CN101921025B - Recycle of solid flocculation in nickel plating waste water - Google Patents
Recycle of solid flocculation in nickel plating waste water Download PDFInfo
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- CN101921025B CN101921025B CN 201010120556 CN201010120556A CN101921025B CN 101921025 B CN101921025 B CN 101921025B CN 201010120556 CN201010120556 CN 201010120556 CN 201010120556 A CN201010120556 A CN 201010120556A CN 101921025 B CN101921025 B CN 101921025B
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Abstract
The invention relates to a simple chemical method for recycling recycle solid flocculation extracted from industrial electroplating (nickel) waste water which is hard to treat as raw materials for electroplating (nickel). The method not only solves the difficulty of influencing environment, but also reduces the cost of raw materials in the industry. The solid flocculation after electroplating (nickel) waste water treatment is still a difficulty in the electroplating industry. Conventional methods are burning or land filling which can not solve the problem fundamentally. By adopting the method of the patent, the difficulty is easy to solve, and waste use is realized. The technology belongs to the environmental protection range, and the theory applied is that the solid flocculation-nickel hydroxide reacts with sulphuric acid to generate nickel sulfate, the chemical reaction formula is 2Ni(OH)2+H2SO4=NiSO4+2H2O. The chemical reaction is easy to carry out with little technical difficulties.
Description
One, technical field: the environment protection of electroplating (casting) industry production
Two, suitable application area: the solid flocculation thing recycling of industrial electro nickel plating
Three, background technology
The treatment process that solid precipitation thing after the electroplating wastewater processing is general is: burning or buried, this method can not fundamentally be eliminated it to the pollution of environment, and nickeliferous solids is returned the original production line again with then fundamentally having solved this problem after chemical treatment.
Four, summary of the invention:
The recycling of solid flocculation in nickel plating:
Inventive principle: the primary product with simple alkaline chemical precipitation method is nickel hydroxide, goes can become single nickel salt after the neutralization with sulfuric acid, and its reaction formula is: Ni (OH)
2+ H
2SO
4=NiSO
4+ 2H
2O
Five, technological process:
1, precondition: forbidding tap water in nickel plating workshop carries out operation, and printed nickel net factory preferably uses deionized water in the buffer operator order, worst also will be with softening water flushing and mill tire, general Electroplate Factory also wants so during common operation.
2, early-stage preparations: at first the solid flocculation thing is carried out mixing after the processing in small, broken bits, make it even, get the small portion chip and weigh, carry out the nickel content that assay is determined its unit weight, and calculate whole nickeliferous total amount, press again NiSO
4, 7H
2The reaction formula of O calculates the amount that should add sulfuric acid and water, contains excessive acid for fear of solution, and the acid adding amount 95% is got sulfuric acid ready by what answer dosage, gets water ready by 100% the water yield.
3, operation steps: all solids in small, broken bits is packed into acidproof, in the resistant to elevated temperatures container, all pour into the water (deionized water) of getting ready in the container afterwards, slowly whole sulfuric acid are added in the container again, acid adding speed will be noted liquid temperature (sulfuric acid entry meeting produces high temperature), general control is advisable about 80 ℃, acid adding to note simultaneously stirring so that solution evenly and maximum meltage arranged, lysate can be introduced behind the sufficient reacting and carry out the crystallization treatment first time in another empty receptacle: its method is to make it be down to normal temperature or lower from 80 ℃, so just have and crystallize out, its uncrystallized liquid is introduced another container and is carried out the crystallization treatment second time, its method is: available electrical heating method is warming up to 80 ℃, and insulation, evaporation for some time, after be cooled to again low temperature, at this moment have again and crystallize out.Twice crystallization can be put together, dissolves, and carries out the general goal reason.Liquid after large the processing can have been surveyed its nickel content, prepares against back former coating bath and replenishes its consumption.And uncrystallized raffinate is few during for the second time crystallization, can return for the second time crystallisation vessel or add solid-state chip dissolution vessel temperature adjustment usefulness, also will chemically examine its nickel content before returning, in order to participate in the whole calculating.Solution after large the processing also can carry out the recrystallize processing and become solid-state single nickel salt, as commodity selling.
4, the treating processes schematic diagram is seen " Figure of description "---solid flocculation in nickel plating recycling process flow chart
5, the large treatment process of attached nickel liquid:
Large treating processes can be reduced to: acidifying → oxidation → alkalization → activated carbon adsorption → orientation adds big event scavenging agent → several times filtration.
Specific practice is: transfer about pH value to 3 with sulfuric acid first, add-on is H
2SO
480~150ml/m
3Liquid temperature is cooled to below 30 ℃ again, behind the amount adding solution of dual oxide with 30% by 0.5~2ml/L, more than the warming while stirring to 60 ℃, and more than the insulation 1.5h, hydrogen peroxide is played one's part to the full, this purpose is to make ferrous iron all be converted into ferric iron, sexavalent chrome is converted into trivalent chromium etc., add new self-control nickelous carbonate again and transfer more than the pH value to 5, at this moment the oxyhydroxide such as ferric iron begins precipitation, adds powdered activated carbon adsorb organic compound by 1~2g/L again, stir and leave standstill more than 4 hours after 0.5 hour, after (liquid temperature maintains 50~60 ℃) solution is extracted the sand rod that wraps by filter paper and terylen cloth with vacuum pump and filter one time.Afterwards, in solution, add again directed quantitative Impurity removal agent (as going copper agent etc.), and after fully stirring makes it evenly, leave standstill for some time, refilter one time, can again this liquid be heated to 50~60 ℃ in order to increase filter effect, and continuous filtration twice, solution can use in return-enclosure generally speaking.
Six, description of drawings:
Accompanying drawing is solid flocculation in nickel plating recycling process flow chart.Concrete process flow is as follows:
1. operation is to pulverize: the solid flocculation thing is carried out pulverization process;
2. operation is to stir: chip is carried out uniform stirring;
3. operation is to survey unit content: get unit weight and analyze nickel content;
4. operation is to calculate total amount: press NiSO
47H
2O calculates to be needed with Total Water and total sulfuric acid amount;
5. operation gets the raw materials ready: by standby 100% water of the water yield, get sulfuric acid ready by 95% sulfuric acid;
6. operation is to carry out chemical reaction: slowly add the sulfuric acid (80 ℃ of temperature) (leaving remnants) of getting ready after adding first whole water;
7. operation is primary crystal: the solution that will react is put into the cooling ware, and crystallisation by cooling comes;
8. operation is recrystallize: top not crystallized liquid is put into another container carry out heating evaporation, crystallisation by cooling to the certain volume;
9. operation is that xln is processed greatly;
Operation 10-1 is reuse: liquid returns the coating bath fluid infusion;
Operation 10-2 is that crystallization is sold: liquid carries out recrystallize and sells;
Operation 11 is that raffinate returns: top not crystallized liquid is returned operation 8 or enter operation 6 temperature adjustments and use;
Operation 12: prepare next circulation.
Seven, embodiment:
This method is prepared to implement in Hebei province's Zhuozhou City three ring textile equipment company limiteds.Enforcement is finished nearly 50 of the backward whole nation and is promoted with the product industry, and other electronickelling industries also can be with reference to execution.
Claims (1)
1. process the processing method of solid flocculation in nickel plating with simple alkaline chemical precipitation method:
Process the solid flocculation thing that nickel-plating waste water produces with simple alkaline chemical precipitation method and be mainly nickel hydroxide, this product with in the sulfuric acid with can generate single nickel salt, its chemical equation is:
Ni (OH)
2+ H
2SO
4=NiSO
4+ 2H
2Its technological process of O is as follows:
1.1 precondition: forbidding tap water in nickel plating workshop carries out operation, and printed nickel net factory preferably uses deionized water in the buffer operator order, worst also will be with softening water flushing and mill tire, general Electroplate Factory also wants so during common operation;
1.2 early-stage preparations: at first the solid flocculation thing is carried out mixing after the processing in small, broken bits, make it even, get the small portion chip and weigh, carry out the nickel content that assay is determined its unit weight, and calculate whole nickeliferous total amount, press again NiSO
4, 7H
2The reaction formula of O calculates the amount that should add sulfuric acid and water, contains excessive acid for fear of solution, and the acid adding amount 95% is got sulfuric acid ready by what answer dosage, gets water ready by 100% the water yield;
1.3 operation steps: all solids in small, broken bits is packed into acidproof, in the resistant to elevated temperatures container, all pour into the deionized water of getting ready in the container afterwards, slowly whole sulfuric acid are added in the container again, acid adding speed will be noted liquid temperature, general control is advisable at 80 ℃, acid adding to note simultaneously stirring so that solution evenly and maximum meltage arranged, behind the sufficient reacting lysate introduced and carry out the crystallization treatment first time in another empty receptacle: its method is to make it be down to normal temperature or lower from 80 ℃, so just have and crystallize out, its uncrystallized liquid is introduced another container and is carried out the crystallization treatment second time, its method is: be warming up to 80 ℃ with electrical heating method, and insulation, be cooled to again low temperature after evaporation for some time, at this moment have again and crystallize out, twice crystallization, put together, dissolve, and carry out general goal and manage, liquid after large the processing, survey good its nickel content, prepare against back former coating bath and replenish its consumption, and uncrystallized raffinate is few during for the second time crystallization, return for the second time crystallisation vessel or add solid-state chip dissolution vessel temperature adjustment and use, also to chemically examine its nickel content before returning, in order to participate in the whole calculating, solution after large the processing carries out the recrystallize processing and becomes solid-state single nickel salt, as commodity selling;
1.4 the large treatment process of nickel liquid: large treating processes can be reduced to: acidifying → oxidation → alkalization → activated carbon adsorption → orientation adds big event scavenging agent → several times filtration;
Specific practice is: transfer pH value to 3 with sulfuric acid first, add-on is H
2SO
480~150ml/m
3Liquid temperature is cooled to below 30 ℃ again, behind the amount adding solution of hydrogen peroxide with 30% by 0.5~2ml/L, more than the warming while stirring to 60 ℃, and more than the insulation 1.5h, hydrogen peroxide is played one's part to the full, this purpose is to make ferrous iron all be converted into ferric iron, sexavalent chrome is converted into trivalent chromium, adds new self-control nickelous carbonate again and transfers more than the pH value to 5, and at this moment ferric hydroxide begins precipitation, add powdered activated carbon adsorb organic compound by 1~2g/L again, stir and leave standstill more than 4 hours after 0.5 hour, liquid temperature remains on 50~60 ℃, after solution extracted the sand rod that wraps by filter paper and terylen cloth with vacuum pump filter one time, afterwards, in solution, add again directed quantitative Impurity removal agent, and after fully stirring makes it evenly, leave standstill for some time, refilter one time, can again this liquid be heated to 50~60 ℃ in order to increase filter effect, and continuous filtration twice, solution can use in return-enclosure generally speaking.
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CN 201010120556 CN101921025B (en) | 2010-03-10 | 2010-03-10 | Recycle of solid flocculation in nickel plating waste water |
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CN 201010120556 CN101921025B (en) | 2010-03-10 | 2010-03-10 | Recycle of solid flocculation in nickel plating waste water |
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CS268094B1 (en) * | 1987-03-18 | 1990-03-14 | Krcma Ladislav | Method of thermical liquidation of used denickeling bath |
JPH07267616A (en) * | 1994-03-28 | 1995-10-17 | Nippon Chem Ind Co Ltd | Method for treating aged electroless nickel plating liquid |
CN1108885C (en) * | 2000-06-06 | 2003-05-21 | 广东工业大学 | Technological process using electroplating sludge as resource to make harmless treatment |
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