CN101125689A - Method for preparing water treatment medicament by using sludge residue and water treatment medicament thereof - Google Patents
Method for preparing water treatment medicament by using sludge residue and water treatment medicament thereof Download PDFInfo
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- CN101125689A CN101125689A CNA200710069559XA CN200710069559A CN101125689A CN 101125689 A CN101125689 A CN 101125689A CN A200710069559X A CNA200710069559X A CN A200710069559XA CN 200710069559 A CN200710069559 A CN 200710069559A CN 101125689 A CN101125689 A CN 101125689A
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- treatment agent
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Abstract
The invention discloses a method to produce water treatment agentia with mud residue and a water treatment agentia, which takes mud residue, lixiviated acid and water as raw materials and comprises the steps of acid dipping, filter residue and conditioning. Rich inorganic mineral composition in mud residue is prepared into water treatment agentia with the process such as acid dipping, filter residue, conditioning, etc., and the water treatment agentia can be recycled, thus meeting the requirements of cyclic economical development, leading mud residue to be stable and reduced, preventing secondary pollution, deceasing agentia input amount with annual transportation cost of 2.3x105m3/d mud and sewage treatment cost and effectively improving the economical benefit of sewage treatment.
Description
Technical field
The present invention relates to a kind of utilize sludge residue to prepare the method for water treatment agent and adopt the preparation of this method and water treatment agent, belong to technical field of sewage.
Background technology
Mud is the sedimentable matter that sewage work produces in sewage treatment process, contain large quantity of moisture and organism, bacterium, also contain multiple metallic element, be mainly iron, silicon, calcium, sulphur, aluminium, phosphorus, magnesium etc., the method of disposal of mud mainly contains compost treatment at present, sanitary landfill, agricultural greening, Ocean dumping, technology such as burning disposal, along with the progress of science and technology with to the attention of environment, the recycling of mud is paid attention to, the burning of mud utilizes technology because can be rapidly and make mud reach minimizing largely, not only solve the problem of outlet of mud but also utilized fully the energy in the mud, therefore be able to extensive utilization.Organism has been removed in sludge incineration, and inorganics still exists with the form of burning ash, and the treating method of sludge residue mainly contains at present: 1, system light ceramic, to be used as roadbed material, aggregate or flowers covering material etc.; 2, system melting material is as roadbed material, aggregate or flowers covering material etc.; 3, system devitrified glass is made the building inside/outside decorative material and is used; 4, preparation ground changes.
To certain sludge residue analysis revealed, it consists of: ferric oxide (Fe
2O
3) content greater than 50%, dehydrated gyp-(CaSO
4) about 20%, trimagnesium phosphate (MgPO
4) less than 2%, feldspar (CaAl
2Si
2O
8) 5% with interior, sulphur ferrosilicon (Fe
2SiS
4) about 4%, quartzy (SiO
2) 5%, mullite (Al
4.59Si
1.41O
9.7) 1%, therefore, how inorganic mineral abundant in the burning ash especially ferro element can be recycled fully, and prevent the generation of secondary pollution, be new problem in the water technology.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing sludge residue to prepare water treatment agent, to realize the circulation of inorganic water treatment agent in sewage work, sludge residue obtains comprehensive utilization, sludge residue decrement and stabilization simultaneously.
For achieving the above object, the technical solution used in the present invention is, a kind of method of utilizing sludge residue to prepare water treatment agent, with sludge residue, leach acid, water is raw material, comprises acidleach～filter residue～conditioning, wherein:
1, acidleach: in reaction utensil, press 15～30molH
+/ kg ratio adds sludge residue, leaches acid and water, the stirring and refluxing reaction, and temperature of reaction is 80～150 ℃, and the reaction times is 1～5 hour, and liquid-solid ratio is controlled to be 2～5ml/g.
Described sludge residue is meant the mud that sewage work handles through biochemical treatment or materialization, and 650 ℃ of roasting temperatures are 4 hours in stoving oven, and after the cooling, pulverizing forms.
Described leaching acid is used as leaching agent and (is mainly iron with the metallic element that exists with solid form in the sludge incineration ash, contain small amount of aluminum, calcium, magnesium) effect, the form that metallic element is changed into soluble compound enters the aqueous solution, can select mineral acid or organic acid any one or any two kinds combination, preferred adopt at least a of hydrochloric acid in the mineral acid, sulfuric acid, nitric acid, be preferably the combination of hydrochloric acid and vitriolic especially.
Described reaction liquid-solid ratio is the ratio that adds acid and water cumulative volume and sludge residue quality in the reaction system, is preferably 2.0～3.7ml/g, is preferably 2.0～3.0 especially.
Temperature of reaction preferably is controlled at 110～120 ℃, is preferably 115～120 ℃ especially;
Reaction times is preferably 2～4 hours, is preferably 2.5～3 hours especially;
2, filter residue: after the reaction soln after the acidleach filtered, filtrate was water treatment agent finished product just prepare the dilution proportion of 10mL water treatment agent by the 1g sludge residue after.
Above-mentioned water treatment agent is finished product just, and composition is as shown in the table:
Table 1 water treatment agent performance analysis table look-up
| Sequence number | Analysis indexes | Content | Sequence number | | Content | |
| 1 2 3 4 5 6 7 8 9 10 11 12 13 | The total titanium mg/L of the total magnesium g/L of the total calcium g/L of the total aluminium g/L of the total iron g/L of density g/mL solid content % pH (1%) the pH total tin mg/L of the total copper mg/L of the total zinc mg/L of sodium g/L | 1.096 11.80 2.2 -0.11 28.504 1.624 1.705 1.709 2.39 341.9 0.06 8.16 149.9 | 14 15 16 17 18 19 20 21 22 23 24 25 | The total total manganese mg/L of the total chromium mg/L of the total cadmium mg/L of the total plumbous mg/L of nickel mg/ total mercury mg/L arsenic mg/L muriate g/L sulfate radical g/L total phosphorus g/L tropeolin-D acidity (CaCO 3, g/L) redox potential mv | 13.1 9.04＜4.0 43.1 193.2 do not detect 59.12 21.541 2.048 81.33-700 |
As can be seen from the above table, water treatment agent just finished product mainly is made up of metal ingredients such as iron, aluminium, calcium, magnesium on chemical constitution, they have accounted for about 90% of whole metallic cations, be topmost composition with iron again wherein, total iron content is substantially greater than 28g/L (content of amounting to into ferric oxide is 3.63%), account for about 75% of whole metallic cations, can in the pre-treatment of water inlet, use.
Constituent contents such as zinc, manganese, titanium are not high, only account for 1.8% of whole metallic cations, can play booster action, and trace elements such as nickel, manganese, zinc are that microorganism physiology is necessary.Constituent contents such as harmful element nickel, lead, cadmium, chromium are very low, only account for 0.18% of whole metallic cations, are the 2.5mL/L meter according to adding dose, and what the water outlet harmful element increased after the pre-treatment so at utmost is: total nickel 32.75mg/m
3, total plumbous 22.6mg/m
3, total cadmium 10mg/m
3, total chromium 107.75mg/m
3, harmful heavy metal sees Table 2 to the maximum permissible concentration of sewage biochemical treatment.
Table 2 heavy metal poison maximum permissible concentration
| Title | Concentration (mg/L) | Title | Concentration (mg/L) |
| Cadmium (cd 2+) chromium (cr 6+) | 0.1 0.5 | Nickel (Ni 2+) plumbous (Pb 2+) | 2.0 1.0 |
Analyze as can be known from table 2, the content of poisonous metal element all is significantly less than the desired scope of document, shows that such ionic concn can not cause adverse influence to biochemical treatment.
Solid content consist of 11.80%, i.e. 129g/L, this can play good booster action in preprocessing process.
3, conditioning: the medicament that makes in step 2 just adds an amount of solid solubility ferrous salt in the finished product, mixes, get final product finished product.
Because iron can not be dissolved fully in the acid leaching process, therefore only depend on the water treatment agent reuse of sludge residue preparation still can not satisfy the production needs, in actual procedure, can suitably replenish certain raw material, promptly the solubility ferrous salt preferably adopts FeSO
4.7H
2O, add-on is every 1m
3Add 60～80kg in the medicament.
Benefit of the present invention is: 1 social benefit: refuse is fully utilized, by will be in the sludge residue abundant inorganic mineral be prepared in addition recycle of water treatment agent, meet the requirement of recycling economy development, have certain exemplary role; Residue obtains stable and minimizing, has prevented secondary pollution; 2, economic benefit: after adopting the present invention, reduced the medicament input amount, can save medicament expense every year with 2400～2,500 ten thousand yuan, sludge residue obtains decrement and stabilization, and can reduce 2.3 * 10 every year
5m
3The transportation cost of/d mud, cost of sewage disposal reduces, and has improved the economic benefit of sewage disposal effectively.
Description of drawings
The graphic representation of Fig. 1 for concerning between iron solubility rate of the present invention and the sour add-on;
Fig. 2 is the graphic representation that iron solubility rate of the present invention and acid-leaching reaction concerned between the time;
The graphic representation of Fig. 3 for concerning between iron solubility rate of the present invention and the acid-leaching reaction temperature;
The graphic representation of Fig. 4 for concerning between iron solubility rate of the present invention and the acid-leaching reaction liquid-solid ratio;
Fig. 5 removes the situation comparison diagram for the two kinds of medicaments and the existing medicament that adopt the present invention's preparation to the integrated printing and dyeing waste water COD;
Fig. 6 for two kinds of medicaments adopting the present invention's preparation and existing medicament to integrated printing and dyeing wastewater treatment pH value variation diagram;
Fig. 7 is two kinds of medicaments adopting the present invention's preparation and the existing medicament BOD to the integrated printing and dyeing wastewater treatment
5/ CODcr comparison diagram;
Fig. 8 is two kinds of medicaments adopting the present invention's preparation and the existing medicament percent of decolourization comparison diagram to the integrated printing and dyeing wastewater treatment.
Embodiment
Implement 1: the control of acid selection and consumption
1.1 in reaction utensil, add the vitriol oil of 1000g sludge residue, 18mol/L in the ratio of 0.6～1.6ml/g, and an amount of water, the stirring and refluxing reaction, temperature of reaction is 120 ℃, reaction times is 2.5 hours, liquid-solid ratio is controlled to be 4.0ml/g, and after the solution after the acidleach was filtered, filtrate was water treatment agent finished product just prepare the dilution proportion of 10mL water treatment agent by the 1g sludge residue after.
1.2 the preparation method is with implementing 1.1, different is that minimizing vitriol oil add-on is 0.4ml/g, adds the concentrated hydrochloric acid of 12mol/L again in 0.6～1.2ml/g ratio.
1.3 the preparation method is with implementing 1.1, different is that minimizing vitriol oil add-on is 0.2ml/g, adds the concentrated hydrochloric acid of 12mol/L again in 1.2～1.6ml/g ratio.
To the add-on relation of the solubility rate of implementing iron in 1 and acid analyze Fig. 1, analyze relevant data: the increase that 1, acid amount adds can make the solubility rate of residue improve; 2, be example with single situation with the vitriol oil, add-on solubility rate increasing degree of iron behind the 1.1mL/g diminishes, but test finds that the mixing acidity of medicament but promotes very soon in test, and total medicament acidity is higher, so the acidity of acid is had certain requirement; 3, the add-on of concentrated hydrochloric acid is 1.9991mL/g in test, and the solubility rate of iron is 81.15%; And the solubility rate of iron is 51.54% when adding the vitriol oil (0.6664mL/g) be equivalent to the same acids amount, on data, can see that use hydrochloric acid is more much better than vitriolic effect, but the volatility of hydrochloric acid is stronger under higher temperature, therefore consider to use sulfuric acid and mixed in hydrochloric acid acid, based on hydrochloric acid; 4, as shown in Figure 1, adopt the nitration mixture of sulfuric acid 0.2mL/g+ hydrochloric acid 1.5mL/g to be combined as the best.
Implement 2: reaction times and temperature of reaction control
2.1 in reaction utensil, add the 1000g sludge residue, press nitration mixture combination a certain amount of acid of adding and the water of vitriol oil 0.2mL/g+ concentrated hydrochloric acid 1.5mL/g, liquid-solid ratio is controlled to be 4.0ml/g, control certain reaction temperature is 100～150 ℃, reaction times is 1～5 hour, stirring and refluxing reaction, after the solution after the acidleach filtered with filter cloth, filtrate was water treatment agent finished product just prepare the dilution proportion of 10mL water treatment agent by the 1g sludge residue after.
The reaction times of control is respectively 1 hour, 2 hours, 3 hours, 5 hours.
The temperature of reaction of control is respectively 100 ℃, 115 ℃, 130 ℃, 150 ℃.
To the relation of the solubility rate of implementing iron in 2 and reaction times and temperature analyze Fig. 2 and Fig. 3.
As can be seen from Figure 2, under identical temperature, the solubility rate of iron prolongs with the reaction times and increases, comprehensive yied and economy, and the reaction times is controlled at 2.0～2.5 hours for best.
As can be seen from Figure 3: when temperature of reaction during less than 130 ℃, the solubility rate of iron raises with the rising of temperature of reaction in the identical time, and this shows that the rising of system temperature makes reaction activity descend, thereby has accelerated the stripping of iron in the residue; After temperature surpassed 130 ℃, the solubility rate of iron descended to some extent with the rising of temperature on the contrary, and this may be the volatilization that too high temperature has caused system hydrochloric acid, thereby made the iron solubility rate descend.Therefore for this system, preferable temperature of reaction should be controlled between 110 ℃ to 120 ℃, preferably is controlled at 115 ℃ to 120 ℃ scopes, and this moment, the solubility rate of iron reached maximum.
Implement 3: the control of liquid-solid ratio
3.1 in reaction utensil, add the 1000g sludge residue, press nitration mixture combination a certain amount of acid of adding and the water of vitriol oil 0.2mL/g+ concentrated hydrochloric acid 1.5mL/g, 120 ℃ of control reaction temperature, reaction times is 2.5 hours, liquid-solid ratio is controlled to be 2～6ml/g, the stirring and refluxing reaction, after solution after the acidleach filtered with filter cloth, filtrate was water treatment agent finished product just prepare the dilution proportion of 10mL water treatment agent by the 1g sludge residue after.
3.2 implementation method is with 3.1, different is the nitration mixture portfolio ratio, and the nitration mixture combination of pressing vitriol oil 0.15mL/g+ concentrated hydrochloric acid 1.5mL/g adds a certain amount of acid and water.
3.3 implementation method is with 3.1, different is the nitration mixture portfolio ratio, and the nitration mixture combination of pressing vitriol oil 0.10mL/g+ concentrated hydrochloric acid 1.5mL/g adds a certain amount of acid and water.
The enforcement of these steps is in order rationally to control the acidity for preparing.To the relation of the solubility rate of implementing iron in 3 and reaction liquid-solid ratio analyze Fig. 4, as can be seen from Figure 4: when the vitriol oil is 0.2mL/g, liquid-solid ratio be controlled at 3.7 with interior be proper, this moment, hydrogen ion concentration should be controlled at more than the 6.8moL/L; When the vitriol oil is 0.15mL/g, liquid-solid ratio be controlled at 3.3 with interior be proper, this moment hydrogen ion concentration should be controlled at more than the 7.1moL/L; When the vitriol oil is 0.1mL/g, liquid-solid ratio be controlled at 3.0 with interior be proper, this moment hydrogen ion concentration should be controlled at more than the 7.2moL/L.Acid-leaching reaction system hydrogen ion concentration is controlled at more than the 7moL/L in sum, should be controlled at 21-25moLH with sour amount
+/ kg residue, the size as benchmark adjustment control liquid-solid ratio is generally more than 2.0, and reduces as far as possible with the acid amount, and acid that is to say that based on hydrochloric acid chlorine ion concentration is controlled at about the 18moL/kg residue.
The water treatment agent that the foregoing description preparation is got just product marking is Shaoxing Y189, and the first finished product of above-mentioned water treatment agent is pressed every 1m
3Add 75kg FeSO in the medicament
4.7H
2O makes water treatment agent and is labeled as Shaoxing modified form Y189, original water treatment agent on the market is labeled as Zhejiang University's medicament, advancing factory's integrated printing and dyeing sewage with Shaoxing sewage work is process object, aspect the wastewater treatment efficiency evaluation, established corresponding change of water quality evaluation analysis index and mainly comprised CODcr, PH, BOD
5/ CODcr and percent of decolourization, with reference to shown in Figure 5, Zhejiang University's medicament generally can reach about 36% the maximum material removal rate of water inlet CODcr, and modified form Y189 medicament maximum material removal rate generally can reach 34%, and common Y189 medicament generally can reach 31%.By above result as can be seen, in removal to water inlet CODcr, the acid solution of incineration residue can reach the treatment effect of Zhejiang University's medicament (on-the-spot operation) substantially, Y189 medicament to modified form is all the more so, with reference to shown in Figure 6, in correlated three kinds of medicaments, in suitable adding under the dose condition, modified form Y189 medicament is the most obvious to the reduction of water inlet pH value.For example, when the dose that adds of Zhejiang University's medicament is 1.1～1.2mL/L, water inlet pH can drop to about 10.10; During the adding dose and be 3mL/L of Y189, the pH value can drop to 9.84, and the Y189 of modified form (adding dose is 2.5mL/L) can drop to about 9.8, and hence one can see that, and Y189 type medicament is aspect the pH value of regulating sewage, and its performance is better than Zhejiang University medicament.With reference to shown in Figure 7, from this figure as seen, the same with the Zhejiang University pre-treatment medicaments, Y189 type medicament also can promote the BOD of water inlet
5/ CODcr value, when Zhejiang University's medicament add-on is 1.1～1.2mL/L, the BOD of sewage
5/ CODcr is by rising to 0.306 0.274 of pre-treatment early stage; And the Y189 medicament adds dose when being 3mL/L, BOD
5X/CODcr can rise to 0.285, and it is that 2.5mL/L can rise to about 0.30 that the Y189 medicament of modified form adds dose.With reference to shown in Figure 8, when the adding dose and be 1.1～1.2mL/L of Zhejiang University's medicament, percent of decolourization can reach 30%～37%; In the lab scale of laboratory, when Y189 added dose and is 3mL/L, percent of decolourization was about 17%, and the Y189 improved medicine adds dose when 2.5mL/L, and percent of decolourization is about 18%.
Claims (10)
1. method of utilizing sludge residue to prepare water treatment agent is characterized in that: with sludge residue, leach acid, water is raw material, comprises acidleach～filter residue, wherein:
1., acidleach: in reaction utensil, press 15～30molH
+/ kg ratio adds sludge residue, leaches acid and water, the stirring and refluxing reaction, and temperature of reaction is 80～150 ℃, and the reaction times is 1～5 hour, and liquid-solid ratio is controlled to be 2～5ml/g;
2., filter residue: after the reaction soln after the acidleach filtered, filtrate was water treatment agent finished product just prepare the dilution proportion of 10mL water treatment agent by the 1g sludge residue after.
2. a kind of method of utilizing sludge residue to prepare water treatment agent according to claim 1, it is characterized in that: described sludge residue is meant the mud of sewage work through biochemical treatment or materialization processing, 650 ℃ of roasting temperatures are 4 hours in stoving oven, after the cooling, pulverize and get.
3. a kind of method of utilizing sludge residue to prepare water treatment agent according to claim 1 is characterized in that: describedly leach that acid is preferred adopts at least a of hydrochloric acid in the mineral acid, sulfuric acid, nitric acid.
4. a kind of method of utilizing sludge residue to prepare water treatment agent according to claim 3 is characterized in that: described leaching acid is hydrochloric acid and vitriolic combination.
5. a kind of method of utilizing sludge residue to prepare water treatment agent according to claim 1 is characterized in that: described reaction liquid-solid ratio is 2.0～3.7ml/g.
6. a kind of method of utilizing sludge residue to prepare water treatment agent according to claim 5 is characterized in that: described reaction liquid-solid ratio is 2.0～3.0.
7. a kind of method of utilizing sludge residue to prepare water treatment agent according to claim 1 is characterized in that: described temperature of reaction is 110～120 ℃.
8. a kind of method of utilizing sludge residue to prepare water treatment agent according to claim 1 is characterized in that: the described reaction times is 2～4 hours.
9. a kind of method of utilizing sludge residue to prepare water treatment agent according to claim 1, it is characterized in that: also include conditioning technology, conditioning technology is included in the medicament that step makes in 2. and just adds an amount of solid solubility ferrous salt in the finished product, mixes, get final product finished product.
10. a kind of method of utilizing sludge residue to prepare water treatment agent according to claim 9 is characterized in that: described solid solubility ferrous salt is FeSO
4.7H
2O, add-on is every 1m
3Add 60～80kg in the medicament.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200710069559XA CN100551835C (en) | 2007-07-13 | 2007-07-13 | Utilize sludge residue to prepare the method for water treatment agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200710069559XA CN100551835C (en) | 2007-07-13 | 2007-07-13 | Utilize sludge residue to prepare the method for water treatment agent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101125689A true CN101125689A (en) | 2008-02-20 |
| CN100551835C CN100551835C (en) | 2009-10-21 |
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ID=39093844
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112094004A (en) * | 2020-09-07 | 2020-12-18 | 天津壹新环保工程有限公司 | Novel sludge pyrohydrolysis treatment system and method capable of recycling carbon source |
| CN113213564A (en) * | 2021-05-17 | 2021-08-06 | 深圳市金海威景观设计工程有限公司 | Method for preparing water treatment medicament by using sludge residues |
| CN113248095A (en) * | 2021-05-28 | 2021-08-13 | 山东利废厚生环保科技有限公司 | Ferric salt sludge treatment process and treatment system |
| CN115849539A (en) * | 2023-01-09 | 2023-03-28 | 长沙华时捷环保科技发展股份有限公司 | Fluorine removal agent and preparation method and application thereof |
-
2007
- 2007-07-13 CN CNB200710069559XA patent/CN100551835C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112094004A (en) * | 2020-09-07 | 2020-12-18 | 天津壹新环保工程有限公司 | Novel sludge pyrohydrolysis treatment system and method capable of recycling carbon source |
| CN113213564A (en) * | 2021-05-17 | 2021-08-06 | 深圳市金海威景观设计工程有限公司 | Method for preparing water treatment medicament by using sludge residues |
| CN113248095A (en) * | 2021-05-28 | 2021-08-13 | 山东利废厚生环保科技有限公司 | Ferric salt sludge treatment process and treatment system |
| CN115849539A (en) * | 2023-01-09 | 2023-03-28 | 长沙华时捷环保科技发展股份有限公司 | Fluorine removal agent and preparation method and application thereof |
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|---|---|
| CN100551835C (en) | 2009-10-21 |
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Granted publication date: 20091021 Termination date: 20130713 |