CN101269889A - Processing method for stainless steel acid cleaning waste water and liquid - Google Patents
Processing method for stainless steel acid cleaning waste water and liquid Download PDFInfo
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- CN101269889A CN101269889A CNA2007100677498A CN200710067749A CN101269889A CN 101269889 A CN101269889 A CN 101269889A CN A2007100677498 A CNA2007100677498 A CN A2007100677498A CN 200710067749 A CN200710067749 A CN 200710067749A CN 101269889 A CN101269889 A CN 101269889A
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Abstract
The invention relates to a processing method of stainless steel pickling waste liquid, which is characterized in that the processing method includes the steps that: neutral salt wastewater flows into a neutral reduction cell, and mixed acid pickling waste waters flow into a neutralizing tank; reducing agent is added into the neutral reduction cell, and then the reduced wastewater liquid is put into the neutralizing tank and is mixed with the adjusted mixed acid pickling waste waters, and liquid alkali is added into the neutralizing tank; the separated clear waste liquid removes fluorin ions in a settlement tank; neutralizing liquid is added into a final neutralizing tank to cause the pH value of treatment liquid to adjust to be neutralized wastewater liquid which passes through a sand filter to be discharged. The processing method has the advantages that metal ions and fluorin ions are performed the subsection treatment, and neutralizing agent is changed into the liquid alkali from lime cream, the requirement of reaching the standard of the waste liquid emission is not only achieved, but also the mud quantity produced by a mass of lime cream is greatly reduced, heavy metal mud of a retention pond only contains heavy metal compound, the salts of calcium fluoride and calcium sulphate, etc. are separated from the inclined plate settlement tank during the fluoridation stage, thereby the treatment cost is effectively lowered.
Description
Technical field
The present invention relates to a kind of mud branch matter of stainless steel cold-rolling pickling wastewater liquid and the treatment process of decrement.
Background technology
In the acid-washing stainless steel process, can produce acid cleaning waste water and liquid, acid cleaning waste water and liquid has neutral exhausted water and acid waste water liquid, in neutral exhausted water, contain sexavalent chrome, nickel, iron, sodium and sulfate radical plasma, pH value scope in the exhausted water is 3～4, wherein the concentration of hexavalent chromium is in 200～600mg/L scope, and sexavalent chrome is to need pretreated ions.Contain nickel, iron, manganese, nitrate radical and fluorion plasma in the acid waste water liquid of nitration mixture, the wastewater pH scope is 2～3, and wherein nickel, iron, manganese and fluorion are the ions that needs removal.
The exhausted water treatment process of enterprises of producing stainless steel employing both at home and abroad is at first to adopt oxidation reduction process that hexavalent chrome reduction is become trivalent chromium at present, sodium bisulfite is as reductive agent, with hydrochloric acid with the pH value transfer to 2.5～3, ORP (redox potential) value is controlled at 280～320mv; To mix by pretreated neutral salt waste water and nitration mixture pickling waste waters then, and adopt the neutralization precipitation method that each heavy metal ion and fluorion are removed; Use milk of lime as neutralizing agent, reaction pH value is controlled at 9.5～10.5; Waste water after the neutralization carries out the muddy water shunting at the reaction settling pond, and the mud thing is handled by outward transport after the plate-and-frame filter press press filtration, and exhausted water carries out effluxing behind the pH regulator.Above-mentioned treatment process can make the Cr in the exhausted water
6+, Cr
3+, Ni
2+, Mn
4+, Fe
3+And F
-Qualified discharge, but its shortcoming is F
-Ion and Cr
3+, Ni
2+, Mn
4+, Fe
3+In Deng Qingchi, remove simultaneously, and employing milk of lime is neutralizing agent, the sludge quantity of its generation is very big like this, and in the mud thing, there are compositions such as chromium hydroxide, nickel hydroxide, manganous hydroxide, ironic hydroxide, Calcium Fluoride (Fluorspan), calcium sulfate simultaneously, this mud thing is the HW17 item Hazardous wastes of China national Hazardous wastes catalogue, and it does not possess comprehensive utilization value, and the processing costs height.
Summary of the invention
Technical problem to be solved by this invention is that the treatment process that a kind of processing costs is low, can effectively guarantee the stainless steel acid cleaning waste water and liquid that the waste liquid qualified discharge also can fully utilize the refuse work is provided at above-mentioned prior art present situation.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: the treatment process of this stainless steel acid cleaning waste water and liquid is characterized in that may further comprise the steps successively:
A, neutral salt waste water flow in the neutral wastewater equalization pond regulate water quality, the neutral exhausted water after will regulating is then put in the neutral reduction groove, regulates water quality in the acid waste water equalizing tank and the nitration mixture pickling waste waters flow into; Acid waste water liquid after will regulating is then put in the neutralizing well;
B, add reductive agent in the neutral reduction groove, by pH value and current potential ORP control, the span of control of pH value is 2.5-3 to the add-on of reductive agent respectively, and current potential ORP is 280-320mv; Hexavalent chromium is reduced into trivalent chromic ion, exhausted water after will reducing then put in the neutralizing well with regulate after nitration mixture pickling waste waters liquid phase mixed, in neutralizing well, add liquid caustic soda, make the pH value in the neutralization tank be adjusted to 9.0～9.5, and will mix liquid flow into the reaction settling pond in, make iron ion, trivalent chromic ion, nickel ion and mn ion generate Fe (OH) respectively
3, Cr (OH)
3, Ni (OH)
2And Mn (OH)
4The precipitation and from water, separate;
C, the clarification waste liquid after will separating are put in the fluoridation pond, add hydrochloric acid, lime and polymerize aluminum chloride in the fluoridation pond, the hydrochloric acid that adds is controlled at pH 8～9 scope, the dosage of polymerize aluminum chloride PAC is for handling 0.2～0.4% of the water yield, the calcium injected volume is more than 1.3 times of theoretical value, and will mix liquid and flow in the settling tank, make fluorion become CaF to symphysis with calcium ion
2The precipitation and remove;
D, the exhausted water that will remove fluorion flow in the final neutralizing well, are adding neutralizer in final neutralizing well, and the pH regulator that makes treatment solution is flowed through sand-bed filter and discharged to the neutral exhausted water.
As improvement, described reducing bath can divide 1# reducing bath and 2# reducing bath, and exhausted water flows in the 2# reducing bath from the 1# reducing bath; And described neutralizing well also can divide 1# neutralizing well and 2# neutralizing well, and exhausted water flows in the 2# neutralizing well from the 1# neutralizing well; Described settling tank can be designed to inclined-plate clarifying basin.
As further improvement, its precipitating sludge thing can concentrate in concentration basin in the described settling pond, then enriched material is done the resource recycling after plate-and-frame filter press carries out extrusion molding; And its CaF in the described settling tank
2The precipitating sludge thing also can concentrate in concentration basin, then enriched material is done the resource recycling after plate-and-frame filter press carries out extrusion molding.
Improve, described reductive agent may be selected to be hydrochloric acid and sodium bisulfite again, and described reductive agent can add by volume pump, and hydrochloric acid can be by the aperture and the on-off control dosage of control pneumavalve; Described liquid caustic soda can be preferably NaOH; Described neutralizer may be selected to be NaOH or HCl solution.
Compared with prior art, the invention has the advantages that its process using makes staging treating with metal ion and fluorion, and change neutralizing agent into liquid caustic soda by milk of lime, not only reached the requirement up to standard of discharging of waste liquid, but also greatly reduce the sludge quantity that is produced by the large quantities of lime breast, and in the heavy metal sewage sludge thing of settling pond, only contain chromium hydroxide, nickel hydroxide, manganous hydroxide, a huge sum of money such as ironic hydroxide compound, have and melt down again and as the comprehensive utilization value of stainless steel metallurgical raw material, and salt such as Calcium Fluoride (Fluorspan) and calcium sulfate are separated in the inclined-plate clarifying basin in fluoridation stage, thereby reduced the cost of handling effectively, and also reached the purpose of refuse reclamation.
Description of drawings
Fig. 1 is a liquid waste disposal schema of the present invention.
Embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
As shown in Figure 1, the treatment process of the stainless steel acid cleaning waste water and liquid of present embodiment may further comprise the steps successively:
A, neutral salt waste water flow in the neutral wastewater equalization pond regulate water quality, utilize the capacity of equalizing tank to carry out the modified and flow peak regulation of concentration of waste water, neutral exhausted water after will regulating is then put in the neutral reduction groove, regulates water quality in the acid waste water equalizing tank and the nitration mixture pickling waste waters flow into; Acid waste water liquid after will regulating is then put in the 1# neutralizing well;
B, add hydrochloric acid and sulfurous acid iron reductive agent in 1# neutral reduction groove, the add-on of reductive agent is controlled by pH value and current potential ORP respectively, and the span of control of pH value is 2.5-3, and current potential ORP is 280-320mv; Then exhausted water is continued to add reductive agent at the 2# reducing bath and do further reduction, hexavalent chromium is reduced into trivalent chromic ion, exhausted water after will reducing then put in the 1# neutralizing well with regulate after nitration mixture pickling waste waters liquid phase mixed, in the 1# neutralizing well, add the NaOH liquid caustic soda, make the pH value in the neutralization tank be adjusted to 9.0～9.5, then exhausted water is continued to add the NaOH liquid caustic soda at the 2# neutralizing well and do further neutralization, and will mix liquid flow into the reaction settling pond in, make iron ion, trivalent chromic ion, nickel ion and mn ion generate Fe (OH) respectively
3, Cr (OH)
3, Ni (OH)
2And Mn (OH)
4And the precipitation and from water, separate;
C, the clarification waste liquid after will separating are put in the fluoridation pond, add hydrochloric acid, lime and polymerize aluminum chloride in the fluoridation pond, the hydrochloric acid that adds is controlled at pH 8～9 scope, the dosage of polymerize aluminum chloride PAC is for handling 0.2～0.4% of the water yield, and will mix liquid and flow in the inclined-plate clarifying basin, make fluorion become CaF to symphysis with calcium ion
2The precipitation and remove;
D, the exhausted water that will remove fluorion flow in the final neutralizing well, are adding neutralizer in final neutralizing well, and the pH regulator that makes treatment solution is flowed through sand-bed filter and discharged to the neutral exhausted water.Its sedimentary heavy metal sewage sludge thing concentrates in concentration basin in the described settling pond, then enriched material is done the resource recycling after plate-and-frame filter press carries out extrusion molding, and in inclined-plate clarifying basin CaF
2Precipitation and CaSO
4Concentrate in concentration basin Deng the mud thing, then enriched material is done the resource recycling after plate-and-frame filter press carries out extrusion molding.
The main chemical reactions formula that the present invention relates to has:
2Cr
2O
7 2-+3HSO
3 -+19H
+→4Cr
3++3SO
4 2-+11H
2O
2Cr
3++3OH
-→2Cr(OH)
3↓
Ni
2++2OH
-→Ni(OH)
2↓
Mn
4++4OH
-→Mn(OH)
4↓
Fe
3++3OH
-→Fe(OH)
3↓
2F
-+Ca(OH)
2+2H
+→CaF
2↓+2H
2O
In the above-mentioned treatment process, taked the treatment process of waste water staging treating, mud branch matter, made sludge quantity reduce 67% than former technology, heavy metal sewage sludge wherein possesses again and melts down, and can be used as the comprehensive utilization of stainless steel smelting raw material.
Below be the removal technological test of heavy metal ion of the present invention:
Cr in the neutral salt waste water
6+Be reduced into Cr
3+After, mix with nitration mixture waste water, and handle heavy metal in the waste water with sheet alkali (sodium hydroxide) obtain solution replacing lime.
2.1 reaction controlled variable scope:
First step neutralization reaction groove second stage neutralization reaction groove
PH is 9.0-9.5 for 4.0-7.0 pH
2.2 raw wastewater water quality (before handling): the implication of SS is suspended solids (suspend solid)
Sequence number neutral salt waste water (mg/L) is produced steel grade
PH Ni
2+Total Fe SS Cr
6+Total No. 2 units of No. 1 unit of Cr
1 1.7 20 788 950 ＜0.001 80 SUS430 SUS430
2 3.4 40 917 12500 187 200 SUS430 SUS430
3 3.1 40 545 7220 182 207 SUS430 SUS430
4 2.7 25 225 852 109 133 SUS430 silicon steel
5 2.43 30 83 209 89 201 SUS430 SUS304
6 3.65 45 108 360 70 106 SUS430 SUS304
Mean value 33 444 3,682 127 155
Sequence number nitration mixture waste water (mg/L) is produced steel grade
PH Ni
2+Total Fe SS F
-No. 2 units of No. 1 unit
1 3.4 50 291 49600 1190 SUS430 SUS430
2 2.7 70 528 1080 180 SUS430 SUS430
3 1.5 20 162 3400 270 SUS430 SUS430
4 1.5 20 170 259 155 SUS430 silicon steel
5 1.4 60 185 305 100 SUS430 SUS304
6 1.45 30 149 30 220 SUS430 SUS304
Mean value 42 248 9,112 353
2.3 the implication of processed waste water index: SS is suspended solids (suspend solid)
The total Fe Cr of sequence number pH
6+Total Cr Ni
2+SS F
-
mg/L mg/L mg/L mg/L mg/L mg/L
1 11.3 0.735 0.003 0.092 0.11 16 60
2 11.1 0.975 0.015 0.026 0.03 9 30
3 8.7 2.084 0.010 0.145 0.31 12 110
4 8.7 0.784 0.006 0.048 0.02 11 115
5 8.8 1.610 0.025 0.029 0.06 21 41
6 8.7 0.737 0.009 0.065 0.03 16 13
7 8.7 0.604 0.023 0.058 0.02 15 16
8 8.8 0.820 0.003 0.047 0.03 13 28
9 8.8 1.598 0.021 0.052 0.04 11 25
10 8.9 1.153 0.022 0.059 0.05 16 18
11 9.1 1.414 0.034 0.060 0.10 23 27
12 9.4 0.896 0.018 0.057 0.04 6 41
13 9.1 1.011 0.033 0.069 0.04 42 27
14 9.1 1.145 0.052 0.071 0.04 16 22
15 9.4 1.198 0.004 0.066 0.12 20 22
16 9.4 2.007 0.016 0.079 0.07 33 43
179.4 2.355 0.016 0.056 0.09 - 55
Invented technology
Water outlet mean value
-- 1.243 0.018 0.063 0.07 18 41
Clearance 99.619%
99.986％
99.959％
99.816％
99.748％
Former technology effluent index
8.9 0.214 0.062 0.069 0.07 10 1.95
Emission standard 10 0.5 1.5 1.0 70 10
2.4 analyze:
From 17 times sampling analysis, it is all up to standard that all go out the heavy metal index of water monitoring, and well below the emission standard of regulation, can verify that under the quantity-produced situation reforming technology can guarantee water outlet heavy metal index stably reaching standard.
3, fluoride ion removing technological test:
3.1 medicament is prepared:
PAC (polyfluorine ion) is mixed with the solution of 1% concentration, and lime is mixed with the milk of lime of 2% concentration.
3.2 process of the test:
Because of field apparatus does not possess on-the-spot commerical test condition, built 1m
3The pilot plant of/h processing power carries out the fluoride ion removing technological test.
3.3 reaction parameter: pH scope 8～9, calcium source dosage are 1.3 times of theoretical value.
3.4 testing data:
pH F
-(mg/L) SO4
2-(mg/L)
1# fluorine reactive tank
Former water 10.97 1,780 8000
Sampling 18.17----
Take a sample 27.50 7.4--
2# fluorine reactive tank
Former water 11.05 1,990 8000
Sampling 18.10----
Take a sample 27.40 7.2--
3# fluorine reactive tank
Former water 11.17 1,780 9000
Take a sample 17.98 9.8--
Take a sample 27.48 7.8--
Emission standard: 10
*Sludge settling ratio is taken from the sedimentation of reactive tank mixed solution and was recorded in 30 minutes.
3.4 data analysis:
The dosage of calcium salt should be 1.3 times of theoretical amount can guarantee that the fluorion in the waste water reaches emission standard.But the reaction conditions of considering pilot scale is better, and in actual engineering, the dosage of calcium salt should be more than 1.5 times of theoretical amount, and concrete higher limit can be determined according to the practical situation of each factory, also should be taken into account the interference of sulfate radical simultaneously.
4, mud analysis:
4.1 sludge quantity analysis
4.1.1 adopt original technology to produce sludge quantity
Use the waste water processing station average treatment water yield of original place science and engineering skill to be 70m
3/ h, it is 1000 tons that monthly average produces mud; Handling the water yield at full capacity according to design is 100m
3/ h, monthly output raw sludge amount will reach 1429 tons, amount to and produce 17143 tons of raw sludges (water ratio is 50%) per year.
4.1.2 transform sludge quantity and contrast that the back produces:
To transform the sludge quantity that the back produces in order estimating,, to determine in order to the influent quality of estimation sludge quantity as follows according to the influent quality that this experiment records:
| The waste water index (mg/L) of on average intaking | pH | Ni 2+ | Fe 3+ | Total Cr | F - | SS |
| Neutral salt waste water | 1.8 | 35 | 450 | 130 | - | 300 |
| Nitration mixture waste water | 2.2 | 45 | 250 | - | 1500 | 250 |
Below be to transform to implement the guide look that the back sludge quantity changes:
* handle water yield neutral salt waste water 40m
3/ h, nitration mixture waste water 60m
3/ h, year working time 8000h.
* based on this experimental data, sludge yield can be relevant with influent quality.
* moisture percentage in sewage sludge is 50%.
4.2 sludge components:
To the heavy metal sewage sludge sample examination obtained after the test:
Siderochrome nickel manganese F
Heavy metal sewage sludge 41.04% 8.10% 5.65% 0.7% 0
Judge and possess the condition of melting down again.
Claims (10)
1. the treatment process of a stainless steel acid cleaning waste water and liquid is characterized in that may further comprise the steps successively:
A, neutral salt waste water flow in the neutral wastewater equalization pond regulate water quality, the neutral exhausted water after will regulating is then put in the neutral reduction groove, regulates water quality in the acid waste water equalizing tank and the nitration mixture pickling waste waters flow into; Acid waste water liquid after will regulating is then put in the neutralizing well;
B, add reductive agent in the neutral reduction groove, by pH value and current potential ORP control, the span of control of pH value is 2.5-3 to the add-on of reductive agent respectively, and current potential ORP is 280-320mv; Hexavalent chromium is reduced into trivalent chromic ion, exhausted water after will reducing then put in the neutralizing well with regulate after nitration mixture pickling waste waters liquid phase mixed, in neutralizing well, add liquid caustic soda, make the pH value in the neutralization tank be adjusted to 9.0～9.5, and will mix liquid flow into the reaction settling pond in, make iron ion, trivalent chromic ion, nickel ion and mn ion generate Fe (OH) respectively
3, Cr (OH)
3, Ni (OH)
2And Mn (OH)
4The precipitation and from water, separate;
C, the clarification waste liquid after will separating are put in the fluoridation pond, add hydrochloric acid, lime and polymerize aluminum chloride in the fluoridation pond, the hydrochloric acid that adds is controlled at pH 8～9 scope, the dosage of polymerize aluminum chloride PAC is for handling 0.2～0.4% of the water yield, the calcium injected volume is more than 1.3 times of theoretical value, and will mix liquid and flow in the settling tank, make fluorion become CaF to symphysis with calcium ion
2The precipitation and remove;
D, the exhausted water that will remove fluorion flow in the final neutralizing well, are adding neutralizer in final neutralizing well, and the pH regulator that makes treatment solution is flowed through sand-bed filter and discharged to the neutral exhausted water.
2. according to the treatment process of the described stainless steel acid cleaning waste water and liquid of claim 1, it is characterized in that described reducing bath divides 1# reducing bath and 2# reducing bath, exhausted water flows in the 2# reducing bath from the 1# reducing bath.
3. according to the treatment process of the described stainless steel acid cleaning waste water and liquid of claim 1, it is characterized in that described neutralizing well divides 1# neutralizing well and 2# neutralizing well, exhausted water flows in the 2# neutralizing well from the 1# neutralizing well.
4. according to the treatment process of the described stainless steel acid cleaning waste water and liquid of claim 1, it is characterized in that described settling tank is an inclined-plate clarifying basin.
5. according to the treatment process of claim 1 or 2 or 3 or 4 described stainless steel acid cleaning waste water and liquids, it is characterized in that its precipitating sludge thing concentrates in the described settling pond in concentration basin, then enriched material is done the resource recycling after plate-and-frame filter press carries out extrusion molding.
6. according to the treatment process of claim 1 or 2 or 3 or 4 described stainless steel acid cleaning waste water and liquids, it is characterized in that its CaF in the described settling tank
2The precipitating sludge thing concentrates in concentration basin, then enriched material is done the resource recycling after plate-and-frame filter press carries out extrusion molding.
7. according to the treatment process of claim 1 or 2 or 3 or 4 described stainless steel acid cleaning waste water and liquids, it is characterized in that described reductive agent is hydrochloric acid and sodium bisulfite.
8. according to the treatment process of the described stainless steel acid cleaning waste water and liquid of claim 7, it is characterized in that described reductive agent adds by volume pump, hydrochloric acid is by the aperture and the on-off control dosage of control pneumavalve.
9. according to the treatment process of claim 1 or 2 or 3 or 4 described stainless steel acid cleaning waste water and liquids, it is characterized in that described liquid caustic soda is NaOH.
10. according to the treatment process of claim 1 or 2 or 3 or 4 described stainless steel acid cleaning waste water and liquids, it is characterized in that described neutralizer is NaOH or HCl solution.
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