm molybdenum.In hydroxylammonium salt solution filtrate, the molybdenum of 3ppm is equivalent to 0.0003wt%.
In another embodiment of the present utility model, a kind of filter apparatus that reclaims solid catalyst particle from moisture inorganic process liquid is provided, it is the leaf filter that contains at least 1 to 30 filter leaf, wherein at least one filter leaf covers with filter cloth, and moisture inorganic process liquid is used for the production of azanol by filter plant.Comprise following method:
A) pre-coating to form filter cake on filter cloth;
B) filter with the collection catalyst particle;
C) rinse the filter cake on filter cloth;
D) with the filter cake on the dry filter cloth of overheated low-pressure steam;
E) with the filter cake on the dry also cooling filter cloth of inert gas;
F) remove the filter cloth with the catalyst granules of collecting from filter leaf; And/or
G), from the filter cloth that covers filter leaf, machinery is removed the catalyst granules of collecting;
Wherein said filter leaf contains
I) there is the stainless (steel) wire lower than 110 microns mesh; With
Ii) described stainless steel contains 0-0.08wt% carbon and 0-0.03wt% molybdenum.
Optional, optionally remove blade from leaf filter.
Preferably, inert gas is nitrogen.
Subsequently, reclaim heavy metal from the catalyst granules of collecting.
The accompanying drawing explanation
Fig. 1 is shown as the cross-sectional view of leaf filter.In this embodiment, Niagara filter (1) comprises two parts (2) and (3) after opening, and by flange (4), is connected.Partly (3) comprise dismountable filter leaf (5) that is positioned at bottom (6).Filter leaf (5) and bottom (6) are combined into lobate filter.These filter leaves (5) two sides all uses filter cloth (7) to cover.
The specific embodiment
The utility model further illustrates by following embodiment, but is not limited to this.
A basis
in the hydroxylammonium phosphate oxime device of technology continued operation, filter moisture inorganic process liquid (moisture hydroxylammonium salt solution) by the Niagara filter apparatus and fully remove catalyst granules wherein.The particle mean size of catalyst granules (10wt% palladium/activated carbon) is about 15 μ m.
The catalyst granules that inorganic process liquid contains average 1.2wt%, and with Niagara filter filtering inorganic process liquid, this filter has steel filter leaf that 20 of 100 microns mesh contain 0-0.03wt% carbon and 0-0.03wt% molybdenum and a) polypropylene filter cloth (60 micron pore size) and b) no filter-fabric is arranged in a filtration cycle.Filter cloth just as same ' socks ' around each filter, therefore, filter cloth is the both sides that are positioned at plate.After being placed on filter by ' socks ', flow out the openend of sealing filter cloth in order to stop liquid and catalyst granules from filter cloth.
In recovery method, use be to there is the Niagara filter apparatus that 20 filter leaves and each blade cover with filter cloth, the method comprises the steps:
A) pre-coating: be to form the pre-filtration step of filter cake internal layer on filter cloth, by the inorganic process liquid that contains catalyst granules, carry out the pre-coating step;
B) filter with the collection catalyst particle;
C) rinse the filter cake on filter cloth in order to remove nitrate ion with downstream water, the first of filtrate can reuse, until the conductance of filtrate drops to below 1000 μ S/cm, stops rinsing;
D) with the filter cake on the dry filter cloth of overheated low-pressure steam;
E) with the filter cake on nitrogen drying cooling filter cloth;
F) open the Niagara filter;
G) catalyst granules (moisture content 50-60wt%) of collecting is mechanically removed from filter cloth.
The catalyst of then collecting by burning reclaims heavy metal wherein.
In another embodiment, from filter leaf, remove the filter cloth with the catalyst granules of collecting (moisture content 50-60wt%), burn afterwards this filter cloth and reclaim the heavy metal in the catalyst granules of collecting.
In first embodiment, add catalyst in the inorganic process liquid of certain volume.Use this filter plant, the recovery total of heavy metal is 225kg, but when not using filter cloth, the heavy metal overall recovery only 195kg. therefore, owing to having used filter cloth, the heavy metal of recovery has increased by 15%.
And the time of pre-coating reduced to less than 2 hours from 24 hours.Measure molybdenum content the be found to be<1ppm of hydroxylammonium salt solution filtrate.
Claims (8)
1. a filter apparatus that reclaims solid catalyst particle from moisture inorganic process liquid, be the leaf filter that contains at least 1 to 30 filter leaf, and wherein at least one filter leaf covers with filter cloth.
2. filter apparatus according to claim 1, wherein filter leaf consists of austenitic steel.
3. according to the filter apparatus of claim 1, wherein filter cloth comprises the polypropylene cloth.
4. according to the filter apparatus of claim 3, wherein the polypropylene cloth is knitting.
5. according to the filter apparatus of claim 1, wherein filter cloth has the mesh lower than 70 microns.
6. according to the filter apparatus of claim 1, wherein the two sides of filter leaf all covers with filter cloth.
7. according to the filter apparatus of claim 1, wherein filter cloth is got on divided by reclaiming catalyst granules from filter leaf.
8. according to the filter apparatus of claim 1, wherein filter cloth is applied to, on filter leaf, then filter cloth be sealed and closed with the form of the bag of an end opening.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201220746000.2U CN203370367U (en) | 2011-12-29 | 2012-12-28 | Filtering device used for recycling solid catalyst particles in water-containing inorganic process liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110451998 | 2011-12-29 | ||
| CN201110451998.3 | 2011-12-29 | ||
| CN201220746000.2U CN203370367U (en) | 2011-12-29 | 2012-12-28 | Filtering device used for recycling solid catalyst particles in water-containing inorganic process liquid |
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| CN203370367U true CN203370367U (en) | 2014-01-01 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113680117A (en) * | 2020-05-19 | 2021-11-23 | 维美德技术有限公司 | Blade type filter bag |
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2012
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113680117A (en) * | 2020-05-19 | 2021-11-23 | 维美德技术有限公司 | Blade type filter bag |
| CN113680117B (en) * | 2020-05-19 | 2023-08-18 | 维美德技术有限公司 | Vane type filter bag |
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Effective date of registration: 20160106 Address after: Holland Sittard Patentee after: CAP III B.V. Address before: Holland Heerlen Patentee before: DSM IP ASSETS B.V. |
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| CX01 | Expiry of patent term |
Granted publication date: 20140101 |
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