CN104030369A - Method for producing nickel aluminum hydrotalcite by utilizing nickel-containing wastewater intercalation - Google Patents
Method for producing nickel aluminum hydrotalcite by utilizing nickel-containing wastewater intercalation Download PDFInfo
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Abstract
The invention discloses a method for producing nickel aluminum hydrotalcite by utilizing nickel-containing wastewater intercalation. The method is innovatively characterized by comprising the following steps: by taking nickel in nickel-containing wastewater as measurement standard, adding hydrated chloride calcium aluminate according to a mass ratio, reacting at normal temperature, separating the precipitate, drying the precipitate, and obtaining the nickel aluminum hydrotalcite. According to the method for producing nickel aluminum hydrotalcite by utilizing nickel-containing wastewater intercalation, an effective path is developed, chromium in the wastewater is fully recycled, the wastes are changed into valuable materials, the disadvantages are turned into advantages, the heavy metal nickel is fully utilized, the wastewater is effectively treated, the nickel removal rate is 90 percent after the nickel-containing wastewater is replaced through hydrated chloride calcium aluminate intercalation, and the safety emission standard is achieved. Moreover, sludge is not generated in the treatment method, transfer of secondary pollution caused by a solid waste is avoided, the reclaimed water and filter cake are fully utilized, and the method is economic, environment-friendly and high in efficiency.
Description
Technical field
The present invention relates to a kind of method of utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs, belong to environment protection, middle water reuse, function nano technical field.
Background technology
The nearly family more than 10,000 of Electroplate Factory of China.The waste water of annual discharge approximately has 4O hundred million m
3.Nickel-containing waste water is one of main wastewater source of electroplating industry.Nickel has strong toxicity, is the carcinogens that international anticancer research center and U.S.'s toxicology tissue are announced.There is obvious carcinogenesis.Sexavalence nickel compound can not be decomposed by microorganism at nature.And infiltration migration is stronger.Human body is had to strong sensitization.Therefore, dealing carefully with Treating Electroplate Wastewater Containing Nickel.It is an environmental problem that must solve in electroplating industry.
At present, mainly adopt chemical reduction method, electrolytic process, absorption method, microbial method, extraction process etc. for the processing of Treating Electroplate Wastewater Containing Nickel.
The ultimate principle of chemical reduction method is with reductive agent, nickel to be reduced, then adds flocculation agent by nickel flocculation sediment, to realize solid-liquid separation.
Electrolytic process is to utilize nickel generation electrochemical reaction in electrode and waste water and the method for 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 biotechnology the reach of science, people, to the more and more darker people of the understanding of microorganism, utilize microbial method to process nickel-containing waste water and also cause gradually people's concern.
Extraction process is the unit operation that utilizes nickel to have different solubleness to be isolated in different solvents.
Hydrotalcite-based compound comprises hydrotalcite and houghite, and its main body is generally made up of the oxyhydroxide of two kinds of metals, is called again layered di-hydroxyl composite metal oxidate (Layered Double Hydroxide, LDH).
Up to the present, the preparation of hydrotalcite-based compound mainly contains following several method:
1. coprecipitation method
The most frequently used synthetic method of hydrotalcite is exactly coprecipitation method, prepares LDHs with mixing solutions and the alkaline solution mixing generation co-precipitation of the metal ion that forms hydrotalcite layer at a certain temperature.
2. ion exchange method
Unstable in alkaline medium when metal ion, when coprecipitation method cannot be carried out, can adopt ion exchange method.Ion exchange method is from given hydrotalcite, given hydrotalcite is immersed in the solution that contains the negatively charged ion in target hydrotalcite, by the exchange interaction of target negatively charged ion and the original interlayer anion of hydrotalcite, forms new post layer.
3. salt monoxide synthesis method
The method be 1977 by propositions such as boehn, its preparation method is, oxide compound suspension and excessive aqueous chloride solution, in room temperature reaction a couple of days, are obtained consisting of hydrotalcite product.Preparing LDHs by this method is a kind of simple solid-liquid reaction.
4. induction hydrolysis method
This method is that the suspension liquid of the oxyhydroxide of trivalent metal is added in the salts solution of divalent metal, drips (acid or alkali) solution to keep certain pH value under vigorous stirring.
5. roast reduction process
This method is to be based upon (memoryeffect) preparation method on characteristic basis of LDHs " memory effect ".Baked hydrotalcite is at a certain temperature joined containing the aqueous solution of target negatively charged ion or is placed in vapor atmosphere, the reconstruction of LDHs layer pole structure will occur, negatively charged ion and water molecules enter interlayer, form new LDHs.
6. sol-gel method
The employing sol-gel methods such as Prine have synthesized organic anion hydrotalcite.Its building-up reactions is the hydrolysis of metal alkoxide compound in the HCI aqueous solution.The standby product of product prepared by this method and other method legal system is in morphological specificity, and all different on thermal decomposition process, the specific surface area of roasting gained composite oxides is higher by 10% than coprecipitation method sintetics.But because this method is organic reaction, side reaction makes productive rate not high; Crystal morphology is imperfect; Agglomeration is serious; And organometallic compound, poisonous, expensive, be not suitable for large-scale commercial production; So method is also not suitable for the synthetic of all houghites.
7. hydrothermal synthesis method
Hydrothermal synthesis method, is similar to magnesium sulfate, Tai-Ace S 150 mixing solutions and alkaline solution is mixed rapidly and generate white slurries, slurries is poured in autoclave, then reactor is put into crystallization in the baking oven of differing temps and obtained a series of hydrotalcites.
8. microwave process for synthesizing
Similar with coprecipitation method, by alkaline solution and salts solution mix and blend prepared slarry.Then, slurries are inserted in microwave oven, high temperature crystallization tens minutes, washs, filters, dries and to obtain hydrotalcite.
Summary of the invention
The object of this invention is to provide a kind of nickel-containing waste water intercalation that utilizes and produce the method for NiAl-HTLcs, to solve in above-mentioned prior art a still unsolved difficult problem.
The technical solution used in the present invention is: a kind of method of utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs, its innovative point is: taking nickel in nickel-containing waste water as measurement standard, drop into hydrated calcium chloroaluminate according to mass ratio, reaction at normal temperatures, isolate throw out, throw out is dried, and obtains NiAl-HTLcs.
Further, the described method concrete steps of utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs are in nickel-containing waste water, slowly to add the hydrated calcium chloroaluminate of accurate-metering through grinding under stirring at normal temperature, lower stirring that the temperature remains within the normal range, it is 8~96 hours that the stirring reaction time is set, being stirred to the complete intercalation of nickel replaces in hydrated calcium chloroaluminate and generates after NiAl-HTLcs, descended post to realize solid-liquid separation throw out through normal temperature, after the residence time is 4~24 hours, drain direct discharge, throw out is dried, it is 80~500 DEG C that bake out temperature is set, finally grind to finished product.
Further, in described hydrated calcium chloroaluminate input amount and nickel-containing waste water, the mass ratio of nickel is 1:10~20.
Further, in described hydrated calcium chloroaluminate input amount and nickel-containing waste water, the mass ratio of nickel is 1:13~17.
Further, described nickel-containing waste water comprises organic nickel waste water, inorganic nickel waste water and organic-inorganic composite waste; Described organic nickel waste water is nickelous acetate waste water; Described inorganic nickel waste water is single nickel salt, nickelous chloride or nickel oxide waste water; Described organic-inorganic composite waste is organic nickel waste water and the mixing solutions of any ratio of inorganic nickel waste water.
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 normal temperature, the stirring reaction time is 12~48 hours.
Further, to descend the residence time of post be 8~12 hours to described normal temperature.
Further, described throw out bake out temperature is 120~270 DEG C.
Beneficial effect of the present invention is: this method of utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs of the present invention, develop a kind of effective way, the fully chromium in recycling waste water, turn waste into wealth, turn harm into good, when making full use of nickel heavy metal, effectively process waste water, nickel-containing waste water is after the displacement of hydrated calcium chloroaluminate intercalation, and nickel clearance reaches 90%, reaches the standard of safety dumping; Treatment process of the present invention can not produce mud, has avoided the secondary pollution causing with the form of solid waste to shift, and makes full use of middle water and filter cake, economic environmental protection, and efficiency is high.
Embodiment
Implementation column below can make those skilled in the art more fully understand the present invention, but does not therefore limit the present invention among described scope of embodiments.
embodiment 1
Be 128mg/l at nickel concentration, chemical oxygen demand (COD) is in 1 ton of waste water of 108mg/l, stir the lower hydrated calcium chloroaluminate 100Kg that slowly drops into, stirring at normal temperature is set 12 hours, is discharged to suction filtration bucket, descended post to realize solid-liquid separation throw out through normal temperature, after the residence time is 4~24 hours, drain direct discharge, throw out is dried, and finally grinds to finished product;
The wastewater mother liquor that wherein filters the nickeliferous 0.5mg/l obtaining, middle water reuse is to electroplating work procedure; Filter cake is calcium chromium class garnet, cures through 150 DEG C, grinds packaging selling by grade.
The nickel-containing waste water intercalation that utilizes in the present embodiment is produced the method for NiAl-HTLcs, and nickel concentration is reduced to 0.5mg/l by original 128mg/l, reaches the standard of safety dumping; The treatment process of the present embodiment can not produce mud, has avoided the secondary pollution causing with the form of solid waste to shift, and makes full use of middle water and filter cake, economic environmental protection, and efficiency is high.
embodiment 2
Be 100mg/l at nickel concentration, chemical oxygen demand (COD) is in 1 ton of waste water of 90mg/l, stir the lower hydrated calcium chloroaluminate 90Kg that slowly drops into, stirring at normal temperature is set 12 hours, is discharged to suction filtration bucket, descended post to realize solid-liquid separation throw out through normal temperature, after the residence time is 4~24 hours, drain direct discharge, throw out is dried, and finally grinds to finished product;
The wastewater mother liquor that wherein filters the nickeliferous 0.45mg/l obtaining, middle water reuse is to electroplating work procedure; Filter cake is calcium chromium class garnet, cures through 150 DEG C, grinds packaging selling by grade.
The nickel-containing waste water intercalation that utilizes in the present embodiment is produced the method for NiAl-HTLcs, and nickel concentration is reduced to 0.45mg/l by original 100mg/l, reaches the standard of safety dumping; The treatment process of the present embodiment can not produce mud, has avoided the secondary pollution causing with the form of solid waste to shift, and makes full use of middle water and filter cake, economic environmental protection, and efficiency is high.
Claims (10)
1. utilize nickel-containing waste water intercalation to produce a method for NiAl-HTLcs, it is characterized in that: taking nickel in nickel-containing waste water as measurement standard, drop into hydrated calcium chloroaluminate according to mass ratio, reaction at normal temperatures, isolate throw out, throw out is dried, and obtains NiAl-HTLcs.
2. the method for utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs according to claim 1, it is characterized in that: the described method concrete steps of utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs are in nickel-containing waste water, slowly to add the hydrated calcium chloroaluminate of accurate-metering through grinding under stirring at normal temperature, lower stirring that the temperature remains within the normal range, it is 8~96 hours that the stirring reaction time is set, being stirred to the complete intercalation of nickel replaces in hydrated calcium chloroaluminate and generates after NiAl-HTLcs, descended post to realize solid-liquid separation throw out through normal temperature, after the residence time is 4~24 hours, drain direct discharge, throw out is dried, it is 80~500 DEG C that bake out temperature is set, finally grind to finished product.
3. the method for utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs according to claim 1 and 2, is characterized in that: in described hydrated calcium chloroaluminate input amount and nickel-containing waste water, the mass ratio of nickel is 1:10~20.
4. the method for utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs according to claim 1 and 2, is characterized in that: in described hydrated calcium chloroaluminate input amount and nickel-containing waste water, the mass ratio of nickel is 1:13~17.
5. the method for utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs according to claim 1, is characterized in that: described nickel-containing waste water comprises organic nickel waste water, inorganic nickel waste water and organic-inorganic composite waste; Described organic nickel waste water is nickelous acetate waste water; Described inorganic nickel waste water is single nickel salt, nickelous chloride or nickel oxide waste water; Described organic-inorganic composite waste is organic nickel waste water and the mixing solutions of any ratio of inorganic nickel waste water.
6. the method for utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs according to claim 1, is characterized in that: the calcium aluminum ratio of described hydrated calcium chloroaluminate is 1.5~6:1.
7. the method for utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs according to claim 1, is characterized in that: the calcium aluminum ratio of described hydrated calcium chloroaluminate is 2~4:1.
8. the method for utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs according to claim 1, is characterized in that: under described normal temperature, the stirring reaction time is 12~48 hours.
9. the method for utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs according to claim 1, is characterized in that: it is 8~12 hours that described normal temperature descended the residence time of post.
10. the method for utilizing nickel-containing waste water intercalation to produce NiAl-HTLcs according to claim 1, is characterized in that: described throw out bake out temperature is 120~270 DEG C.
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Cited By (2)
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CN105129952A (en) * | 2015-09-14 | 2015-12-09 | 江苏隆昌化工有限公司 | Method for removing cyanide in wastewater |
CN112707448A (en) * | 2020-12-07 | 2021-04-27 | 中南大学 | Hydrotalcite-like compound, preparation method thereof and application thereof in arsenic removal |
Citations (1)
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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 |
Non-Patent Citations (1)
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张娟娟 等: "Friedel 盐对废水中低浓度Cd2+的吸附动力学", 《过程工程学报》, vol. 12, no. 4, 31 August 2012 (2012-08-31), pages 590 - 595 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105129952A (en) * | 2015-09-14 | 2015-12-09 | 江苏隆昌化工有限公司 | Method for removing cyanide in wastewater |
CN112707448A (en) * | 2020-12-07 | 2021-04-27 | 中南大学 | Hydrotalcite-like compound, preparation method thereof and application thereof in arsenic removal |
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