CN103011327A - Method for removing chromium in tanning waste water by using aluminum zirconium tanning wastes to load montmorillonite - Google Patents
Method for removing chromium in tanning waste water by using aluminum zirconium tanning wastes to load montmorillonite Download PDFInfo
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- CN103011327A CN103011327A CN2012105563329A CN201210556332A CN103011327A CN 103011327 A CN103011327 A CN 103011327A CN 2012105563329 A CN2012105563329 A CN 2012105563329A CN 201210556332 A CN201210556332 A CN 201210556332A CN 103011327 A CN103011327 A CN 103011327A
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Abstract
The invention relates to a method for removing chromium in tanning waste water by using aluminum zirconium tanning wastes to load montmorillonite. Methods for treating low-concentration chromium-containing waste water all have problems of high investment, high operating cost, complex operation management and the like. The method comprises the following steps: taking aluminum zirconium compound tanning waste water for mixing, adding alkali in the waste water for adjusting the pH value, stewing, ageing, washing, precipitating, and obtaining (Al2O3-ZrO2) composite oxide after drying; preparing the montmorillonite to a solution, adding the (Al2O3-ZrO2) composite oxide having the same mass with the montmorillonite in the solution, and obtaining Al2O3-ZrO2/montmorillonite through drying; and adding the Al2O3-ZrO2/montmorillonite in low-concentration tanning waste water to absorb and remove Cr3+ in the waste water. The method adopts sintered aluminum zirconium tanning waste water precipitates to load MMT (Methylcyclopentadienyl Manganese Tricarbonyl) as absorbent, so that the absorption speed is fast, and the absorption equilibrium can be achieved by one hour; and after the precipitates are collected, dilute sulfuric acid is used for desorbing, so that the precipitates can be recycled.
Description
Technical field
The invention belongs to Chrome Tanning Wastewater deep purifying processing technology field, be specifically related to a kind of method of utilizing aluminium zirconium tanning waste load polynite to remove chromium in the tanning waste water.
Background technology
China is one of manufacturing center of World Leather Industry, yet curriery has also been brought serious environmental problem in accelerated development.According to statistics, produce 1 ton of leather and will produce 50 tons of waste water, chemical oxygen demand (COD) 250kg, biochemical oxygen demand 100kg, suspended substance 150kg, sulfide 10kg, chromium 5 ~ 6kg.Because the premium properties of chrome tanning agent, most finished leathers are produced by chromic tanning, but the specific absorption of chrome tanning agent is not high in the chromic tanning, Cr in the chrome tanning process institute waste discharge
2O
3Content is generally at 1500 ~ 2000mg/L, and containing behind the waste liquid alkaline chemical precipitation of plurality of heavy metal chromium directly, discharging has caused serious pollution to soil, water; Cr
3+Easily be oxidized to Cr
6+Can directly cause damage to human body skin, bring out various diseases and cancer.
In the Chrome Tanning Wastewater treating processes, the alkaline chemical precipitation method is present domestic the most frequently used ripe treatment process, high-concentration chromium-containing wastewater had preferably effect, the clearance of total chromium can reach more than 98%, but because the industry characteristic of tanning industry self, the chemical reagent that adds in the tannery, the pH value changes, the generation of water-disintegrable Collagen material in metal ion and the process hides process, can make chromium and these materials produce mating reaction, electrostatic adsorption, be oxidized to chromic salt etc., cause precipitating the total chromium concn of rear water outlet usually between 2mg/L ~ 40mg/L, can't reach the discharging standards of 1.5 mg/L.For low-concentration chromate waste water, method commonly used has absorption method, evaporation concentration method, ion-exchange-resin process etc., and investment is large, the problems such as running cost is high, operational administrative trouble but above these methods exist basically.
Summary of the invention
The purpose of this invention is to provide a kind of can effectively remove low concentrations of chromium ion in the Chrome Tanning Wastewater and can wash-out after the aluminium zirconium tanning waste load polynite (MMT) that utilizes of Reusability remove the method for chromium in the tanning waste water.
The technology used in the present invention means are:
Utilize aluminium zirconium tanning waste load polynite to remove the method for chromium in the tanning waste water, it is characterized in that:
Realized by following steps:
Step 1: preparation aluminium zirconium composite tanning technology throw out:
At ambient temperature, get aluminium zirconium composite tanning technology waste water, stir and add alkali and regulate the pH value, still aging 24h at room temperature after stirring; Vacuum filters, and with the distilled water wash precipitation, grinds after 40 ℃ of oven dry, 600 ℃ of calcining 3h, and the gained throw out is (Al
2O
3-ZrO
2) composite oxides;
Step 2: preparation Al
2O
3-ZrO
2/ montmorillonite Composite sorbent material:
Polynite is scattered in to make massfraction in the deionized water be 10% solution, 30 ℃ of lower 60min that stir of constant temperature leave standstill 24h; Ultrasonication, (the Al of the quality such as adding and polynite
2O
3-ZrO
2) composite oxides, 50 ℃ of lower 60min that stir of constant temperature leave standstill 120min, the dry Al that gets
2O
3-ZrO
2/ polynite;
Step 3: utilize Al
2O
3-ZrO
2Cr in the/polynite adsorption of Low Concentration leather-making waste water
3+:
In every liter of lower concentration leather-making waste water, add Al
2O
3-ZrO
2/ polynite quality 0.1～30g is that 10～30 ℃, pH value are the Cr in the planar water under 2.0～13.0 the condition in temperature
3+, adsorption time is 1min ~ 6h, removes the Cr in the waste water
3+, collecting precipitation thing then;
Step 4: the regeneration of collecting precipitation thing:
After the throw out of collecting put container, place 25 ℃ of waters bath with thermostatic control, add washed with de-ionized water, then add the dilute sulphuric acid that volumetric molar concentration is 0.1mol/ L, the mass ratio of throw out and dilute sulphuric acid is 1:4; Wave 3min every 0.5h, desorb 3 hours is poured out supernatant liquor after centrifugal, add deionized water again clean to pH for neutral.
In the step 1, the conditioning agent of pH value is NaOH solution, and its volumetric molar concentration is 2.0 mol/L, rate of addition 5.0mL/min, and the pH value is adjusted to 7.
In the step 3, Cr in the lower concentration leather-making waste water
3+Starting point concentration be 5mg/L～40mg/L.
The present invention has the following advantages:
The present invention adopts the alkaline chemical precipitation thing that produces in the aluminium zirconium tanning waste water processed, and the oxide carried MMT of aluminium zirconium double metal by behind the sintering is made into a kind of sorbent material, with the Cr in its processing lower concentration leather-making waste water
3+, working method is simple, the treatment of wastes with processes of wastes against one another, obvious processing effect and with low cost.
As sorbent material, adsorption rate is fast with the aluminium zirconium tanning wastewater sedimentation thing processed load MMT behind the sintering, and 1h just can reach adsorption equilibrium, and alkalescence and high ion concentration be of value to Cr in the water
3+Absorption.And behind the collecting precipitation thing, utilize the 0.1mol/l dilution heat of sulfuric acid to carry out sedimentary desorption, after desorption was finished, throw out can recycle; And for the first time the desorption and regeneration rate is 94.88%, loops the adsorption and desorption regeneration tests, regenerate after three times, the desorption and regeneration rate be 89.73% (the desorption and regeneration rate be sorbent material this adsorb Cr
3+Quality and the first Cr that adsorbs
3+Mass ratio).
(chromium concn is the Cr of 5mg/L～40mg/L) among the present invention the aluminium zirconium tanning wastewater sedimentation thing processed load MMT behind the sintering to be used for the lower concentration leather-making waste water
3+Removal, have good economic benefit and environmental benefit.Cr
3+Starting point concentration is in the water of 10 mg/L, Cr after the absorption
3+Concentration is 0.252mg/L, and clearance reaches 97.47%; Cr
3+Starting point concentration is in the water of 20 mg/L, Cr after the absorption
3+Concentration is 0.42 mg/L, and clearance reaches 97.87%; Cr
3+Starting point concentration is in the water of 40 mg/L, Cr after the absorption
3+Concentration is 1.02mg/L, and clearance can reach 97.43%.
Embodiment
The present invention will be described in detail below in conjunction with embodiment.
The extensive concern that Heavymetal Wastewater Treatment by Adsorption has efficiently, economic, easy, good selective has caused environmental protection circle.Absorption method is to utilize a kind of effective ways of the unique texture heavy-metal ion removal of sorbent material.The sorbent material that utilizes absorption method to process Cr waste water has gac, humic acids, sepiolite, polysaccharide resins, flyash, slag, wood chip and Pericarppium arachidis hypogaeae etc., and these materials are to the Cr in the water
3+And Cr
6+Certain removal effect is arranged.
The aluminium zirconium partly substituted in the last few years chrome tanning in conjunction with tan (mass ratio of aluminium zirconium is 10:1) and was applied in enterprise gradually, caused producing the aluminium zirconium in conjunction with tanning waste water, and this part waste water and comprehensive wastewater are together processed rear discharging in the actual production.If behind independent tanning effluent segregation, alkaline chemical precipitation is processed, and the throw out main component that can form is aluminium hydroxide and zirconium hydroxide.Can aluminium zirconium tanning wastewater sedimentation thing processed directly or by being used for removing the chromate waste water of lower concentration after the modification as sorbent material, there is not yet both at home and abroad at present studying be reported.
The method of chromium in the tanning waste water is removed in the aluminium zirconium tanning waste load polynite (MMT) that utilizes involved in the present invention, is realized by following steps:
Step 1: preparation aluminium zirconium composite tanning technology throw out:
At ambient temperature, get aluminium zirconium composite tanning technology waste water, stir and add alkali and regulate the pH value, still aging 24h at room temperature after stirring; Vacuum filters, and with the distilled water wash precipitation, grinds after 40 ℃ of oven dry, 600 ℃ of calcining 3h, and the gained throw out is (Al
2O
3-ZrO
2) composite oxides;
Wherein, the conditioning agent of pH value is NaOH solution, and its volumetric molar concentration is 2.0 mol/L, rate of addition 5.0mL/min, and the pH value is adjusted to 7.
Step 2: preparation Al
2O
3-ZrO
2/ montmorillonite Composite sorbent material:
Polynite is scattered in to make massfraction in the deionized water be 10% solution, 30 ℃ of lower 60min that stir of constant temperature leave standstill 24h; Ultrasonication, (the Al of the quality such as adding and polynite
2O
3-ZrO
2) composite oxides, 50 ℃ of lower 60min that stir of constant temperature leave standstill 120min, the dry Al that gets
2O
3-ZrO
2/ polynite;
Step 3: utilize Al
2O
3-ZrO
2Cr in the/polynite adsorption of Low Concentration leather-making waste water
3+:
In every liter of lower concentration leather-making waste water, add Al
2O
3-ZrO
2/ polynite quality 0.1～30g is that 10～30 ℃, pH value are the Cr in the planar water under 2.0～13.0 the condition in temperature
3+, adsorption time is 1min ~ 6h, removes the Cr in the waste water
3+, collecting precipitation thing then;
Cr in the described lower concentration leather-making waste water
3+Starting point concentration be 5mg/L～40mg/L.
Step 4: the regeneration of collecting precipitation thing:
After the throw out of collecting put container, place 25 ℃ of waters bath with thermostatic control, add washed with de-ionized water, then add the dilute sulphuric acid that volumetric molar concentration is 0.1mol/ L, the mass ratio of throw out and dilute sulphuric acid is 1:4; Wave 3min every 0.5h, desorb 3 hours is poured out supernatant liquor after centrifugal, add deionized water again clean to pH for neutral.
Embodiment 1:
Step 1: preparation aluminium zirconium composite tanning technology throw out:
At ambient temperature, get aluminium zirconium composite tanning technology waste water, stir and add alkali and regulate the pH value, still aging 24h at room temperature after stirring; Vacuum filters, and with the distilled water wash precipitation, grinds after 40 ℃ of oven dry, then grinds 40 mesh sieves, 600 ℃ of calcining 3h, and the gained throw out is (Al
2O
3-ZrO
2) composite oxides;
Wherein, the conditioning agent of pH value is NaOH solution, and its volumetric molar concentration is 2.0 mol/L, rate of addition 5.0mL/min, and the pH value is adjusted to 7.
Step 2: preparation Al
2O
3-ZrO
2/ montmorillonite Composite sorbent material:
Polynite is scattered in to make massfraction in the deionized water be 10% solution, 30 ℃ of lower 60min that stir of constant temperature leave standstill 24h; Ultrasonication, (the Al of the quality such as adding and polynite
2O
3-ZrO
2) composite oxides, 50 ℃ of lower 60min that stir of constant temperature leave standstill 120min, the dry Al that gets
2O
3-ZrO
2/ polynite;
Step 3: utilize Al
2O
3-ZrO
2Cr in the/polynite adsorption of Low Concentration leather-making waste water
3+:
In every liter of lower concentration leather-making waste water, add Al
2O
3-ZrO
2/ polynite quality 15g is that 25 ℃, pH value are the Cr in the planar water under 3.76 the condition in temperature
3+, adsorption time is 6h, removes the Cr in the waste water
3+, collecting precipitation thing then;
Cr in the described lower concentration leather-making waste water
3+Starting point concentration be 10mg/L.
Step 4: the regeneration of collecting precipitation thing:
After the throw out of collecting put container, place 25 ℃ of waters bath with thermostatic control, add washed with de-ionized water, then add the dilute sulphuric acid that volumetric molar concentration is 0.1mol/ L, the mass ratio of throw out and dilute sulphuric acid is 1:4; Wave 3min every 0.5h, desorb 3 hours is poured out supernatant liquor after centrifugal, add deionized water again clean to pH for neutral.
In the present embodiment, collect sorbent material after adsorbing 6 h, record Cr
3+Adsorptive capacity be 0.66mg/g, clearance is 99.17%.Cr
3+Adsorptive capacity refer to every gram sorbent material absorption Cr
3+Amount, Cr
3+Clearance refer to the Cr that is adsorbed
3+The ratio of concentration and starting point concentration.
Embodiment 2:
With embodiment 1, but change adsorption conditions into 10 ℃ of water bath with thermostatic control vibrations, Cr in the lower concentration leather-making waste water
3+Starting point concentration be 5mg/L, in every liter of lower concentration leather-making waste water, add Al
2O
3-ZrO
2/ polynite quality 30g, other condition is constant, records Cr
3+Adsorptive capacity be 0.64mg/g, clearance is 96.27%.
Embodiment 3:
With embodiment 1, but change adsorption conditions into 30 ℃ of water bath with thermostatic control vibrations, Cr in the lower concentration leather-making waste water
3+Starting point concentration be 40mg/L, in every liter of lower concentration leather-making waste water, add Al
2O
3-ZrO
2/ polynite quality 0.1g, other condition is constant, records Cr
3+Adsorptive capacity be 0.62mg/g, clearance is 93.21%.
Embodiment 4:
With embodiment 1, but change adsorption time in the adsorption conditions into 1min, other condition is constant, records Cr
3+Adsorptive capacity be 0.60mg/g, clearance is 90.58%.
Embodiment 5:
With embodiment 1, but be 2h with adsorption time in the adsorption conditions, other condition is constant, measures Cr
3+Adsorptive capacity be 0.66mg/g, clearance is 98.74%.
Embodiment 6:
With embodiment 1, the pH value in the adsorption conditions is adjusted to pH=6.00, other conditions are constant, record Cr
3+Adsorptive capacity be 0.64mg/g, clearance is 96.62%;
With embodiment 1, the pH value in the adsorption conditions is adjusted to pH=11.00, other condition is constant, records Cr
3+Adsorptive capacity be 0.64mg/g, clearance is 96.62%;
With embodiment 1, the pH value in the adsorption conditions is adjusted to pH=13.00, other condition is constant, records Cr
3+Adsorptive capacity be 0.63mg/g, clearance is 94.90%
Embodiment 7:
With embodiment 1, after adsorption equilibrium, saturated sorbent material is put into the 100ml beaker, place 25 ℃ of waters bath with thermostatic control, add ionized water and clean 3 times, then add the sorbent material 0.1mol/l dilute sulphuric acid of 50ml, every 0.5h, wave 3min, desorb 3 hours, static 1h pours out supernatant liquor, add deionized water, cleaning for several times, is neutral to pH, again carries out regeneration tests, clearance is 94.87% for the first time, clearance is 94.56% for the second time, and clearance is that 94.01%, the four clearance is 89.92% for the third time, the 5th clearance is that 74.71%, the six clearance is 63.55%.
It is cited that content of the present invention is not limited to embodiment, and the conversion of any equivalence that those of ordinary skills take technical solution of the present invention by reading specification sheets of the present invention is claim of the present invention and contains.
Claims (3)
1. utilize aluminium zirconium tanning waste load polynite to remove the method for chromium in the tanning waste water, it is characterized in that:
Realized by following steps:
Step 1: preparation aluminium zirconium composite tanning technology throw out:
At ambient temperature, get aluminium zirconium composite tanning technology waste water, stir and add alkali and regulate the pH value, still aging 24h at room temperature after stirring; Vacuum filters, and with the distilled water wash precipitation, grinds after 40 ℃ of oven dry, 600 ℃ of calcining 3h, and the gained throw out is (Al
2O
3-ZrO
2) composite oxides;
Step 2: preparation Al
2O
3-ZrO
2/ montmorillonite Composite sorbent material:
Polynite is scattered in to make massfraction in the deionized water be 10% solution, 30 ℃ of lower 60min that stir of constant temperature leave standstill 24h; Ultrasonication, (the Al of the quality such as adding and polynite
2O
3-ZrO
2) composite oxides, 50 ℃ of lower 60min that stir of constant temperature leave standstill 120min, the dry Al that gets
2O
3-ZrO
2/ polynite;
Step 3: utilize Al
2O
3-ZrO
2Cr in the/polynite adsorption of Low Concentration leather-making waste water
3+:
In every liter of lower concentration leather-making waste water, add Al
2O
3-ZrO
2/ polynite quality 0.1～30g is that 10～30 ℃, pH value are the Cr in the planar water under 2.0～13.0 the condition in temperature
3+, adsorption time is 1min ~ 6h, removes the Cr in the waste water
3+, collecting precipitation thing then;
Step 4: the regeneration of collecting precipitation thing:
After the throw out of collecting put container, place 25 ℃ of waters bath with thermostatic control, add washed with de-ionized water, then add the dilute sulphuric acid that volumetric molar concentration is 0.1mol/ L, the mass ratio of throw out and dilute sulphuric acid is 1:4; Wave 3min every 0.5h, desorb 3 hours is poured out supernatant liquor after centrifugal, add deionized water again clean to pH for neutral.
2. the method for utilizing aluminium zirconium tanning waste load polynite to remove chromium in the tanning waste water according to claim 1 is characterized in that:
In the step 1, the conditioning agent of pH value is NaOH solution, and its volumetric molar concentration is 2.0 mol/L, rate of addition 5.0mL/min, and the pH value is adjusted to 7.
3. the method for utilizing aluminium zirconium tanning waste load polynite to remove chromium in the tanning waste water according to claim 1 and 2 is characterized in that:
In the step 3, Cr in the lower concentration leather-making waste water
3+Starting point concentration be 5mg/L～40mg/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105563329A CN103011327A (en) | 2012-12-20 | 2012-12-20 | Method for removing chromium in tanning waste water by using aluminum zirconium tanning wastes to load montmorillonite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105563329A CN103011327A (en) | 2012-12-20 | 2012-12-20 | Method for removing chromium in tanning waste water by using aluminum zirconium tanning wastes to load montmorillonite |
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|---|---|
| CN103011327A true CN103011327A (en) | 2013-04-03 |
Family
ID=47960508
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012105563329A Pending CN103011327A (en) | 2012-12-20 | 2012-12-20 | Method for removing chromium in tanning waste water by using aluminum zirconium tanning wastes to load montmorillonite |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110614076A (en) * | 2019-10-14 | 2019-12-27 | 西安工程大学 | Preparation method of zirconium dioxide/aluminum oxide composite adsorption material |
| CN111732148A (en) * | 2020-06-29 | 2020-10-02 | 河海大学 | System for retrieve phosphate in follow surface eutrophic water |
| CN115465968A (en) * | 2022-09-16 | 2022-12-13 | 嘉兴学院 | Method for separating and recovering chromium in chrome tanning waste liquid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58202044A (en) * | 1982-05-21 | 1983-11-25 | Agency Of Ind Science & Technol | Preparation of novel (di)chromate ion adsorbent |
| CN102091609A (en) * | 2010-12-03 | 2011-06-15 | 于向真 | Modified clay new material and preparation method thereof |
| CN102233259A (en) * | 2010-05-04 | 2011-11-09 | 北京林业大学 | Adsorbent for removing heavy metal from water and preparation method of adsorbent |
| CN102745764A (en) * | 2012-07-20 | 2012-10-24 | 陕西科技大学 | Method of using aluminum-titanium composite tanning wastes to remove trivalent chromium in chrome tanning wastewater |
-
2012
- 2012-12-20 CN CN2012105563329A patent/CN103011327A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58202044A (en) * | 1982-05-21 | 1983-11-25 | Agency Of Ind Science & Technol | Preparation of novel (di)chromate ion adsorbent |
| CN102233259A (en) * | 2010-05-04 | 2011-11-09 | 北京林业大学 | Adsorbent for removing heavy metal from water and preparation method of adsorbent |
| CN102091609A (en) * | 2010-12-03 | 2011-06-15 | 于向真 | Modified clay new material and preparation method thereof |
| CN102745764A (en) * | 2012-07-20 | 2012-10-24 | 陕西科技大学 | Method of using aluminum-titanium composite tanning wastes to remove trivalent chromium in chrome tanning wastewater |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110614076A (en) * | 2019-10-14 | 2019-12-27 | 西安工程大学 | Preparation method of zirconium dioxide/aluminum oxide composite adsorption material |
| CN111732148A (en) * | 2020-06-29 | 2020-10-02 | 河海大学 | System for retrieve phosphate in follow surface eutrophic water |
| CN115465968A (en) * | 2022-09-16 | 2022-12-13 | 嘉兴学院 | Method for separating and recovering chromium in chrome tanning waste liquid |
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Application publication date: 20130403 |