CN106746391A - A kind of phosphatization recycling sludge method of disposal - Google Patents
A kind of phosphatization recycling sludge method of disposal Download PDFInfo
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- CN106746391A CN106746391A CN201611033293.9A CN201611033293A CN106746391A CN 106746391 A CN106746391 A CN 106746391A CN 201611033293 A CN201611033293 A CN 201611033293A CN 106746391 A CN106746391 A CN 106746391A
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- phosphatization
- filtrate
- recycling
- sludge
- disposal
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/265—General methods for obtaining phosphates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/14—Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention discloses a kind of phosphatization recycling sludge method of disposal, belong to field of solid waste resource utilization.The present invention limits phosphatization recycling sludge Utilizing question for phosphatization Heavy Metals in Sludge impurity, carried using acidleach+materializing strategy operation by the way of, realize the recycling of phosphatization sludge.The present invention carries out acidleach and carries using Waste Sulfuric Acid, cooperative disposal spent acid while recycling phosphatization sludge, greatly reduce the operation processing cost of technique, realize the new approaches of the treatment of wastes with processes of wastes against one another, the treatment disposal of discarded object is effectively combined with recycling, with good environmental benefit, economic benefit, it is suitable to promote the use of.
Description
Technical field
The invention belongs to environmental protection and resource regeneration field, and in particular to a kind of phosphatization recycling sludge method of disposal.
Background technology
Along with the high speed development of the industries such as automobile making, electronics processing, plating, metal surface phosphating handling process is extensive
It is applied.Phosphorating treatment is to form a kind of insoluble phosphate film in metal surface using phosphoric acid or phosphatic solution
Process, be technology that Treatment of Metal Surface is generally used.General parkerizing process includes alkali cleaning oil removing, acid pickling and rust removing, phosphorus
Change and Passivation Treatment, produce substantial amounts of pollutant in the process, such as oil emulsion, surfactant and phosphate, especially with phosphorus
The discharge capacity of hydrochlorate is larger, exceeded serious, and because the species of pollutant is various, suitable difficulty is brought to wastewater treatment.
Current waste water dephosphorization method mainly has the united application of bioanalysis, chemical method, physical-chemical process and these methods.Institute
It is all that the solid constituent that the phosphate anion in waste water changes into slightly solubility is precipitated the effect for reaching dephosphorization to have method.Change
Method and bioanalysis are the more extensive methods of application at present, wherein chemical method again so that its treatment effeciency is high, it is effect stability, simple
Easy the advantages of, is as most effective, the most common method for processing high-concentration phosphorus-containing wastewater.It is usually used in the slaine of chemical dephosphorization
There are three kinds：Calcium salt, molysite and aluminium salt.It is generally acknowledged that calcium phosphate precipitation is by PO4 3-With Ca2+、Fe3+Or Al3+Chemical precipitation
What effect settled down.Because molysite is higher with the relative cost of aluminium salt, source is extensive not as calcium salt, and high-density phosphorus are useless
Water water is smaller, generation precipitation stabilization, therefore at present more than high concentration phosphorized waste water using calcium-phosphorus precipitation method method dephosphorization.
However, calcium-phosphorus precipitation method also have the defect of its own, substantial amounts of sludge can be produced.Containing a large amount of in such sludge
Calcium phosphate, with great resource potentiality, but the heavy metal substance for wherein containing limits the recycling of phosphatization sludge,
Therefore rationally efficient phosphatization sludge process for separation and purification is urgently developed.
Chinese Patent Application No. 200410039017.4, the date of application discloses gold for the patent application document of 2005.8.3
The waste sludge absorption method of metal surface phosphorating treatment processing procedure, is made up of the connection of multiple unit process rooms, and phosphorus is prepared by chemical reaction
The technique of sour sodium, of the invention to have the disadvantage that reative cell is more, structure is complex, after long-play, in each reactive tank easily
There is deposition, the preparation efficiency of sodium phosphate is relatively low.Chinese Patent Application No. is 201210488837.6, and the date of application is
2012.11.27 a kind of patent application document extracts ferric phosphate method in disclosing waste residue from phosphatization.The method is by adding
Enriching hydrochloric acid, NaOH prepare ferric orthophosphate product through drying；The shortcoming of the invention is because heavy metal contains in phosphatization waste residue
Amount is relatively low, and the preparation rate of ferric orthophosphate is not enough, and so as to cause the method operating cost higher, operability is not strong.
Compared with above-mentioned patent, the present invention realizes the thinking of the treatment of wastes with processes of wastes against one another, effectively by the use of Waste Sulfuric Acid as Acid leaching agent
Cost of disposal is reduced, in technique of the invention, by the aggregation of phosphatization sludge step-by-step classifier, and resource profit is realized according to its feature
With so that Processes and apparatus is simple to operate, treatment effect is preferable, is worthy of popularization.
The content of the invention
For existing phosphorized waste water is difficult and the features such as processing cost higher, the invention provides a kind of new phosphide
The device and method of waste water cooperative disposal ammonia nitrogen waste water.By the way of cooperative disposal phosphorized waste water and ammonia nitrogen waste water, using certainly
The precipitating reagent of row configuration prepares high-efficiency sustained-release fertilizer guanite (MAP) under certain condition, realizes phosphorized waste water and ammonia nitrogen waste water
Recycling.
To realize above-mentioned technical purpose, the technical scheme that the present invention takes is：
A kind of phosphatization recycling sludge method of disposal, comprises the following steps：
Step one, in phosphatization sludge Waste Sulfuric Acid is added, Acid leaching reaction is carried out to phosphatization sludge using Waste Sulfuric Acid,
Step 2, the Acid leaching filter residue for producing step one are heavy by being made building material, filtrate feeding after washing, press filtration
In the reactor of shallow lake,
Step 3, precipitating reagent is added in precipitation reactor, is reclaimed by the heavy metal precipitation in filtrate, after press filtration,
Step 4, by step 3 precipitate after filtrate carry out ion exchange purification,
Step 5, the filtrate of purification is added white lime be sufficiently mixed after, be prepared into phosphate pigment.
It is optimization above-mentioned technical proposal, the concrete measure taken also includes：
Sulfur waste acid concentration is 5%~30% in step one, and the amount of phosphatization sludge and Waste Sulfuric Acid add ratio (mass ratio)
It is 1:3~20, stirring incorporation time is 1~3h.
Moisture content is down to 40% or so by Acid leaching filter residue after washing press filtration in step 2, and feeding cement plant prepares water
Mud building materials, the filtrate being press-filtered out carries out Acid leaching reaction again in being recycled to step one.
Precipitating reagent is by NaOH, EDTA and FeSO4Mix, and ratio (mol ratio) is NaOH：EDTA：FeSO4=(2~
6)：(1~3)：(0.5~1), the dosage (mass ratio) of precipitating reagent is the 0.3%~1.5% of filtrate, and the stirring reaction time is
0.5~2h.
The heavy metal that precipitating reagent is isolated includes Cd, Pb, Cu and Zn.
It is by strong basic type anion-exchange resin, highly basic by the filtrate after precipitation that step 4 intermediate ion exchanges purification step
Type anion exchange resin by the anion exchange in filtrate out, to strong basic type anion-exchange resin successively through 1mol/L's
HCl and NaOH is eluted, and elution rate is 1.2~1.8 volume posts/hour, and heavy metal, eluent feeding mixing are free of in eluent
Waited in reactor and mixed with white lime.
Mix with eluent during white lime is put into mixing reactor, the dosage (mass ratio) of white lime is eluent
5%~20%, 1~3h of reaction time, reaction pH is 5~9, ultimately forms phosphate pigment.
Compared to prior art, beneficial effects of the present invention are：
(1) present invention realizes the recycling of phosphatization sludge using the technique of Acid leaching+ion exchange, with other method
Compare, the technology has treatment effeciency higher, and energy consumption, processing cost are relatively low；
(2) present invention compared with the prior art, is realized using Waste Sulfuric Acid as leaching agent while phosphatization sludge is leached
The recycling of spent acid, has reached the purpose of the treatment of wastes with processes of wastes against one another.
(3) phosphatization sludge is prepared into industrial by-products phosphate pigment by the present invention, realizes the resource of phosphatization sludge
Utilize, suitably promote the use of.
Brief description of the drawings
Fig. 1 is process flow diagram of the invention.
Specific embodiment
Embodiments of the invention are described in further detail below in conjunction with accompanying drawing.
A kind of phosphatization recycling sludge method of disposal of the invention, comprises the following steps：
Step one, in phosphatization sludge Waste Sulfuric Acid is added, Acid leaching reaction is carried out to phosphatization sludge using Waste Sulfuric Acid,
Step 2, the Acid leaching filter residue for producing step one are heavy by being made building material, filtrate feeding after washing, press filtration
In the reactor of shallow lake,
Step 3, precipitating reagent is added in precipitation reactor, is reclaimed by the heavy metal precipitation in filtrate, after press filtration,
Step 4, by step 3 precipitate after filtrate carry out ion exchange purification,
Step 5, the filtrate of purification is added white lime be sufficiently mixed after, be prepared into phosphate pigment.
Sulfur waste acid concentration is 5%~30% in step one, and the amount of phosphatization sludge and Waste Sulfuric Acid add ratio (mass ratio)
It is 1:3~20, stirring incorporation time is 1~3h.
Moisture content is down to 40% or so by Acid leaching filter residue after washing press filtration in step 2, and feeding cement plant prepares water
Mud building materials, the filtrate being press-filtered out carries out Acid leaching reaction again in being recycled to step one.
Precipitating reagent is by NaOH, EDTA and FeSO4Mix, and ratio (mol ratio) is NaOH：EDTA：FeSO4=(2~
6)：(1~3)：(0.5~1), the dosage (mass ratio) of precipitating reagent is the 0.3%~1.5% of filtrate, and the stirring reaction time is
0.5~2h.
The heavy metal that precipitating reagent is isolated includes Cd, Pb, Cu and Zn.
It is by strong basic type anion-exchange resin, highly basic by the filtrate after precipitation that step 4 intermediate ion exchanges purification step
Type anion exchange resin by the anion exchange in filtrate out, to strong basic type anion-exchange resin successively through 1mol/L's
HCl and NaOH is eluted, and elution rate is 1.2~1.8 volume posts/hour, and heavy metal, eluent feeding mixing are free of in eluent
Waited in reactor and mixed with white lime.
Mix with eluent during white lime is put into mixing reactor, the dosage (mass ratio) of white lime is eluent
5%~20%, 1~3h of reaction time, reaction pH is 5~9, ultimately forms phosphate pigment.
Illustrated with specific embodiment below：
Embodiment 1
Using the phosphatization sludge of present invention treatment Jiangsu surface treatment enterprise generation, its service condition is：It is dense using acid
Spend the Waste Sulfuric Acid for 10%, the ratio (each embodiment is) that adds of phosphatization sludge and Waste Sulfuric Acid is 1：5, stirring incorporation time is
1h, cement plant cement will be delivered to after reaction after filter residue press filtration；Filtrate adds the precipitating reagent for voluntarily configuring, precipitating reagent allocation ratio
It is NaOH：EDTA：FeSO4=2：3：0.5, the dosage of precipitating reagent is the 0.3% of filtrate, and the reaction time is 1h；By the moon from
The resin of adsorption saturation is eluted after sub-exchange resin with the speed of 1.4 volume posts/hour, and added in eluent 10% it is ripe
Lime, reacts 1.5h, and reaction pH is 6, forms phosphate pigment.
Embodiment 2
Using the phosphatization sludge of present invention treatment Anhui chemical enterprise, its service condition is：It is 5% to use acid concentration
The ratio that adds of Waste Sulfuric Acid, phosphatization sludge and Waste Sulfuric Acid is 1：15, stirring incorporation time is 2h, will be sent after filter residue press filtration after reaction
To cement plant cement；Filtrate adds the precipitating reagent for voluntarily configuring, and precipitating reagent allocation ratio is NaOH：EDTA：FeSO4=6：1：
1, the dosage of precipitating reagent is the 1.2% of filtrate, and the reaction time is 1.5h；By after anion exchange resin with 1.8 volume posts/
The speed of hour elutes the resin of adsorption saturation, and 15% white lime is added in eluent, reacts 2h, and reaction pH is 7, shape
Into phosphate pigment.
Embodiment 3
Using the phosphatization sludge of present invention treatment Anhui enterprises of producing stainless steel, its service condition is：Using acid concentration
It is 20% Waste Sulfuric Acid, the ratio that adds of phosphatization sludge and Waste Sulfuric Acid is 1：3, stirring incorporation time is 1.5h, will filter after reaction
Cement plant cement is delivered to after slag press filtration；Filtrate adds the precipitating reagent for voluntarily configuring, and precipitating reagent allocation ratio is NaOH：EDTA：
FeSO4=3：2：0.8, the dosage of precipitating reagent is the 1.5% of filtrate, and the reaction time is 0.5h；By anion exchange resin
The resin of adsorption saturation is eluted with the speed of 1.2 volume posts/hour afterwards, and 20% white lime is added in eluent, reaction
2.5h, reaction pH is 8, forms phosphate pigment.
The above is only the preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-described embodiment,
All technical schemes belonged under thinking of the present invention belong to protection scope of the present invention.It should be pointed out that for the art
For those of ordinary skill, some improvements and modifications without departing from the principles of the present invention should be regarded as protection of the invention
Scope.
Claims (7)
1. a kind of phosphatization recycling sludge method of disposal, it is characterized in that：Comprise the following steps：
Step one, in phosphatization sludge Waste Sulfuric Acid is added, Acid leaching reaction is carried out to phosphatization sludge using Waste Sulfuric Acid,
Step 2, the Acid leaching filter residue for producing step one are anti-by being made building material, filtrate feeding precipitation after washing, press filtration
In answering device,
Step 3, precipitating reagent is added in precipitation reactor, is reclaimed by the heavy metal precipitation in filtrate, after press filtration,
Step 4, by step 3 precipitate after filtrate carry out ion exchange purification,
Step 5, the filtrate of purification is added white lime be sufficiently mixed after, be prepared into phosphate pigment.
2. a kind of phosphatization recycling sludge method of disposal according to claim 1, it is characterized in that：It is useless described in step one
Sulfuric acid concentration is 5%~30%, and the amount of phosphatization sludge and the ratio (mass ratio) that adds of Waste Sulfuric Acid are 1:3~20, stirring mixing
Time is 1~3h.
3. a kind of phosphatization recycling sludge method of disposal according to claim 1, it is characterized in that：Acid leaching filter in step 2
Moisture content is down to 40% or so by slag after washing press filtration, and feeding cement plant prepares cement building material, and the filtrate being press-filtered out is recycled to
Acid leaching reaction is carried out in step one again.
4. a kind of phosphatization recycling sludge method of disposal according to claim 1, it is characterized in that：Described precipitating reagent by
NaOH, EDTA and FeSO4Mix, and ratio (mol ratio) is NaOH：EDTA：FeSO4=(2~6)：(1~3)：(0.5~
1), the dosage (mass ratio) of precipitating reagent is the 0.3%~1.5% of filtrate, and the stirring reaction time is 0.5~2h.
5. a kind of phosphatization recycling sludge method of disposal according to claim 4, it is characterized in that：Described precipitating reagent is separated
The heavy metal for going out includes Cd, Pb, Cu and Zn.
6. a kind of phosphatization recycling sludge method of disposal according to claim 1, it is characterized in that：Step 4 intermediate ion is exchanged
Purification step is that strong basic type anion-exchange resin is by filtrate by strong basic type anion-exchange resin by the filtrate after precipitation
Anion exchange out, strong basic type anion-exchange resin is eluted through the HCl and NaOH of 1mol/L successively, elution rate is
1.2~1.8 volume posts/hour, wait in eluent feeding mixing reactor and mixing with white lime.
7. a kind of phosphatization recycling sludge method of disposal according to claim 6, it is characterized in that：White lime is put into and is mixed
Mix with eluent in reactor, the dosage (mass ratio) of white lime is 5%~20%, 1~3h of reaction time of eluent,
Reaction pH is 5~9, ultimately forms phosphate pigment.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108249721A (en) * | 2018-03-20 | 2018-07-06 | 河北工业大学 | The minimizing technology of zinc in a kind of phosphatization solid hazardous waste |
| CN109437508A (en) * | 2018-12-17 | 2019-03-08 | 苏州比雷艾斯电子科技有限公司 | A kind of printing and dyeing sludge processing system removing heavy metal and water removal |
| CN110183020A (en) * | 2019-06-06 | 2019-08-30 | 福建兴万祥建设集团有限公司 | A kind of processing method for heavy metal wastewater thereby of digging up mine |
| CN110255845A (en) * | 2019-07-09 | 2019-09-20 | 中国科学院城市环境研究所 | A kind of resource utilization method of pyrolyzing sludge charcoal |
| CN111484214A (en) * | 2020-06-03 | 2020-08-04 | 华电水务科技股份有限公司 | Phosphorus recycling device and method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108249721A (en) * | 2018-03-20 | 2018-07-06 | 河北工业大学 | The minimizing technology of zinc in a kind of phosphatization solid hazardous waste |
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| CN109437508A (en) * | 2018-12-17 | 2019-03-08 | 苏州比雷艾斯电子科技有限公司 | A kind of printing and dyeing sludge processing system removing heavy metal and water removal |
| CN110183020A (en) * | 2019-06-06 | 2019-08-30 | 福建兴万祥建设集团有限公司 | A kind of processing method for heavy metal wastewater thereby of digging up mine |
| CN110183020B (en) * | 2019-06-06 | 2020-04-24 | 福建兴万祥建设集团有限公司 | Mining heavy metal wastewater treatment method |
| CN110255845A (en) * | 2019-07-09 | 2019-09-20 | 中国科学院城市环境研究所 | A kind of resource utilization method of pyrolyzing sludge charcoal |
| CN110255845B (en) * | 2019-07-09 | 2020-08-21 | 中国科学院城市环境研究所 | Resource utilization method of sludge pyrolytic biochar |
| CN111484214A (en) * | 2020-06-03 | 2020-08-04 | 华电水务科技股份有限公司 | Phosphorus recycling device and method |
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Application publication date: 20170531 |