CN104030369B - A kind of method utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs - Google Patents
A kind of method utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs Download PDFInfo
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Abstract
The invention discloses a kind of method utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs, its innovative point is in that: in nickel-containing waste water, nickel is measurement criteria, puts into hydrated calcium chloroaluminate according to mass ratio, react at normal temperatures, isolating precipitate, precipitate is dried, and obtains NiAl-HTLcs. This method utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs of the present invention, develop a kind of effective way, chromium in abundant recycling waste water, turn waste into wealth, turn harm into good, waste water has effectively been processed while making full use of nickel heavy metal, nickel-containing waste water is after hydrated calcium chloroaluminate intercalation is replaced, and nickel clearance reaches 90%, reaches the standard of safety dumping; The processing method of the present invention will not produce mud, it is to avoid with the secondary pollution transfer that the form of solid waste causes, making full use of middle water and filter cake, economic and environment-friendly, efficiency is high.
Description
Technical field
The present invention relates to a kind of method utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs, belong to environmental conservation, Treated sewage reusing, function nano technical field.
Background technology
The nearly family more than 10,000 of Electroplate Factory of China. The waste water of annual discharge there are about 4O hundred million m3. Nickel-containing waste water is one of main wastewater source of electroplating industry. Nickel has strong toxicity, is International Contre research center and the carcinogen of U.S.'s toxicology tissue announcement. There is obvious carcinogenesis. Sexavalence nickel compound can not be decomposed by the microorganisms at nature. And infiltration migration is stronger. Human body is had strong sensitization. Therefore, dealing carefully with Treating Electroplate Wastewater Containing Nickel. It it is an environmental problem that must solve in electroplating industry.
Process currently for Treating Electroplate Wastewater Containing Nickel mainly adopts chemical reduction method, electrolysis, absorption method, microbial method, extraction etc.
The ultimate principle of chemical reduction method is to be reduced by nickel with reducing agent, then adds flocculant by nickel flocculation sediment, to realize solid-liquid separation.
Electrolysis is the method utilizing nickel generation electrochemical reaction in electrode and waste water and eliminating its toxicity, belongs to electrochemical process.
Absorption method is to utilize porous solid material absorption water pollutant to process a kind of common method of waste water.
In recent years. along with biological engineering the reach of science, the people increasingly deeper people of understanding to microorganism, utilize microbial method also to cause the concern of people gradually to process nickel-containing waste water.
Extraction is the unit operation utilizing nickel to have different dissolubility to be isolated in different solvents.
Hydrotalcite-based compound includes brucite and houghite, and its main body is generally made up of the hydroxide of two kinds of metals, is also called layered di-hydroxyl composite metal oxidate (LayeredDoubleHydroxide, LDH).
Up to the present, the preparation of hydrotalcite-based compound mainly has following several method:
1. coprecipitation
The most frequently used synthetic method of brucite is exactly coprecipitation, namely occurs co-precipitation to prepare LDHs with the mixed solution of metal ion and aqueous slkali mixing that constitute neatly rock layers at a certain temperature.
2. ion exchange
When metal ion instability in alkaline medium, when coprecipitation cannot be carried out, ion exchange can be adopted. Ion exchange is from given brucite, is immersed in the solution containing the anion in target brucite by given brucite, by the exchange interaction of desired anion Yu the original interlayer anion of brucite, forms new post layer.
3. salt monoxide synthetic method
The method is to be proposed by boehn etc. for 1977, and its preparation method is, by oxide suspension with excessive aqueous chloride solution in room temperature reaction a couple of days, obtains consisting of hydrotalcite product. Preparing LDHs by the method is a kind of simple solid-liquid reaction.
4. induced hydrolysis method
This method is to be added to by the suspension of the hydroxide of trivalent metal in the saline solution of divalent metal, is stirred vigorously lower dropping (acid or alkali) solution to keep certain pH value.
5. roast reduction process
This method is built upon the preparation method on LDHs " memory effect " (memoryeffect) characteristic basis. Baked brucite at a certain temperature joined the aqueous solution containing desired anion or is placed in vapor atmosphere, by occurring the reconstruction of LDHs layer pole structure, anion and hydrone to enter interlayer, forming new LDHs.
6. sol-gel method
Prine etc. adopt sol-gel method to synthesize organic anion brucite. Its synthetic reaction is metal alkoxide hydrolysis in HCI aqueous solution. Product prepared by product prepared by this method and other method is all different in morphological characteristic, thermal decomposition process, and the specific surface area of roasting gained composite oxides is higher by 10% than Co deposited synthesis product. But owing to this method is organic reaction, side reaction makes productivity not high; Crystal morphology is imperfect; Agglomeration is serious; And organo-metallic compound, poisonous, expensive, be not suitable for large-scale industrial production; So method is not appropriate for the synthesis of all of houghite.
7. hydrothermal synthesis method
Hydrothermal synthesis method, is similar to magnesium sulfate, aluminum sulfate mixture solution and aqueous slkali and to mix rapidly generation white serosity, poured in autoclave by serosity, then reactor is put into crystallization in the baking oven of different temperatures obtains a series of brucite.
8. microwave process for synthesizing
Similar with coprecipitation, aqueous slkali and saline solution mix and blend are prepared serosity. Then, serosity is inserted in microwave oven, high temperature crystallization tens minutes, wash, filter, dry to obtain brucite.
Summary of the invention
It is an object of the invention to provide a kind of method utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs, to solve a still unsolved difficult problem in above-mentioned prior art.
The technical solution used in the present invention is: a kind of method utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs, its innovative point is in that: in nickel-containing waste water, nickel is measurement criteria, hydrated calcium chloroaluminate is put into according to mass ratio, react at normal temperatures, isolate precipitate, precipitate is dried, and obtains NiAl-HTLcs.
Further, the described method utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs concretely comprises the following steps and is slowly added to accurately measure the ground hydrated calcium chloroaluminate pulverized under stirring at normal temperature in nickel-containing waste water, lower stirring that the temperature remains within the normal range, arranging the stirring reaction time is 8～96 hours, stirring to the complete intercalation of nickel is replaced after generating NiAl-HTLcs in hydrated calcium chloroaluminate, post was descended to realize solid-liquid separation precipitate through room temperature, the time of staying is after 4～24 hours, drain direct discharge, precipitate is dried, arranging drying temperature is 80～500 DEG C, finally grind to finished product.
Further, described hydrated calcium chloroaluminate input amount is 1:10～20 with the mass ratio of nickel in nickel-containing waste water.
Further, described hydrated calcium chloroaluminate input amount is 1:13～17 with the mass ratio of nickel in nickel-containing waste water.
Further, described nickel-containing waste water includes organic nickel waste water, inorganic nickel waste water and organic-inorganic composite waste; Described organic nickel waste water is nickel acetate waste water; Described inorganic nickel waste water is nickel sulfate, Nickel dichloride. or nickel oxide waste water; Described organic-inorganic composite waste be organic nickel waste water with inorganic nickel waste water arbitrarily than mixed solution.
Further, the calcium aluminum ratio of described hydrated calcium chloroaluminate is 1.5～6:1.
Further, the calcium aluminum ratio of described hydrated calcium chloroaluminate is 2～4:1.
Further, under described room temperature, the stirring reaction time is 12～48 hours.
Further, described room temperature descended the time of staying of post to be 8～12 hours.
Further, described precipitate dries temperature is 120～270 DEG C.
The invention have the benefit that this method utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs of the present invention, develop a kind of effective way, chromium in abundant recycling waste water, turn waste into wealth, turn harm into good, waste water has effectively been processed while making full use of nickel heavy metal, nickel-containing waste water is after hydrated calcium chloroaluminate intercalation is replaced, and nickel clearance reaches 90%, reaches the standard of safety dumping; The processing method of the present invention will not produce mud, it is to avoid with the secondary pollution transfer that the form of solid waste causes, making full use of middle water and filter cake, economic and environment-friendly, efficiency is high.
Detailed description of the invention
Following enforcement row can make those skilled in the art be more completely understood by the present invention, but does not therefore limit the present invention among described scope of embodiments.
Embodiment 1
It is 128mg/l at nickel concentration, COD is in 1 ton of waste water of 108mg/l, stirring is lower slowly puts into hydrated calcium chloroaluminate 100Kg, stirring at normal temperature is set 12 hours, is discharged to sucking filtration bucket, descended post to realize solid-liquid separation precipitate through room temperature, the time of staying is after 4～24 hours, draining direct discharge, precipitate is dried, and finally grinds to finished product;
The wastewater mother liquor of the nickeliferous 0.5mg/l being wherein filtrated to get, Treated sewage reusing is to electroplating work procedure; Filter cake is calcium chromium class garnet, through 150 DEG C of bakings, grinds packaging selling by grade.
The method utilizing nickel-containing waste water intercalation production NiAl-HTLcs in the present embodiment, nickel concentration is reduced to 0.5mg/l by original 128mg/l, reaches the standard of safety dumping; The processing method of the present embodiment will not produce mud, it is to avoid with the secondary pollution transfer that the form of solid waste causes, making full use of middle water and filter cake, economic and environment-friendly, efficiency is high.
Embodiment 2
It is 100mg/l at nickel concentration, COD is in 1 ton of waste water of 90mg/l, stirring is lower slowly puts into hydrated calcium chloroaluminate 90Kg, stirring at normal temperature is set 12 hours, is discharged to sucking filtration bucket, descended post to realize solid-liquid separation precipitate through room temperature, the time of staying is after 4～24 hours, draining direct discharge, precipitate is dried, and finally grinds to finished product;
The wastewater mother liquor of the nickeliferous 0.45mg/l being wherein filtrated to get, Treated sewage reusing is to electroplating work procedure; Filter cake is calcium chromium class garnet, through 150 DEG C of bakings, grinds packaging selling by grade.
The method utilizing nickel-containing waste water intercalation production NiAl-HTLcs in the present embodiment, nickel concentration is reduced to 0.45mg/l by original 100mg/l, reaches the standard of safety dumping;The processing method of the present embodiment will not produce mud, it is to avoid with the secondary pollution transfer that the form of solid waste causes, making full use of middle water and filter cake, economic and environment-friendly, efficiency is high.
Claims (8)
1. one kind utilizes the method that nickel-containing waste water intercalation produces NiAl-HTLcs, it is characterised in that: in nickel-containing waste water, nickel is measurement criteria, puts into hydrated calcium chloroaluminate according to mass ratio, react at normal temperatures, isolating precipitate, precipitate is dried, and obtains NiAl-HTLcs;
Concretely comprise the following steps and be slowly added to accurately measure the ground hydrated calcium chloroaluminate pulverized under stirring at normal temperature in nickel-containing waste water, lower stirring that the temperature remains within the normal range, arranging the stirring reaction time is 8～96 hours, stirring to the complete intercalation of nickel is replaced after generating NiAl-HTLcs in hydrated calcium chloroaluminate, post was descended to realize solid-liquid separation precipitate through room temperature, the time of staying is after 4～24 hours, drain direct discharge, precipitate is dried, arranging drying temperature is 80～500 DEG C, finally grinds to finished product;
Described hydrated calcium chloroaluminate input amount is 1:10～20 with the mass ratio of nickel in nickel-containing waste water.
2. the method utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs according to claim 1, it is characterised in that: described hydrated calcium chloroaluminate input amount is 1:13～17 with the mass ratio of nickel in nickel-containing waste water.
3. the method utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs according to claim 1, it is characterised in that: described nickel-containing waste water is organic nickel waste water, inorganic nickel waste water or organic-inorganic composite waste; Described organic nickel waste water is nickel acetate waste water; Described inorganic nickel waste water is nickel sulfate, Nickel dichloride. or nickel oxide waste water; Described organic-inorganic composite waste be organic nickel waste water with inorganic nickel waste water arbitrarily than mixed solution.
4. the method utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs according to claim 1, it is characterised in that: the calcium aluminum ratio of described hydrated calcium chloroaluminate is 1.5～6:1.
5. the method utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs according to claim 1, it is characterised in that: the calcium aluminum ratio of described hydrated calcium chloroaluminate is 2～4:1.
6. the method utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs according to claim 1, it is characterised in that: under described room temperature, the stirring reaction time is 12～48 hours.
7. the method utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs according to claim 1, it is characterised in that: described room temperature descended the time of staying of post to be 8～12 hours.
8. the method utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs according to claim 1, it is characterised in that: it is 120～270 DEG C that described precipitate dries temperature.
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| CN112707448B (en) * | 2020-12-07 | 2022-06-21 | 中南大学 | Hydrotalcite-like compound, preparation method thereof and application thereof in arsenic removal |
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| CN103191784A (en) * | 2013-03-28 | 2013-07-10 | 北京化工大学 | Magnetic nickel aluminum hydrotalcite composite material loaded with gold nanoparticles and application thereof for catalyzing reduction reaction of p-nitrophenol |
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| CN103191784A (en) * | 2013-03-28 | 2013-07-10 | 北京化工大学 | Magnetic nickel aluminum hydrotalcite composite material loaded with gold nanoparticles and application thereof for catalyzing reduction reaction of p-nitrophenol |
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| Title |
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| Friedel 盐对废水中低浓度Cd2+的吸附动力学;张娟娟 等;《过程工程学报》;20120831;第12卷(第4期);第590-595页 * |
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