CN102974312A - Method for synthesizing organic hydrotalcite by using electroplating wastewater and washing wastewater - Google Patents
Method for synthesizing organic hydrotalcite by using electroplating wastewater and washing wastewater Download PDFInfo
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- CN102974312A CN102974312A CN2012104943049A CN201210494304A CN102974312A CN 102974312 A CN102974312 A CN 102974312A CN 2012104943049 A CN2012104943049 A CN 2012104943049A CN 201210494304 A CN201210494304 A CN 201210494304A CN 102974312 A CN102974312 A CN 102974312A
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- wastewater
- hydrotalcite
- electroplating wastewater
- washes
- sediment
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Abstract
The invention discloses a method for synthesizing organic hydrotalcite by using electroplating wastewater and washing wastewater. The method comprises the following steps of: respectively filtering the electroplating wastewater and the washing wastewater to remove solid particles, and analyzing ions in the electroplating wastewater and the washing wastewater by an electroplating production process, wherein the divalent ion molar concentration is 2-4 times of that trivalent ion molar concentration; dripping a KOH solution with the concentration of 50-70% in the electroplating wastewater, so as to separate sediments; preparing turbid liquid by using the separated sediments, wherein a solid-liquid ratio is in a range from 1: 4 to 1: 8; continuously dripping the KOH solution with the concentration of 50-70% until the pH value reaches to 10-13; aging for 24-48 hours at the room temperature and separating the sediments; adding the sediments into the washing wastewater, and stirring the mixture at the rotation speed of 300-400rpm for 3-4 hours, so as to separate the sediments; and drying the mixture at the temperature of 70-90 DEG C, so that an anionic surfactant in the washing wastewater enters a hydrotalcite interlayer so as to finally obtain the organic hydrotalcite, so that the waste recovery can be realized.
Description
Technical field
The present invention relates to the exploitation of environmental pollution control new material, relate in particular to a kind of method of utilizing electroplating wastewater and the synthetic organic hydrotalcite of washes.
Background technology
Electroplate waste water and waste liquid that factory (or workshop) discharges, such as plating piece washings, useless tank liquor, component cooling water and the flushing surface water etc., its water quality is different because of production technology, and often in general the oil-containing many kinds of metal ions, often contains Cr
6+, Cd
2+, Ni
2+, Cu
2+, Zn
2+, Fe
2+In heavy metal; How poisonous electroplating wastewater is, endangers larger.Can cause people and animals' acute poisoning such as cyanogen, cause death that the low concentration long term also can cause slow poisoning.Cadmium can make kidney generation pathology, and can cause itai-itai.Cr VI can cause lung cancer, intestines and stomach disease and anaemia, and can accumulate in bone, spleen and liver.Therefore, electroplating wastewater must strictly be controlled, and deals carefully with.
Surfactant used in the articles for washing is take anionic as most important.Wherein the linear alkylbenzene sulfonate (LAS) consumption is maximum, is aliphatic alcohol sulfate, fatty alcohol polyoxyethylene ether sulfate, alkylsulfonate etc. secondly.Anion surfactant take neopelex as representative, responsive to the water hardness, be difficult for oxidation, foaming power is strong, cost is lower, synthesis technique is ripe, to particulate fouling, albumen dirt and oily dirt have significant clean effect, and be especially good to the cleaning function of particulate fouling on the natural fiber, detergency strengthens with the rising of wash temperature, effect to the albumen dirt is higher than non-ionic surface active agent, and foam is abundant, is very effective washing agent, be usually used in washing powder, liquid detergent and hand cleanser, consumption is very large.Neopelex also is widely used in washing and the degreasing of the industry such as process hides, weaving except being used for articles for washing.Exhibiting high surface activating agent waste water has been discharged in the production of neopelex, because neopelex content is high in the waste water, if directly enter environment, not only affect aquatile existence, the self-purification of water is obstructed, environment is caused severe contamination, and activity and the propagation of microbial cell there is certain inhibition, animals and plants and human body there is chronic toxic action, can upset internal system, cause the anomalies such as male and female one, animal immune parasthenia, development of fetus deformity, children mental retardation.
Neopelex waste water treatment process such as coagulating sedimentation, catalytic oxidation, foam separation, charcoal absorption, biodegradation and their group technology commonly used are realized its purified treatment.Wherein absorption method is efficient, simple, but acticarbon is expensive.
Layered di-hydroxyl composite metal oxidate (Layered Double Hydroxides is called for short LDH) claims again hydrotalcite, is the important inorganic functional material of a class.The adjustable sex change of the layer structure that it is unique and laminate element and interlayer anion gets more and more people's extensive concerning, introduce new object anion through ion-exchange to interlayer and can make layer structure and composition produce corresponding the variation, thereby can prepare the functional material that a large class has special nature.Hydrotalcite material belongs to anion type laminated compound.The compounds that lamellar compound refers to have layer structure, interlayer ion has interchangeability, utilize intercalation that the lamellar compound main body has and the interchangeability of interlayer ion under strong polar molecule effect, form layer-pillared compound thereby some functional guest species are introduced bedding voids and the laminate distance strutted.
The hydrotalcite chemical structure of general formula is: [M
2+ 1-xM
3+X (OH)
2]
X+[(A
N-)
X/nMH
2O], M wherein
2+Be Mg
2+, Ni
2+, Mn
2+, Zn
2+, Ca
2+, Fe
2+, Cu
2+Deng the divalent metal anion; M
3+Be Al
3+, Cr
3+, Fe
3+, Co
3+Deng the trivalent metal anion; A
N-Be anion, such as CO
3 2-, NO
3 -, Cl
-, OH
-, SO
4 2-, PO
4 3-, C
6H
4(COO)
2 2-Etc. inorganic and organic ion and complex ion, different when the interlayer inorganic anion, the interlamellar spacing of hydrotalcite is different, and after hydrotalcite adsorption fouling thing, interlamellar spacing also can increase, to hold more pollutant simultaneously.
At present, the synthetic method of hydrotalcite-like material mainly contains salt-alkaline process, salt-conventional ceramic technique and ion-exchange, also derives Hydrolyze method, hydro-thermal method, the again hydration method of heat treatment etc. of inducing.Wherein the most frequently used method is coprecipitation, namely with the metallic ion mixed liquor that consists of the hydrotalcite layer co-precipitation occurs under the effect of alkali at a certain temperature and prepares.The method is simple to operation, is the preparation method who commonly uses, and needs to utilize a certain amount of bivalent metal ion and trivalent metal ion in the method, has increased input from the angle of economy; From the synthetic process of the angle of administering environment, increased the generation of waste water, environmental improvement has been proposed new problem.
Summary of the invention
The objective of the invention is to prepare the deficiency that organic hydrotalcite also is used for treatment of Organic Wastewater in the prior art for overcoming, a kind of method of utilizing electroplating wastewater and the synthetic organic hydrotalcite of washes is provided.
The technical solution used in the present invention is in turn include the following steps:
1) electroplating wastewater and washes are filtered respectively the removal solid particle, the ion that analysis wherein exists according to electroplate technology, add suitable metal cation, or multiple electroplating wastewater is mixed, guarantee that the divalent ion molar concentration is 2 ~ 4 times of trivalent ion molar concentration;
2) in electroplating wastewater, drip 50% ~ 70% KOH solution, continue 200 ~ 300 rpm and stir, when without the precipitation regeneration, stop to drip KOH solution, sediment separate out;
3) sediment after will separating is made suspension, solid-to-liquid ratio is 1:4 ~ 1:8, in this suspension, continue to drip 50% ~ 70% KOH solution, until till pH value to 10 ~ 13, under 300 ~ 400 rpm, stir during dropping, be added dropwise to complete at room temperature aging 24 ~ 48 h of rear suspension, sediment separate out;
4) this sediment is joined in the washes, solid-to-liquid ratio is 1:1000 ~ 1:5000, stirs 3 ~ 4 h under 300 ~ 400 rpm rotating speeds, sediment separate out, 70 ~ 90 ℃ of lower oven dry, the anion surfactant in the washes then enters hydrotalcite layers, is prepared into organic hydrotalcite.
Advantage of the present invention is to utilize metal ion in the electroplating wastewater and the anion in the washes, the organic hydrotalcite that simultaneously preparation has broad field of application, realize twice laid, and can remove heavy metal in the electroplating wastewater, with the anionic dye in the washes, although the synthetic organic hydrotalcite that obtains contains various metals, can not satisfy the needs of high-level (such as the medication chemistry aspect), but can be used as sorbing material as the material that hydrotalcite structure is arranged, continue on for environmental improvement.
The specific embodiment
Electroplating wastewater and washes are filtered respectively the removal solid particle, the ion that wherein may exist according to the electroplate technology analysis, add suitable metal cation, or with multiple electroplating wastewater mixing, guarantee that divalent ion concentration is 2 ~ 4 times (molar concentrations) of trivalent ion concentration, if only have divalent metal, then add a small amount of trivalent metal cation (such as comparatively cheap Al
3+, Fe
3+), if only have trivalent metal cation, then add a small amount of divalent metal (such as comparatively cheap Mg
2+, Fe
2+), if divalent metal and trivalent metal cation have been arranged, then investigate concentration, the ratio that the concentration ratio of guaranteeing the two meets above-mentioned molar concentration is 2 ~ 4 times scope.
Drip fast 50% ~ 70% KOH solution in the electroplating wastewater, continue 200 ~ 300 rpm and stir, metal ion precipitates under the alkali effect, when alkali lye without precipitating regeneration, stop to drip KOH solution, sediment separate out; Sediment after separating be need not oven dry, make suspension, solid-to-liquid ratio is 1:4 ~ 1:8(mass ratio), continue in this suspension to drip 50% ~ 70% KOH solution, until till pH value to 10 ~ 13, during dropping under 300 ~ 400 rpm rapid stirring, be added dropwise to complete at room temperature aging 24 ~ 48 h of rear suspension, sediment separate out, in this process, metal ion generates hydrotalcite under alkali condition; This sediment is joined in the washes, and solid-to-liquid ratio is 1:1000 ~ 1:5000, stirs 3 ~ 4 h under 300 ~ 400 rpm rotating speeds, sediment separate out, 70 ~ 90 ℃ of lower oven dry, the anion surfactant in the washes then enters hydrotalcite layers, namely is prepared into organic hydrotalcite.
3 embodiment of the present invention below further are provided:
Embodiment 1
Electroplating wastewater and washes are filtered respectively the removal solid particle, according to analysis of Production Technology, contain Ni in the electroplating wastewater
2+And Fe
2+, add a small amount of Al
3+, making divalent ion concentration is 2 times of trivalent ion concentration; Drip fast 50% KOH solution in the electroplating wastewater, continue 200 rpm and stir, metal ion precipitates under the alkali effect, when alkali lye without precipitating regeneration, stop to drip KOH solution, sediment separate out; Sediment after the separation need not oven dry, make suspension, solid-to-liquid ratio is the 1:4(mass ratio), continue in this suspension to drip 50% KOH solution, until till the pH value to 10, during dropping under 300 rpm rapid stirring, be added dropwise to complete at room temperature aging 24h of rear suspension, sediment separate out, in this process, metal ion generates hydrotalcite under alkali condition; This sediment is joined in the washes, and solid-to-liquid ratio is 1:1000, stirs 3 h under the 300rpm rotating speed, sediment separate out, and 70 ℃ of lower oven dry, the anion surfactant in the washes then enters hydrotalcite layers, namely is prepared into organic hydrotalcite.
With the organic wastewater of this organic hydrotalcite powder for the treatment of the p-nitrophenyl that contains 15mg/L, the handled wastewater volume that every gram organic hydrotalcite is corresponding is about 1 L, rapid stirring 60 minutes; Product stopped 30 minutes at sedimentation basin, Separation of Solid and Liquid, and ultraviolet-uisible spectrophotometer is measured supernatant concentration, and pollutants removal rate is 96.7%.
Embodiment 2
Electroplating wastewater and washes are filtered respectively the removal solid particle, according to analysis of Production Technology, contain Al in the electroplating wastewater
3+, add a small amount of Mg
2+, making divalent ion concentration is 4 times of trivalent ion concentration; Drip fast 70% KOH solution in the electroplating wastewater, continue 300 rpm and stir, metal ion precipitates under the alkali effect, when alkali lye without precipitating regeneration, stop to drip KOH solution, sediment separate out; Sediment after the separation need not oven dry, make suspension, solid-to-liquid ratio is the 1:8(mass ratio), continue in this suspension to drip 70% KOH solution, until till the pH value to 13, during dropping under 400 rpm rapid stirring, be added dropwise to complete at room temperature aging 48 h of rear suspension, sediment separate out, in this process, metal ion generates hydrotalcite under alkali condition; This sediment is joined in the washes, and solid-to-liquid ratio is 1:5000, stirs 4 h under the 400 rpm rotating speeds, sediment separate out, and 90 ℃ of lower oven dry, the anion surfactant in the washes then enters hydrotalcite layers, namely is prepared into organic hydrotalcite.
For the treatment of the organic wastewater to toluene that contains 10 mg/L, the handled wastewater volume that every gram organic hydrotalcite is corresponding is about 1 L with this organic hydrotalcite powder, rapid stirring 60 minutes; Product stopped 30 minutes at sedimentation basin, Separation of Solid and Liquid, and ultraviolet-uisible spectrophotometer is measured supernatant concentration, and pollutants removal rate is 97.5%.
Embodiment 3
Multiple electroplating wastewater and washes are mixed respectively, remove solid particle, according to having Ni in the analysis of Production Technology electroplating wastewater
2+, Cu
2+, Fe
3+And Al
3+, and divalent ion concentration is 3 times of trivalent ion concentration, drips fast 60% KOH solution in electroplating wastewater, continue 250 rpm and stir, metal ion precipitates under the alkali effect, when alkali lye without precipitating regeneration, stop to drip KOH solution, sediment separate out; Sediment after the separation need not oven dry, make suspension, solid-to-liquid ratio is the 1:6(mass ratio), continue in this suspension to drip 60% KOH solution, until till the pH value to 12, during dropping under 350 rpm rapid stirring, be added dropwise to complete at room temperature aging 35 h of rear suspension, sediment separate out, in this process, metal ion generates hydrotalcite under alkali condition; This sediment is joined in the washes, and solid-to-liquid ratio is 1:3000, stirs 4 h under the 350 rpm rotating speeds, sediment separate out, and 80 ℃ of lower oven dry, the anion surfactant in the washes then enters hydrotalcite layers, namely is prepared into organic hydrotalcite.
With the organic wastewater of this organic hydrotalcite powder for the treatment of the p-nitrophenol that contains 10 mg/L, the handled wastewater volume that every gram organic hydrotalcite is corresponding is about 1 L, rapid stirring 60 minutes; Product stopped 30 minutes at sedimentation basin, Separation of Solid and Liquid, and ultraviolet-uisible spectrophotometer is measured supernatant concentration, and pollutants removal rate is 93.1%.
Claims (1)
1. method of utilizing the synthetic organic hydrotalcite of electroplating wastewater and washes is characterized in that in turn including the following steps:
1) electroplating wastewater and washes are filtered respectively the removal solid particle, the ion that analysis wherein exists according to electroplate technology, add suitable metal cation, or multiple electroplating wastewater is mixed, guarantee that the divalent ion molar concentration is 2 ~ 4 times of trivalent ion molar concentration;
2) in electroplating wastewater, drip 50% ~ 70% KOH solution, continue 200 ~ 300 rpm and stir, when without the precipitation regeneration, stop to drip KOH solution, sediment separate out;
3) sediment after will separating is made suspension, solid-to-liquid ratio is 1:4 ~ 1:8, in this suspension, continue to drip 50% ~ 70% KOH solution, until till pH value to 10 ~ 13, under 300 ~ 400 rpm, stir during dropping, be added dropwise to complete at room temperature aging 24 ~ 48 h of rear suspension, sediment separate out;
4) this sediment is joined in the washes, solid-to-liquid ratio is 1:1000 ~ 1:5000, stirs 3 ~ 4 h under 300 ~ 400 rpm rotating speeds, sediment separate out, 70 ~ 90 ℃ of lower oven dry, the anion surfactant in the washes then enters hydrotalcite layers, is prepared into organic hydrotalcite.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104003456A (en) * | 2014-05-30 | 2014-08-27 | 江苏隆昌化工有限公司 | Method for preparing nickel-aluminum hydrotalcite by using nickel-containing wastewater |
| CN104549130A (en) * | 2014-12-04 | 2015-04-29 | 常州大学 | Preparation method of nickel-aluminum hydrotalcite doped with surfactant |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1569671A (en) * | 2003-07-24 | 2005-01-26 | 合肥工业大学 | Water treatment method for instant synthesis of laminated bis-hydroxide |
| CN101376537A (en) * | 2008-09-24 | 2009-03-04 | 上海大学 | Method for processing electroplating waste containing Ni2+, Zn2+ and Cr3+ |
-
2012
- 2012-11-28 CN CN2012104943049A patent/CN102974312A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1569671A (en) * | 2003-07-24 | 2005-01-26 | 合肥工业大学 | Water treatment method for instant synthesis of laminated bis-hydroxide |
| CN101376537A (en) * | 2008-09-24 | 2009-03-04 | 上海大学 | Method for processing electroplating waste containing Ni2+, Zn2+ and Cr3+ |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104003456A (en) * | 2014-05-30 | 2014-08-27 | 江苏隆昌化工有限公司 | Method for preparing nickel-aluminum hydrotalcite by using nickel-containing wastewater |
| CN104003456B (en) * | 2014-05-30 | 2016-01-20 | 江苏隆昌化工有限公司 | A kind of nickel-containing waste water prepares the method for nickel aluminum hydrotalcite |
| CN104549130A (en) * | 2014-12-04 | 2015-04-29 | 常州大学 | Preparation method of nickel-aluminum hydrotalcite doped with surfactant |
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Application publication date: 20130320 |