CN102745766A - Method for treating leather dyeing wastewater by using chromium-enriched sludge - Google Patents
Method for treating leather dyeing wastewater by using chromium-enriched sludge Download PDFInfo
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Abstract
A method for treating leather dyeing wastewater by using chromium-enriched sludge includes the following steps of firstly, preheating the chromium-enriched sludge: crushing the blocky chromium-enriched sludge; secondly, performing acid leaching: using a sulfuric acid solution as an extractant of chromium, adding chromium-enriched sludge powders into the sulfuric acid solution and subjecting the mixture to reaction for 60-180 minutes, wherein the volume ratio of sulfuric acid and water of the sulfuric acid solution is (1:5)-(1:20); thirdly, performing solution-residue separation: separating the chromium-enriched sludge powders which are subjected to acid leaching into chromium liquid and primary solid residues, subjecting the chromium liquid to acid leaching, storing the chromium liquid for standby and collecting the primary solid residues for the next treatment; fourthly, performing secondary treatment: adding a phosphoric acid solution into the primary solid residues in a container to react for 10-180 minutes; fifthly, recycling secondary solid residues: subjecting a mixture which is obtained from the reaction of the step four to solid-liquid separation, collecting liquid for standby and recycling the secondary solid residues for the next treatment; and sixthly, absorbing the dyeing wastewater: placing the secondary solid residues obtained from the step five into the leather dyeing wastewater and reducing chromaticity of the dyeing wastewater to the standard of chromaticity of water treatment. The method for treating the leather dyeing wastewater by using the chromium-enriched sludge has the advantages of being simple in process and capable of conserving energy and reducing emission.
Description
Technical field
The invention belongs to environmental technology field, relate to first processing, secondary treatment and the body refuse application method of the rich chromium mud of process hides, be specifically related to a kind of method of utilizing rich chromium sludge treatment leather coloring waste water.
Background technology
Can produce a large amount of trivalent chromium waste water that contain in the leather industry; Rich chromium mud is directed to handles the chromium cake that Chrome Tanning Wastewater produces; Accumulated the trivalent chromium compound of a large amount of chromium hydroxides and a small amount of other form in this part solid waste,, can cause secondary pollution if deal with improperly; Also can lose a large amount of chromium, all be irrational from resource view and environmental.At present, existing treatment process has the recycle of preparation tanning agent, preparation haydite, coating pigment etc., and direct landfill, burning, biological compost etc. are also arranged.
The patent No. is that [200910230708.5], name are called the patent of " a kind of method of utilizing leather-making mud to prepare haydite "; Leather-making mud, clay, flyash are processed ceramic product through high temperature sintering according to a certain percentage; Be a kind of cope well method, but energy consumption is bigger, technology is more loaded down with trivial details.
The patent No. is that [201110249007.3], name are called the patent of " method of regenerated using chromium mud from the tanned waste liquid of hair leather skin "; With adjusting potential of hydrogen after the acidifying of chromium mud cake; Adding chromium powder in proportion is made into tanning agent and is back to tanning; Can practice thrift the discharging of waste liquid, but this method there is certain influence to the stability of leather tanning effect in the big production, the quality of wet blue.
The patent No. is that [200610023805.3], name are called the patent of " a kind of chromium of steel plant wastewater mud reclaims and method of resource "; Mud is mixed the back 600～900 ℃ of following roastings with yellow soda ash; And realize the recovery of chromium with flooding, residue uses as the raw material of good biogas desulfurizer.This method has proposed a kind of processing thinking of chromium mud, but energy consumption is bigger, and the processing of pollutent is thorough inadequately.
Summary of the invention
In order to overcome the deficiency of prior art; The object of the present invention is to provide a kind of rich chromium sludge treatment leather coloring method for waste water that utilizes, two steps of rich chromium mud have been handled take off the effective way that chromium utilizes the secondary waste simultaneously, will take off body refuse behind the chromium and be used to prepare sorbing material and handle waste water once more; Technology is simple; Play environmental protection, energy-conservation effect, reach the purpose of " treatment of wastes with processes of wastes against one another ", for the processing of rich chromium mud provides new method.
To achieve these goals, the technical scheme that the present invention adopts is: a kind ofly utilize rich chromium sludge treatment leather coloring method for waste water, rich chromium mud utilizes after taking off chromium again, may further comprise the steps:
The solid slag of rich chromium mud pre-treatment → acidleach processing → melt cinder separation → secondary treatment → recovery secondary → absorption dyeing waste-water;
The concrete technical scheme of aforesaid operations step is following:
One, the pre-treatment of rich chromium mud: blocky rich chromium mud is pulverized;
Two, acidleach is handled: with sulfuric acid and water volume ratio is that the sulphuric acid soln of 1:5～1:20 is as the chromium extraction agent; With step 1) rich chromium mud powder add sulphuric acid soln; The solid-to-liquid ratio of rich chromium mud powder and sulphuric acid soln is 1:1～1:20, and sludge quality unit is g, and then the sulfuric acid volume unit is mL; Mud unit is kg, and then the sulfuric acid volume unit is L, under 20～60 ℃ of conditions, reacts 60～180min;
Three, melt cinder separates: will pass through step 2) the rich chromium mud powder separation handled of acidleach is chrome liquor and first slag admittedly, and the acidleach chrome liquor stores for future use, and slag collects and does next step processing admittedly for the first time;
Four, secondary treatment: (phosphoric acid solution is that the volume ratio of phosphoric acid and water is 1:5～1:30) to add phosphoric acid solution in the first slag admittedly in container; Making the solid-to-liquid ratio of first slag admittedly and phosphoric acid solution is 1:1～1:20; First slag amount unit admittedly is g, and then the phosphoric acid volume unit is mL; First slag unit admittedly is kg, and then the phosphoric acid volume unit is L, under 20～60 ℃ of conditions, reacts 10～180min;
Five, the solid slag of recovery secondary: with step 4) post reaction mixture is carried out solid-liquid separation, and liquid collecting is subsequent use, and the solid slag of secondary reclaims does next step utilization;
Six, absorption dyeing waste-water: get step 5) to place mass concentration be the leather coloring waste water of 10mg/L～1g/L to the solid slag of secondary, and solid-to-liquid ratio is 10:1～1:1, and the solid slag amount unit of secondary is g, and then the dyeing waste-water volume unit is mL; The solid slag unit of secondary is kg, and then the dyeing waste-water volume unit is L, and behind treated 10～180min, the colourity of dyeing waste-water obviously is reduced to the standard of water treatment colourity.
Beneficial effect of the present invention:
The present invention chooses the rich chromium mud of tannery; Use common sulphuric acid soln and phosphoric acid solution that mud is extracted; Body refuse has after treatment reached State Standard of the People's Republic of China's soil environment quality standard GB15618-1995; The primary standard that is chromium in the paddy field is 90mg/kg, and secondary standard is respectively 250mg/kg, 300mg/kg, 350mg/kg, and grade III Standard is 400mg/kg; The primary standard of chromium is 150mg/kg in the nonirrigated farmland; Secondary standard is respectively 150mg/kg, 200mg/kg, 250mg/kg; Grade III Standard is 300mg/kg and urban wastewater treatment firm pollutant emission standard GB18918-2002; The per day the highest permission discharge value of total chromium is 0.1mg/L, and chromic the highest per day permission discharge value is 0.05mg/L; Solid slag after treatment is directly discharging, and with the dyeing waste-water that its absorption tannery discharges, the method that belongs to a kind of cyclic regeneration is handled rich chromium mud, has utilized harmful solid waste greatly, has that technology is simple, the characteristics of energy-saving and emission-reduction.
Description of drawings
Fig. 1 is the testing standard sample.
Fig. 2 is the massfraction of rich each element atom of chromium mud of being untreated.
Fig. 3 handles the massfraction of each element atom of back for the chromium-bearing sludge acidleach.
Fig. 4 is the massfraction of each element atom after the secondary treatment.
Fig. 5 is the preceding mud Electronic Speculum figure of absorption.
Fig. 6 is the mud Electronic Speculum figure after adsorbing.
Fig. 7 is the ultraviolet spectrogram contrast of waste water from dyestuff before and after the absorption.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is done further explain.
Embodiment one
A kind ofly utilize rich chromium sludge treatment leather coloring method for waste water, may further comprise the steps:
One, the pre-treatment of rich chromium mud: blocky chromium-bearing sludge is pulverized;
Two, acidleach is handled: the sulphuric acid soln of choosing sulfuric acid and water volume ratio and be 1:5 is as the chromium extraction agent; With step 1) rich chromium mud powder and the solid-to-liquid ratio of sulphuric acid soln be controlled to be 1:5; Chromium mud powder quality unit is g, and the volume unit of sulphuric acid soln is mL, reacts 30min down at 20 ℃;
Three, melt cinder separates: will pass through step 2) the rich chromium mud powder separation handled of acidleach is chrome liquor and first slag admittedly, and the acidleach chrome liquor stores for future use, and slag collects and does next step processing admittedly for the first time;
Four, secondary treatment: choose the phosphoric acid solution that phosphoric acid and water volume ratio are 1:5, the solid-to-liquid ratio of first slag admittedly of control and phosphoric acid solution is 1:5, and slag amount unit is g admittedly for the first time, and the volume unit of phosphoric acid solution is mL, effect 30min under 20 ℃;
Five, the solid slag of recovery: with step 4) post reaction mixture is carried out solid-liquid separation, and liquid collecting is for use, and the solid slag of secondary is collected and done next step utilization;
Six, absorption dyeing waste-water: get step 5) to place mass concentration be the leather coloring waste water of 500mg/L to the solid slag of secondary, and solid-to-liquid ratio is 10:1, and the solid slag amount unit of secondary is g, and the volume unit of dyeing waste-water is mL, handles 30min.
Embodiment two
A kind ofly utilize rich chromium sludge treatment leather coloring method for waste water, may further comprise the steps:
One, the pre-treatment of rich chromium mud: blocky chromium-bearing sludge is pulverized;
Two, acidleach is handled: the sulfuric acid of choosing volume ratio and be 1:10 is as the chromium extraction agent; With step 1) rich chromium mud powder and the solid-to-liquid ratio of sulphuric acid soln be controlled to be 1:10; Chromium mud powder quality unit is g, and the volume unit of sulphuric acid soln is mL, reacts 30min down at 40 ℃;
Three, melt cinder separates: the chromium-bearing sludge that will pass through the acidleach processing is separated into chrome liquor and first slag admittedly, and the acidleach chrome liquor stores for future use, and slag collects and does next step processing admittedly for the first time;
Four, secondary treatment: choose the phosphoric acid solution that volume ratio is 1:5, the solid-to-liquid ratio of first slag admittedly of control and phosphoric acid solution is 1:5, and slag amount unit is g admittedly for the first time, and the volume unit of phosphoric acid solution is mL, effect 90min under 40 ℃;
Five, the solid slag of recovery: with step 4) post reaction mixture is carried out solid-liquid separation, and liquid collecting is for use, and the solid slag of secondary is collected and done next step utilization;
Six, absorption dyeing waste-water: get step 5) to place mass concentration be the leather coloring waste water of 300mg/L to the solid slag after the secondary treatment, and solid-to-liquid ratio is 5:1, and the solid slag amount unit after the processing is g, and the volume unit of dyeing waste-water is mL, and concentration is handled 90min.
Embodiment three
A kind ofly utilize rich chromium sludge treatment leather coloring method for waste water, may further comprise the steps:
One, rich chromium mud pre-treatment: blocky chromium-bearing sludge is pulverized;
Two, acidleach is handled: the sulfuric acid of choosing volume ratio and be 1:20 is as the chromium extraction agent; With step 1) rich chromium mud powder and the solid-to-liquid ratio of sulphuric acid soln be controlled to be 1:1; Chromium mud powder quality unit is g, and the volume unit of sulphuric acid soln is mL, reacts 180min down at 60 ℃;
Three, melt cinder separates: will pass through step 2) the rich chromium mud powder separation handled of acidleach is chrome liquor and first slag admittedly, and the acidleach chrome liquor stores for future use, and slag collects and does next step processing admittedly for the first time;
Four, secondary treatment: choose the phosphoric acid solution that volume ratio is 1:5, the solid-to-liquid ratio of first slag admittedly of control and phosphoric acid solution is 1:5, Gu slag amount unit is g, the volume unit of phosphoric acid solution is mL, acts on 180min down at 60 ℃;
Five, the solid slag of recovery: with step 4) post reaction mixture is carried out solid-liquid separation, and liquid collecting is for use, does next step utilization Gu slag is collected;
Six, absorption dyeing waste-water: get step 5) to place mass concentration be the leather coloring waste water of 10mg/L to the solid slag of secondary, and solid-to-liquid ratio is 1:1, and the solid slag amount unit of secondary is g, and the volume unit of dyeing waste-water is mL, handles 180min.
In order to verify beneficial effect of the present invention, the contriver handles the chromium-bearing sludge method to the embodiment of the invention 2 and tests.Test case is following:
The Oxford INCA newton energy spectrometer that used instrument is produced for Oxford instrument company, but the content of contained each element in this instrument rapid and accurate determination pressed powder sample.Before the test sample is thoroughly dried grinding and be fine-powder.
The standard model of test shows the element kind that this instrument can directly be measured when using for instrument referring to Fig. 1.Can survey Elements C, its corresponding standard model is CaCO
3, element O, its corresponding standard model is SiO
2, Elements C a, its corresponding standard model is the calcium lime stone, element Cr, its corresponding standard model is Cr, other element is not listed one by one.
In the as can be seen from Figure 2 untreated original chromium-bearing sludge: the massfraction of Elements C is 19.54%; The massfraction of element O is 24.67%; The massfraction of Elements C a is 3.89%, and the massfraction of element Cr is 42.76%, and the massfraction of other element is 9.14%.
As can be seen from Figure 3 in the chromium-bearing sludge through the acidleach processing: the massfraction of Elements C is 36.71%; The massfraction of element O is 25.18%; The massfraction of elements Si is 1.08%; The massfraction of element S is 14.76%, and the massfraction of Elements C a is 21.66%, and the massfraction of element Cr is 0.60%.After showing that acidleach is handled, by a large amount of removals, residual volume only reaches 0.60% to Cr from primary sludge.
After as can beappreciated from fig. 4 passing through secondary treatment, the massfraction of Elements C is 17.42% in the body refuse, and the massfraction of element O is 22.35%, and the massfraction of Elements C a is 10.03%, and the massfraction of element Cr is 0.48%.This content that is illustrated in through Cr element after the secondary treatment has reached lower, is merely 0.48%, proves that it is effective that secondary treatment is taken off chromium to body refuse.
Configuration of surface such as Fig. 5 and shown in Figure 6 of before the absorption and absorption back body refuse.Solid slag surface before and after the absorption is observed when amplifying 1000 times through ESEM; Can find out that the solid slag surface before the absorption is more smooth; Too much particle does not appear; And obvious some dyestuff molecules that adsorbed can be found out in the solid slag surface after the absorption, and this shows that the solid slag after the processing has tangible adsorption effect to this dyestuff.
Fig. 7 is waste water from dyestuff absorbancy contrast before and after handling, and adopts the beautiful UV2300 ultraviolet spectrophotometer in sky, Shanghai that the dyeing waste-water before and after the absorption is measured, and the result is as shown in Figure 7.510nm represents the characteristic absorption wavelength of dye molecule; Before the absorption, dyeing waste-water is that 510nm exists stronger absorption peak at wavelength, and through after the body refuse processing that obtains; Waste water is the absorption peak disappearance of 510nm at wavelength; Simultaneously do not occur absorbing in other wavelength, color and pure water color indifference show that the body refuse after dye granule in the dyeing waste-water is processed adsorbs fully.
It is thus clear that rich chromium mud has been removed the Cr element after handling through technological step of the present invention basically; Solid slag after handling is simultaneously used as sorbing material can effectively remove the dye granule in the dyeing waste-water, explains that the solid slag after this art breading can use as the sorbing material of removing dyeing waste-water well.
Claims (4)
1. one kind is utilized rich chromium sludge treatment leather coloring method for waste water, it is characterized in that, may further comprise the steps:
One, the pre-treatment of rich chromium mud: blocky rich chromium mud is pulverized;
Two, acidleach is handled: with sulfuric acid and water volume ratio is that the sulphuric acid soln of 1:5～1:20 is as the chromium extraction agent; With step 1) rich chromium mud powder add sulphuric acid soln; The solid-to-liquid ratio of rich chromium mud powder and sulphuric acid soln is 1:1～1:20, and sludge quality unit is g, and then the sulfuric acid volume unit is mL; Mud unit is kg, and then the sulfuric acid volume unit is L, under 20～60 ℃ of conditions, reacts 60～180min;
Three, melt cinder separates: will pass through step 2) the rich chromium mud powder separation handled of acidleach is chrome liquor and first slag admittedly, and the acidleach chrome liquor stores for future use, and slag collects and does next step processing admittedly for the first time;
Four, secondary treatment: (phosphoric acid solution is that phosphoric acid and water volume ratio are 1:5～1:30) to add phosphoric acid solution in the first slag admittedly in container; Making the solid-to-liquid ratio of first slag admittedly and phosphoric acid solution is 1:1～1:20; First slag amount unit admittedly is g, and then the phosphoric acid volume unit is mL; First slag unit admittedly is kg, and then the phosphoric acid volume unit is L, under 20～60 ℃ of conditions, reacts 10～180min;
Five, the solid slag of recovery secondary: with step 4) post reaction mixture is carried out solid-liquid separation, and liquid collecting is subsequent use, and the solid slag of secondary reclaims does next step utilization;
Six, absorption dyeing waste-water: get step 5) to place mass concentration be the leather coloring waste water of 10mg/L～1g/L to the solid slag of secondary, and solid-to-liquid ratio is 10:1～1:1, and the solid slag amount unit of secondary is g, and then the dyeing waste-water volume unit is mL; The solid slag unit of secondary is kg, and then the dyeing waste-water volume unit is L, and behind treated 10～180min, the colourity of dyeing waste-water obviously is reduced to the standard of water treatment colourity.
2. a kind of rich chromium sludge treatment leather coloring method for waste water that utilizes according to claim 1 is characterized in that, may further comprise the steps:
One, the pre-treatment of rich chromium mud: blocky chromium-bearing sludge is pulverized;
Two, acidleach is handled: the sulfuric acid of choosing volume ratio and be 1:5 is as the chromium extraction agent; With step 1) rich chromium mud powder and the solid-to-liquid ratio of sulphuric acid soln be controlled to be 1:5; Chromium mud powder quality unit is g, and the volume unit of sulphuric acid soln is mL, reacts 30min down at 20 ℃;
Three, melt cinder separates: will pass through step 2) the rich chromium mud powder separation handled of acidleach is chrome liquor and first slag admittedly, and the acidleach chrome liquor stores for future use, and slag collects and does next step processing admittedly for the first time;
Four, secondary treatment: choose the phosphoric acid solution that volume ratio is 1:5, the solid-to-liquid ratio of first slag admittedly of control and phosphoric acid solution is 1:5, and slag amount unit is g admittedly for the first time, and the volume unit of phosphoric acid solution is mL, effect 30min under 20 ℃, and the chromium clearance is 14.4%;
Five, the solid slag of recovery: with step 4) post reaction mixture is carried out solid-liquid separation, and liquid collecting is for use, and the solid slag of secondary is collected and done next step utilization;
Six, absorption dyeing waste-water: get step 5) to place mass concentration be the leather coloring waste water of 500mg/L to the solid slag of secondary, and solid-to-liquid ratio is 10:1, and the solid slag amount unit of secondary is g, and the volume unit of dyeing waste-water is mL, handles 30min.
3. a kind of rich chromium sludge treatment leather coloring method for waste water that utilizes according to claim 1 is characterized in that, may further comprise the steps:
One, the pre-treatment of rich chromium mud: blocky chromium-bearing sludge is pulverized;
Two, acidleach is handled: the sulfuric acid of choosing volume ratio and be 1:10 is as the chromium extraction agent; With step 1) rich chromium mud powder and the solid-to-liquid ratio of sulphuric acid soln be controlled to be 1:10; Chromium mud powder quality unit is g, and the volume unit of sulphuric acid soln is mL, reacts 30min down at 40 ℃;
Three, melt cinder separates: the chromium-bearing sludge that will pass through the acidleach processing is separated into chrome liquor and first slag admittedly, and the acidleach chrome liquor stores for future use, and slag collects and does next step processing admittedly for the first time;
Four, secondary treatment: choose the phosphoric acid solution that volume ratio is 1:5, the solid-to-liquid ratio of first slag admittedly of control and phosphoric acid solution is 1:5, and slag amount unit is g admittedly for the first time, and the volume unit of phosphoric acid solution is mL, effect 90min under 40 ℃;
Five, the solid slag of recovery: with step 4) post reaction mixture is carried out solid-liquid separation, and liquid collecting is for use, and the solid slag of secondary is collected and done next step utilization;
Six, absorption dyeing waste-water: get step 5) to place mass concentration be the leather coloring waste water of 300mg/L to the solid slag of secondary, and solid-to-liquid ratio is 5:1, and the solid slag amount unit of secondary is g, and the volume unit of dyeing waste-water is mL, handles 90min.
4. a kind of rich chromium sludge treatment leather coloring method for waste water that utilizes according to claim 1 is characterized in that, may further comprise the steps:
One, rich chromium mud pre-treatment: blocky chromium-bearing sludge is pulverized;
Two, acidleach is handled: the sulfuric acid of choosing volume ratio and be 1:20 is as the chromium extraction agent; With step 1) rich chromium mud powder and the solid-to-liquid ratio of sulphuric acid soln be controlled to be 1:1; Chromium mud powder quality unit is g, and the volume unit of sulphuric acid soln is mL, reacts 180min down at 60 ℃;
Three, melt cinder separates: will pass through step 2) the rich chromium mud powder separation handled of acidleach is chrome liquor and first slag admittedly, and the acidleach chrome liquor stores for future use, and slag collects and does next step processing admittedly for the first time;
Four, secondary treatment: choose the phosphoric acid solution that volume ratio is 1:5, the solid-to-liquid ratio of first slag admittedly of control and phosphoric acid solution is 1:5, Gu slag amount unit is g, the volume unit of phosphoric acid solution is mL, acts on 180min down at 60 ℃;
Five, the solid slag of recovery: with step 4) post reaction mixture is carried out solid-liquid separation, and liquid collecting is for use, does next step utilization Gu slag is collected;
Six, absorption dyeing waste-water: get step 5) to place mass concentration be the leather coloring waste water of 10mg/L to the solid slag of secondary, and solid-to-liquid ratio is 1:1, and the solid slag amount unit of secondary is g, and the volume unit of dyeing waste-water is mL, handles 180min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310733A (en) * | 2014-11-05 | 2015-01-28 | 北京泛博化学股份有限公司 | Method and device for recycling chromium-containing sludge |
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| JPH1133594A (en) * | 1996-06-07 | 1999-02-09 | Shiro Yoshizaki | Method for removing heavy metals from sludges |
| CN102303940A (en) * | 2011-08-22 | 2012-01-04 | 陕西科技大学 | Method for treating sludge containing trivalent chromium |
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2012
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH1133594A (en) * | 1996-06-07 | 1999-02-09 | Shiro Yoshizaki | Method for removing heavy metals from sludges |
| CN102303940A (en) * | 2011-08-22 | 2012-01-04 | 陕西科技大学 | Method for treating sludge containing trivalent chromium |
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| Title |
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| K. FYTIANOS等: "LEACHING OF HEAVY METALS FROM MUNICIPAL SEWAGE SLUDGE", 《ENVIRONMENT INTERNATIONAL》 * |
| MARINOS A. STYLIANOU等: "Effect of acid treatment on the removal of heavy metals from sewage sludge", 《DESALINATION》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310733A (en) * | 2014-11-05 | 2015-01-28 | 北京泛博化学股份有限公司 | Method and device for recycling chromium-containing sludge |
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