CN1445031A - Recycling handles method for dirty mire containing heavy metals - Google Patents
Recycling handles method for dirty mire containing heavy metals Download PDFInfo
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- CN1445031A CN1445031A CN 02107442 CN02107442A CN1445031A CN 1445031 A CN1445031 A CN 1445031A CN 02107442 CN02107442 CN 02107442 CN 02107442 A CN02107442 A CN 02107442A CN 1445031 A CN1445031 A CN 1445031A
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Abstract
A process for reclaiming the sludge containing heavy metal includes such steps as cracking by mixing sludge with acidic solution and peroxide and high-temp reaction to release the mixed solution of high-molecular coagulant and metallic ions, the first homogenizing, the first separation for obtaining said coagulant used in treating sewage, the second homogenizing, the second separation for obtaining metallic oxide, and crystallizing separation for filtering the neutralizing material and oxidizing agent used for improving soil or treating water.
Description
Technical field
The invention relates to a kind of recycling handles method for dirty mire containing heavy metals, be meant especially a kind ofly heavy metal sewage sludge and printed circuit board (PCB) to be contained copper etchant solution (hereinafter to be referred as etching waste liquor) with the circulating processing and utilizing of carrying out.Recyclings such as solid metal oxide that produces after being about to handle and liquid water treatment agent, agglutinant have the valency utilization in processing procedure own, Waste Water Treatment or work, and can not produce the heavy metal sewage sludge recycling processing method of secondary public hazards.
Background technology
As everyone knows, the circuit card production accounts for suitable critical role in the strategic industries at home, also is the march toward importance industry of scientific and technological developed country of China.But because of mud and the high and low concentration etching solution that produces in the processing procedure, all contain heavy metal and waste liquid and be classified as harmful cause waste, thereby under the bright and new beautiful appearance that high development and height are made a profit, this industry problem of environmental pollution behind is the secret worry in this industry development in fact.According to incomplete statistics, the annual output of national circuit plate production surpasses the harmful mud more than 200,000 tons, and annual speed with 20% increases, and along with each process unit functional requirement in the printed circuit board (PCB) processing procedure, the organic or inorganic pharmaceutical chemicals that is added, also can produce various high-concentration waste liquids, as: video picture waste liquid, stripping waste liquid, etching waste liquor, tin-lead soldering waste liquid etc., therefore, how effectively to handle the problem of heavy metal sewage sludge and waste liquid thereof, be the quite deeply concerned and problem extremely to be solved of industry all the time.
At present the treatment process of the relevant heavy metal sewage sludge in home and abroad is a lot, as: bury, calcination, curing, high temperature melting, acidleach, ammonia are soaked etc., the English Patent of correlation technique has GE844722; United States Patent (USP) has 3,300, and 2 99,4,428,773,4,242,127,4,162,294,5,599,458,5,807,478,5,234, No. 669; The Taiwan patent has 81106585,82103460,89123260,89112071,89116503 etc.Its major defect is:
1, in above-mentioned numerous treatment process, the problem that all has the secondary public hazards, that is in terminal point of handling and process, all deleterious waste gas, waste water, waste can't be prevented really, and only be that it is handled in can received scope, and/or clear mechanism by sale monopoly and remove processing in accordance with the law, the risk that it is hidden behind, as: throw aside, bury the pollution hazard of cause arbitrarily to regional water quality or soil, or fail to transport to smoothly the waste of removing area and resource etc., be all the insurmountable problem of present various heavy metal sewage sludge treatment processs.
2, except the problem of secondary public hazards, the cost height of handling also becomes the important burden in dealer's operation, at present domestic unique government approval employing method is a solidification method, in the processing cost of right this method, promptly reach New Taiwan Currency 10-12 unit/kg (do not contain clear and processing cost is buried in the rear end), dealer for tons of every day, be heavy cost burden, the processing cost of more leisure opinion integral body is with present domestic this kind of employing treatment process reality and do not meet the whole economic benefit and the sustainable target of enterprise of resource reutilization.
Summary of the invention
Main purpose of the present invention provides a kind of recycling handles method for dirty mire containing heavy metals, can form complete waste life cycle circulation by treatment scheme, make the product in each cell processing processing procedure return utilization again in the processing procedure, or import Waste Water Treatment or utilize in the recovery system again and use, reach the purpose that can not produce the secondary public hazards.
Another purpose of the present invention provides a kind of recycling handles method for dirty mire containing heavy metals, by recycling handles method for dirty mire containing heavy metals, reaches the purpose that reduces production costs, increases the processing procedure benefit, reduces the generation of waste material, refuse.
The object of the present invention is achieved like this: a kind of recycling handles method for dirty mire containing heavy metals is characterized in that: it in turn includes the following steps:
(1) cleavage step is mud to be reached with sulphuric acid soln mix with the height/superoxide of the suitable weight ratio of mud, through the reaction treatment of high-temperature pressure for some time, disengages polymer coagulant and metal hydroxides mixed solution;
(2) first homogenizing steps are the mixed solutions after described cleavage step is handled, and adjust pH value at acid state;
(3) first separating steps are that the acid mixed solution after first homogenizing step is handled is isolated polymer coagulant and metal ion acidic solution;
(4) second homogenizing steps are with the isolated metal ion acidic solution of first separating step, adjust its pH value at the alkali sexual state;
(5) second separating steps are that alkali mixed solution after second homogenizing step is handled is isolated the saline solution that cupric oxide and residue contain oxygenant;
(6) Crystallization Separation step is that second separating step is handled the remaining acid waste liquid in back, filters to isolate salt compounds and oxidizing agent solution.
Height/the superoxide of this cleavage step and the weight ratio of mud are: height/superoxide 0.5-2: mud 40-50.This height/superoxide of this cleavage step is be selected from hydrogen peroxide, di-tert-butyl peroxide, dicumyl peroxide, tertiary butyl peroxide hexene or tertiary butyl peroxide hexane wherein at least a.Be to be selected from wherein at least a its pH value of adjustment of the acidic solution in sulfuric acid, hydrochloric acid, nitric acid, the micro-etched waste liquid in this first homogenizing step.It in this second homogenizing step wherein at least a its pH value of adjustment with the alkali solution that is selected from sodium hydroxide, lime, ammoniacal liquor, etching waste liquor.The temperature of this cleavage step is in 200-250 ℃ the scope.The treatment time of this cleavage step is 3-6 hour.The pH value of this first homogenizing step is 2-7.The pH value of this second homogenizing step is 7-11.The product that produces in this Crystallization Separation step is the wherein at least a of sodium sulfate, ammonium sulfate, sodium-chlor, Repone K, SODIUMNITRATE, ammonium nitrate, calcium sulfate or calcium chloride.This method comprises and further is provided with the stripping step, directly imports the micro-etched waste liquid of printed circuit board (PCB) factory or with general acid solution, enters cleavage step and mud mixed liquid is allocated.This stripping step further imports the handled oxyhydroxide of first separating step, or enters in first homogenizing step and/or second homogenizing step and allocate with mud mixed liquid.The copper content of this isolated cupric oxide is the 30-50 weight percent.This isolated polymer coagulant, its polymer content is the 20-40 weight percent.This isolated oxidizing agent solution, its addition that uses is 3.0-9.0 weight permillage.
Further specify below in conjunction with preferred embodiment and accompanying drawing.
Description of drawings
Fig. 1 is the schematic flow sheet of the embodiment 1 of recycling handles method for dirty mire containing heavy metals of the present invention.
Fig. 2 is the schematic flow sheet of the embodiment 2 of recycling handles method for dirty mire containing heavy metals of the present invention.
Fig. 3 is the schematic flow sheet of the embodiment 3 of recycling handles method for dirty mire containing heavy metals of the present invention.
Embodiment
Embodiment 1
Consult shown in Figure 1, recycling handles method for dirty mire containing heavy metals of the present invention comprises: cleavage step 2, first homogenizing step 3, first separating step 4, second homogenizing step 5, second separating step 6, Crystallization Separation step 7 and stripping step 8 etc., and the treatment scheme of concrete steps is as follows:
This cleavage step 2 is provided with treatment agent storage tank 20, be used to store height/superoxide, adopt di-tert-butyl peroxide in the present embodiment, other commercially available as: hydrogen peroxide, dicumyl peroxide, (tertiary butyl peroxide) hexene, (tertiary butyl peroxide) hexane etc. also all can adopt; In addition, be provided with sulphuric acid soln storage tank 21, be used to store sulphuric acid soln; And reactive tank 22 is provided with agitator in it, mud and above-mentioned solution can be stirred.Be earlier the t-butyl peroxide of 40kg or the sulphuric acid soln of other superoxide and 200kg to be put into reactive tank 22 on this step process, again the about 10% weight percent mud 9 of the cupric of 1000kg is put in the reactive tank 22, mixing formation 1240kg mixed solution stirs, because of reaction is warming up to about 220 ℃, and with normal pressure through about 4 hours reaction treatment, mud mixed liquid Central Plains can not be disengaged by sulphuric acid soln dissolved metal, and polymer coagulant in the mud mixed liquid destroyed by organo-peroxide, cut off polymer, and disengage metal hydroxides in the mud.The height/superoxide in this step and the weight ratio of mud can be done relative allotment with respect to mud at height/superoxide 0.5 to 2 between 40 to 50.Mixed solution after the processing enters first homogenizing step 3.
This first homogenizing step 3 is for storing acidic solution as sulfuric acid in stripping groove 30, what deserves to be mentioned is, stripping step 3 dissolution fluid storage tank 80 of the present invention can be used for storing the micro-etched waste liquid of the outer recycling of the present invention, and the copper ions acidic solution (or oxyhydroxide) after 4 processing of following the present invention's first separating step, can directly be used in the stripping groove 30 and utilize again, or store in aforementioned sulphuric acid soln storage tank 21, further cooperate the processing of the pressure filter of first separating step 4, can be with the 1240kg mud mixed solution after handling via cleavage step 2, adjust its pH value 2 to 7, present embodiment is mixed into 1840kg with the acidic solution of 600kg and handles, can adjust pH value is 5, and filter to isolate the acidic solution of moisture about 70% polymer coagulant of 950kg and 600kg copper ions, wherein polymer coagulant is then recyclable is used in the Waste Water Treatment again.
In addition, this second homogenizing step 5 has precipitation agent storage tank 50 and settling bath 51, wherein precipitation agent storage tank 50 can store alkali solution, as: lime, sodium hydroxide, ammoniacal liquor, give settling bath 51 to provide, present embodiment adds first separating step 4 with 50kg lime, isolate the acidic solution of 600kg copper ions, be mixed into the 650kg mixed solution, pressure filter at second separating step 6 is handled, and adjusts its pH value 7 to 9, contains about 50% cupric oxide and 400kg residue alkali solution and precipitate and isolate 250kg, wherein cupric oxide then can be directly as the raw material material of chemical industry or copper metallurgy industry, recycling.
After this Crystallization Separation step 7, it is provided with alkali solution storage tank 70, crystallizer tank 71 and the centrifugal filter 72 that stores the sulfur-bearing acid group, second separating step can be handled the remaining dissolution fluid crystallization in back filters to isolate vitriol and contains height/peroxide solution, the recyclable raw material that is used in industry or people's livelihood purposes of vitriol wherein, and residue height/peroxide solutions is through adjusting pH value to about neutrality, the treatment agent storage tank 20 that can directly import in the cleavage step 2 uses, or uses as the oxygenant of water treatment.
In sum, treatment scheme of the present invention can be found out the final product of copper-contained sludge in each fabrication process, is all returned in the processing procedure and utilizes, or import Waste Water Treatment or utilize in the recovery system and use, and can not produce the secondary pollution problem.
Consult shown in Figure 2, among the embodiment 2 of recycling handles method for dirty mire containing heavy metals of the present invention, comprise: cleavage step 2 ', first homogenizing step 3 ', first separating step 4 ', second homogenizing step 5 ', second separating step 6 ', Crystallization Separation step 7 ' and stripping step 8 ' etc., stripping step 8 wherein ' be different with embodiment 1, all the other steps are all identical with embodiment 1, and the flow process of each step is also identical, so do not repeat.Stripping step 8 in the present embodiment 2 ' be divided into micro-etched waste liquid storage tank 81 ' and dissolution fluid storage tank 82 ', stripping step 8 wherein ' is exclusively used in the cupric micro-etched waste liquid (hereinafter to be referred as micro-etched waste liquid) of storage by the outer printed circuit board (PCB) factory of the present invention; Dissolution fluid storage tank 82 ' is exclusively used in the acidic solution that reclaims the copper ions after first separating step 4 ' is handled.
Consult shown in Figure 3, among the embodiment 3 of recycling handles method for dirty mire containing heavy metals of the present invention, comprise: cleavage step 2 ", first homogenizing step 3 ", first separating step 4 ", the second equal homogenizing step 5 ", second separating step 6 ", Crystallization Separation step 7 " and stripping step 8 " etc. step; its difference is in stripping step 8 " establish micro-etched waste liquid storage tank 81 as embodiment 2 " and dissolution fluid storage tank 82 '; and add etching waste liquor storage tank 83 " store etching waste liquor separately, and the flow process of each step is still identical with embodiment 1, so do not repeat.
In addition, embodiments of the invention 4 can be with hydrogen peroxide as height/superoxide, and it is described that all the other flow processs are same as aforesaid embodiment 1-3, so do not repeat.
Embodiments of the invention 5 can be with hydrochloric acid as acid dissolution fluid, and it is described that all the other flow processs are same as aforesaid embodiment 1-3, so do not repeat.
Embodiments of the invention 6 can adopt lime as precipitation agent, and it is described that all the other flow processs are same as aforesaid embodiment 1-3, so do not repeat.
Embodiments of the invention 7 can adopt 1 to 5 to 5 to 1 di-tert-butyl peroxide, and it is described that all the other flow processs are same as aforesaid embodiment 1-3, so do not repeat.
Embodiments of the invention 8 can adopt tertiary butyl peroxide mixture of ethylene as height/superoxide, and it is described that all the other flow processs are same as aforesaid embodiment 1-3, so do not repeat.
Embodiments of the invention 9 can adopt nitric acid as acid dissolution fluid and use ammoniacal liquor as precipitation agent, and it is described that all the other flow processs are same as aforesaid embodiment 1-3, so do not repeat.
By the product of the foregoing description gained, wherein the analytical results of cupric oxide as shown in Table 1.The functional test results of polymer coagulant and oxygenant as shown in Table 2.
The analytical results of table cupric oxide
The functional test results of table two polymer coagulant and oxygenant
| Embodiment | ??Cu％ | ??Fe?ppm | ??Sn?ppm | ??Nippm | ??Zn?ppm | ??Pb?ppm | Salt |
| ?1 | ??36.73 | ??903.15 | ??2837.6 | ??683.4 | ??481.2 | ??103.4 | Sodium sulfate |
| ?2 | ??37.24 | ??914.22 | ??2854.2 | ??672.6 | ??489.5 | ??107.2 | Sodium sulfate |
| ?3 | ??28.01 | ??898.63 | ??2812.9 | ??693.5 | ??498.3 | ??115.8 | Ammonium sulfate |
| ?4 | ??42.33 | ??951.78 | ??2962.1 | ??722.2 | ??535.6 | ??137.2 | Calcium chloride |
| ?5 | ??43.57 | ??966.69 | ??2945.8 | ??737.8 | ??547.2 | ??142.6 | Calcium chloride sodium sulfate |
| ?6 | ??43.46 | ??942.59 | ??2973.9 | ??713.9 | ??551.5 | ??132.6 | Ammonium chloride |
| ?7 | ??41.39 | ??875.34 | ??2621.7 | ??654.3 | ??461.7 | ??87.7 | Ammonium nitrate |
| ?8 | ??40.99 | ??897.12 | ??2654.8 | ??662.4 | ??453.4 | ??91.4 | Ammonium nitrate ammonium sulfate |
| ?9 | ??41.83 | ??869.37 | ??2663.2 | ??649.1 | ??442.2 | ??80.6 | Ammonium nitrate |
| Embodiment | Polymer coagulant ‰ (annotating one) | Oxygenant ‰ (annotating three) |
| ??1 | 4.7 (25) (annotate two) | ?6.7 |
| ??2 | ?4.2(27) | ?7.0 |
| ??3 | ?5.0(22) | ?6.9 |
| ??4 | ?/ | ?4.2 |
| ??5 | ?/ | ?4.6 |
| ??6 | ?/ | ?4.5 |
| ??7 | ?3.2(31) | ?5.3 |
| ??8 | ?3.5(33) | ?5.9 |
| ??9 | ?3.1(30) | ?6.4 |
Annotate one: expression is removed to the required interpolation permillage of printed circuit board (PCB) industry wastewater discharge standard rate with metal ion in the waste water.
Annotate two: expression polymer coagulant content %.
Annotate three: expression is reduced to the required interpolation permillage of printed circuit board (PCB) industry wastewater discharge standard rate with the waste water of COD 200 to 500ppm.
In sum; recycling handles method for dirty mire containing heavy metals of the present invention has novelty, creativeness and practicality, and the above only is preferred embodiment of the present invention; all according to equivalence variation or modification person that the present invention did, all belong within protection scope of the present invention.
Claims (15)
1, a kind of recycling handles method for dirty mire containing heavy metals, it is characterized in that: it in turn includes the following steps:
(1) cleavage step is mud to be reached with sulphuric acid soln mix with the height/superoxide of the suitable weight ratio of mud, through the reaction treatment of high-temperature pressure for some time, disengages polymer coagulant and metal hydroxides mixed solution;
(2) first homogenizing steps are the mixed solutions after described cleavage step is handled, and adjust pH value at acid state;
(3) first separating steps are that the acid mixed solution after first homogenizing step is handled is isolated polymer coagulant and metal ion acidic solution;
(4) second homogenizing steps are with the isolated metal ion acidic solution of first separating step, adjust its pH value at the alkali sexual state;
(5) second separating steps are that alkali mixed solution after second homogenizing step is handled is isolated the saline solution that cupric oxide and residue contain oxygenant;
(6) Crystallization Separation step is that second separating step is handled the remaining acid waste liquid in back, filters to isolate salt compounds and oxidizing agent solution.
2, recycling handles method for dirty mire containing heavy metals according to claim 1 is characterized in that: the height/superoxide of this cleavage step and the weight ratio of mud are: height/superoxide 0.5-2: mud 40-50.
3, recycling handles method for dirty mire containing heavy metals according to claim 1 is characterized in that: this height/superoxide of this cleavage step is be selected from hydrogen peroxide, di-tert-butyl peroxide, dicumyl peroxide, tertiary butyl peroxide hexene or tertiary butyl peroxide hexane wherein at least a.
4, recycling handles method for dirty mire containing heavy metals according to claim 1 is characterized in that: be to be selected from wherein at least a its pH value of adjustment of the acidic solution in sulfuric acid, hydrochloric acid, nitric acid, the micro-etched waste liquid in this first homogenizing step.
5, recycling handles method for dirty mire containing heavy metals according to claim 1 is characterized in that: be wherein at least a its pH value of adjustment with the alkali solution that is selected from sodium hydroxide, lime, ammoniacal liquor, etching waste liquor in this second homogenizing step.
6, according to one of them described recycling handles method for dirty mire containing heavy metals of claim 1-5, it is characterized in that: the temperature of this cleavage step is in 200-250 ℃ the scope.
7, according to one of them described recycling handles method for dirty mire containing heavy metals of claim 1-5, it is characterized in that: the treatment time of this cleavage step is 3-6 hour.
8, according to one of them described recycling handles method for dirty mire containing heavy metals of claim 1-5, it is characterized in that: the pH value of this first homogenizing step is 2-7.
9, according to one of them described recycling handles method for dirty mire containing heavy metals of claim 1-5, it is characterized in that: the pH value of this second homogenizing step is 7-10.
10, according to one of them described recycling handles method for dirty mire containing heavy metals of claim 1-5, it is characterized in that: the product that produces in this Crystallization Separation step is the wherein at least a of sodium sulfate, ammonium sulfate, sodium-chlor, Repone K, SODIUMNITRATE, ammonium nitrate, calcium sulfate or calcium chloride.
11, according to one of them described recycling handles method for dirty mire containing heavy metals of claim 1-5, it is characterized in that: this method comprises and further is provided with the stripping step, directly import the micro-etched waste liquid of printed circuit board (PCB) factory or with general acid solution, enter cleavage step and mud mixed liquid is allocated.
12, according to one of them described recycling handles method for dirty mire containing heavy metals of claim 1-5, it is characterized in that: this stripping step further imports the handled oxyhydroxide of first separating step, or enters in first homogenizing step and/or second homogenizing step and allocate with mud mixed liquid.
13, according to one of them described recycling handles method for dirty mire containing heavy metals of claim 1-12, it is characterized in that: the copper content of this isolated cupric oxide is the 30-50 weight percent.
14, according to one of them described recycling handles method for dirty mire containing heavy metals of claim 1-12, it is characterized in that: this isolated polymer coagulant, its polymer content is the 20-40 weight percent.
15, according to one of them described recycling handles method for dirty mire containing heavy metals of claim 1-12, it is characterized in that: this isolated oxidizing agent solution, its addition that uses is 3.0-9.0 weight permillage.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1326639C (en) * | 2004-06-18 | 2007-07-18 | 林裕城 | Method for recovering and treating sewage sludge containing metals |
| CN100503486C (en) * | 2005-02-25 | 2009-06-24 | 惠州大亚湾惠绿环保服务有限公司 | Method for treating waste sludge in wiring board plant into resources |
| CN101858066A (en) * | 2010-04-30 | 2010-10-13 | 北京道顺国际技术开发有限责任公司 | Recycling comprehensive treatment method for endogenous pollution of substrate sludge of lake |
| CN101914404A (en) * | 2010-08-20 | 2010-12-15 | 长沙达华污泥处理科技有限公司 | Method for preparing solid fuel from sludge of sewage treatment plant |
| CN101935121A (en) * | 2010-09-02 | 2011-01-05 | 昆山联鼎环保科技有限公司 | Process for recycling alkali waste etching liquid |
| CN101974359A (en) * | 2010-09-06 | 2011-02-16 | 长沙洁湘环保工程有限公司 | Method for preparing industrial carbons by sludge |
| CN102040238A (en) * | 2010-11-11 | 2011-05-04 | 上海集惠环保科技发展有限公司 | Recycling method for treating sludge containing heavy metals |
| CN105945052A (en) * | 2016-05-30 | 2016-09-21 | 青岛理工大学 | Heavily-polluted site Pb in-situ and ex-situ couplingdetoxificationmethod |
| CN107721106A (en) * | 2017-11-22 | 2018-02-23 | 云南大地绿坤环保科技有限公司 | Utilize the method for acid-soluble oil body refuse processing heavy metal sewage sludge |
-
2002
- 2002-03-15 CN CN 02107442 patent/CN1210114C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1326639C (en) * | 2004-06-18 | 2007-07-18 | 林裕城 | Method for recovering and treating sewage sludge containing metals |
| CN100503486C (en) * | 2005-02-25 | 2009-06-24 | 惠州大亚湾惠绿环保服务有限公司 | Method for treating waste sludge in wiring board plant into resources |
| CN101858066A (en) * | 2010-04-30 | 2010-10-13 | 北京道顺国际技术开发有限责任公司 | Recycling comprehensive treatment method for endogenous pollution of substrate sludge of lake |
| CN101914404A (en) * | 2010-08-20 | 2010-12-15 | 长沙达华污泥处理科技有限公司 | Method for preparing solid fuel from sludge of sewage treatment plant |
| CN101914404B (en) * | 2010-08-20 | 2013-04-10 | 长沙达华污泥处理科技有限公司 | Method for preparing solid fuel from sludge of sewage treatment plant |
| CN101935121A (en) * | 2010-09-02 | 2011-01-05 | 昆山联鼎环保科技有限公司 | Process for recycling alkali waste etching liquid |
| CN101974359A (en) * | 2010-09-06 | 2011-02-16 | 长沙洁湘环保工程有限公司 | Method for preparing industrial carbons by sludge |
| CN102040238A (en) * | 2010-11-11 | 2011-05-04 | 上海集惠环保科技发展有限公司 | Recycling method for treating sludge containing heavy metals |
| CN105945052A (en) * | 2016-05-30 | 2016-09-21 | 青岛理工大学 | Heavily-polluted site Pb in-situ and ex-situ couplingdetoxificationmethod |
| CN107721106A (en) * | 2017-11-22 | 2018-02-23 | 云南大地绿坤环保科技有限公司 | Utilize the method for acid-soluble oil body refuse processing heavy metal sewage sludge |
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