CN102503060B - Method for recovering ferric phosphate from sludge - Google Patents
Method for recovering ferric phosphate from sludge Download PDFInfo
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- CN102503060B CN102503060B CN 201110375682 CN201110375682A CN102503060B CN 102503060 B CN102503060 B CN 102503060B CN 201110375682 CN201110375682 CN 201110375682 CN 201110375682 A CN201110375682 A CN 201110375682A CN 102503060 B CN102503060 B CN 102503060B
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- iron phosphate
- mother liquor
- tertiary iron
- solid residue
- hydrochloric acid
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Abstract
The invention discloses a method for recovering ferric phosphate from sludge. The method comprises the following steps of: firstly, carrying out cracking pretreatment and centrifugal separation on the sludge to obtain solid residue; secondly, dissolving the solid residue in hydrochloric acid; centrifugally separating and taking supernate as a first ferric phosphate separation mother solution; meanwhile, dissolving the fired solid residue in the hydrochloric acid; centrifugally separating and taking supernate as a second ferric phosphate separation mother solution; preparing a PO4<3-> and Fe<3+> supersaturated solution from FeCl3 and H3PO4 to serve as a preparation mother solution; adding a FeCl3 solution into the first ferric phosphate separation mother solution and the second ferric phosphate separation mother solution; adjusting the pH values of the first ferric phosphate separation mother solution and the second ferric phosphate separation mother solution treated in the third step and the pH value of the preparation mother solution prepared in the second step to be higher with an NaOH solution; when the pH values are adjusted to be 2.5-4.5, centrifugally separating three kinds of solutions in which yellowish brown precipitations respectively generate, rinsing and drying to obtain a solid precipitation; and finally, analyzing to determine ferric phosphate as a product. According to the method disclosed by the invention, phosphorus elements in the sludge can be recovered.
Description
Technical field
The invention belongs to the Sludge Disposal Techniques field, be specifically related to a kind of tertiary iron phosphate method that in mud, reclaims.
Background technology
Huge sludge yield has become serious problems that affect the normal operation in China municipal sewage plant.On the other hand, mud is the unique product in the sewage treatment process, and the materials such as most organism, nutritive element all are converted, are concentrated in the mud in the sewage, so that the resource recycling of mud value potentiality are very large.China's mud content organic and nutritive element is all very high, and particularly the content of nitrogen, phosphorus, three kinds of nutritive elements of potassium all is higher than the content of U.S.'s sludge of sewage treatment plant, and nitrogen and phosphorus concentration are higher than the mean value of China's hog manure especially far away.
The mineral total amount of the nutritive elements such as the nitrogen phosphorus in the natural condition is limited, phosphoric particularly, so the nutritive elements such as nitrogen phosphorus of high-content have received people's concern gradually in the mud.In recent years, China is more and more lower to the nutritive element such as nitrogen, phosphorus concentration requirement in the sewage disposal plant effluent, the technology of a lot of intensified denitrification and dephosphorizations has obtained widely research, the compound that wherein adds iron is a kind of important technology of realizing chemical enhanced dephosphorization, and many these technology that studies show that realize that the reason of dephosphorization is to have generated the tertiary iron phosphate compound.
How to reclaim the tertiary iron phosphate in the mud, also do not have Patents and research report both at home and abroad.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of tertiary iron phosphate method that in mud, reclaims, can the phosphoric in the mud be reclaimed.
In order to achieve the above object, the technical scheme taked of the present invention is:
A kind of tertiary iron phosphate method that reclaims in mud may further comprise the steps:
The first step first through cracking pre-treatment, is carried out centrifugation to cracking the mixed solution that pre-treatment obtains with mud, obtains solid residue, and 80-105 ℃ of lower oven dry 8-12 hour,
Second step is dissolved in the solid residue after the oven dry in the hydrochloric acid of 1～3mol/L, and the quality of solid residue and the volume ratio of hydrochloric acid are 1g: 60ml, and centrifugation behind the Turning motion 18-24h is got supernatant liquor and separated mother liquor as the first tertiary iron phosphate; Simultaneously, in 600 ℃ retort furnace, be dissolved in the solid residue after the oven dry in the hydrochloric acid of 1～3mol/L behind calcination 1～3h, the quality of solid residue and the volume ratio of hydrochloric acid are 1g: 60ml, and centrifugation behind the Turning motion 18-24h is got supernatant liquor and separated mother liquor as the second tertiary iron phosphate; With analytically pure FeCl
3And H
3PO
4Configuration PO
4 3-And Fe
3+Concentration is the supersaturated solution of 0.01mol/L as the preparation mother liquor,
In the 3rd step, separate mother liquor to the first tertiary iron phosphate and separate the FeCl that adds 0.01mol/L in the mother liquor with the second tertiary iron phosphate
3Solution makes the Fe of system
3+Concentration and PO
4 3-Concentration identical,
The 4th step, in well-beaten situation, heighten the first tertiary iron phosphate of processing through the 3rd step with NaOH solution and separate mother liquor separates the making of mother liquor pH and second step with the second tertiary iron phosphate preparation mother liquor pH, when pH adjusts to 2.5～4.5, the tawny precipitation all appears in three kinds of solution, the centrifugation sedimentable matter, and be the rinsed with deionized water three times of 10 times of throw outs with volume, in 105 ℃ of baking ovens, dry 24h, obtain pure solid precipitation
The 5th step, adopt Fourier transform infrared spectroscopy, scanning electron microscope and X-ray diffraction analysis sedimentable matter essential property, determine that product is tertiary iron phosphate.
The present invention has following advantage and high-lighting effect:
1. propose first to reclaim the method that the phosphoric in the mud is produced tertiary iron phosphate.
2. the method has reclaimed in the mud 51～60% phosphoric, processes 1m
3Experiment can be produced 1.48～1.74kg tertiary iron phosphate with thickened sludge (98.79% water ratio, total phosphorous 25.18mg/g dewatered sludge).
Embodiment
Below in conjunction with embodiment the present invention is described in detail.
Embodiment 1
A kind of tertiary iron phosphate method that reclaims in mud may further comprise the steps:
The first step first through cracking pre-treatment, is carried out centrifugation to cracking the mixed solution that pre-treatment obtains with mud, obtains solid residue, and 80 ℃ of lower oven dry 12 hours,
Second step is dissolved in the solid residue after the oven dry in the hydrochloric acid of 1.5mol/L, and the quality of solid residue and the volume ratio of hydrochloric acid are 1g: 60ml, and centrifugation behind the Turning motion 24h is got supernatant liquor and separated mother liquor as the first tertiary iron phosphate; Simultaneously, in 600 ℃ retort furnace, be dissolved in the solid residue after the oven dry in the hydrochloric acid of 1.5mol/L behind the calcination 1h, the quality of solid residue and the volume ratio of hydrochloric acid are 1g: 60ml, and centrifugation behind the Turning motion 24h is got supernatant liquor and separated mother liquor as the second tertiary iron phosphate; With analytically pure FeCl
3And H
3PO
4Configuration PO
4 3-And Fe
3+Concentration is the supersaturated solution of 0.01mol/L as the preparation mother liquor,
In the 3rd step, separate mother liquor to the first tertiary iron phosphate and separate the FeCl that adds 0.01mol/L in the mother liquor with the second tertiary iron phosphate
3Solution makes the Fe of system
3+Concentration and PO
4 3-Concentration identical,
The 4th step, in well-beaten situation, heighten the first tertiary iron phosphate of processing through the 3rd step with NaOH solution and separate mother liquor separates the making of mother liquor pH and second step with the second tertiary iron phosphate preparation mother liquor pH, when pH adjusts to 2.5, the tawny precipitation all appears in three kinds of solution, the centrifugation sedimentable matter, and be the rinsed with deionized water three times of 10 times of throw outs with volume, in 105 ℃ of baking ovens, dry 24h, obtain pure solid precipitation
The 5th step, adopt Fourier transform infrared spectroscopy, scanning electron microscope and X-ray diffraction analysis sedimentable matter essential property, determine that product is tertiary iron phosphate.
Present embodiment has reclaimed in the mud 51% phosphoric, processes 1m
3Experiment can be produced the 1.48kg tertiary iron phosphate with thickened sludge (98.79% water ratio, total phosphorous 25.18mg/g dewatered sludge).
Embodiment 2
A kind of tertiary iron phosphate method that reclaims in mud may further comprise the steps:
The first step first through cracking pre-treatment, is carried out centrifugation to cracking the mixed solution that pre-treatment obtains with mud, obtains solid residue, and 95 ℃ of lower oven dry 11 hours,
Second step is dissolved in the solid residue after the oven dry in the hydrochloric acid of 2mol/L, and the quality of solid residue and the volume ratio of hydrochloric acid are 1g: 60ml, and centrifugation behind the Turning motion 24h is got supernatant liquor and separated mother liquor as the first tertiary iron phosphate; Simultaneously, in 600 ℃ retort furnace, be dissolved in the solid residue after the oven dry in the hydrochloric acid of 2mol/L behind the calcination 2h, the quality of solid residue and the volume ratio of hydrochloric acid are 1g: 60ml, and centrifugation behind the Turning motion 24h is got supernatant liquor and separated mother liquor as the second tertiary iron phosphate; With analytically pure FeCl
3And H
3PO
4Configuration PO
4 3-And Fe
3+Concentration is the supersaturated solution of 0.01mol/L as the preparation mother liquor,
In the 3rd step, separate mother liquor to the first tertiary iron phosphate and separate the FeCl that adds 0.01mol/L in the mother liquor with the second tertiary iron phosphate
3Solution makes the Fe of system
3+Concentration and PO
4 3-Concentration identical,
The 4th step, in well-beaten situation, heighten the first tertiary iron phosphate of processing through the 3rd step with NaOH solution and separate mother liquor separates the making of mother liquor pH and second step with the second tertiary iron phosphate preparation mother liquor pH, when pH adjusts to 3.0, the tawny precipitation all appears in three kinds of solution, the centrifugation sedimentable matter, and be the rinsed with deionized water three times of 10 times of throw outs with volume, in 105 ℃ of baking ovens, dry 24h, obtain pure solid precipitation
The 5th step, adopt Fourier transform infrared spectroscopy, scanning electron microscope and X-ray diffraction analysis sedimentable matter essential property, determine that product is tertiary iron phosphate.
Present embodiment has reclaimed in the mud 60% phosphoric, processes 1m
3Experiment can be produced the 1.74kg tertiary iron phosphate with thickened sludge (98.79% water ratio, total phosphorous 25.18mg/g dewatered sludge).
Embodiment 3
A kind of tertiary iron phosphate method that reclaims in mud may further comprise the steps:
The first step first through cracking pre-treatment, is carried out centrifugation to cracking the mixed solution that pre-treatment obtains with mud, obtains solid residue, and 105 ℃ of lower oven dry 10 hours,
Second step is dissolved in the solid residue after the oven dry in the hydrochloric acid of 3mol/L, and the quality of solid residue and the volume ratio of hydrochloric acid are 1g: 60ml, and centrifugation behind the Turning motion 24h is got supernatant liquor and separated mother liquor as the first tertiary iron phosphate; Simultaneously, in 600 ℃ retort furnace, be dissolved in the solid residue after the oven dry in the hydrochloric acid of 3mol/L behind the calcination 3h, the quality of solid residue and the volume ratio of hydrochloric acid are 1g: 60ml, and centrifugation behind the Turning motion 24h is got supernatant liquor and separated mother liquor as the second tertiary iron phosphate; With analytically pure FeCl
3And H
3PO
4Configuration PO
4 3-And Fe
3+Concentration is the supersaturated solution of 0.01mol/L as the preparation mother liquor,
In the 3rd step, separate mother liquor to the first tertiary iron phosphate and separate the FeCl that adds 0.01mol/L in the mother liquor with the second tertiary iron phosphate
3Solution makes the Fe of system
3+Concentration and PO
4 3-Concentration identical,
The 4th step, in well-beaten situation, heighten the first tertiary iron phosphate of processing through the 3rd step with NaOH solution and separate mother liquor separates the making of mother liquor pH and second step with the second tertiary iron phosphate preparation mother liquor pH, when pH adjusts to 4.5, the tawny precipitation all appears in three kinds of solution, the centrifugation sedimentable matter, and be the rinsed with deionized water three times of 10 times of throw outs with volume, in 105 ℃ of baking ovens, dry 24h, obtain pure solid precipitation
The 5th step, adopt Fourier transform infrared spectroscopy, scanning electron microscope and X-ray diffraction analysis sedimentable matter essential property, determine that product is tertiary iron phosphate.
Present embodiment has reclaimed in the mud 56% phosphoric, processes 1m
3Experiment can be produced the 1.61kg tertiary iron phosphate with thickened sludge (98.79% water ratio, total phosphorous 25.18mg/g dewatered sludge).
Claims (4)
1. one kind is reclaimed the tertiary iron phosphate method in mud, it is characterized in that, may further comprise the steps:
The first step first through cracking pre-treatment, is carried out centrifugation to cracking the mixed solution that pre-treatment obtains with mud, obtains solid residue, and 80-105 ℃ of lower oven dry 8-12 hour,
Second step is dissolved in the solid residue after the oven dry in the hydrochloric acid of 1～3mol/L, and the quality of solid residue and the volume ratio of hydrochloric acid are 1g: 60mL, and centrifugation behind the Turning motion 18-24h is got supernatant liquor and separated mother liquor as the first tertiary iron phosphate; Simultaneously, in 600 ℃ retort furnace, be dissolved in the solid residue after the oven dry in the hydrochloric acid of 1～3mol/L behind calcination 1～3h, the quality of solid residue and the volume ratio of hydrochloric acid are 1g: 60mL, and centrifugation behind the Turning motion 18-24h is got supernatant liquor and separated mother liquor as the second tertiary iron phosphate; With analytically pure FeCl
3And H
3PO
4Preparation PO
4 3-And Fe
3+Concentration is the supersaturated solution of 0.01mol/L as the preparation mother liquor,
In the 3rd step, separate mother liquor to the first tertiary iron phosphate and separate the FeCl that adds 0.01mol/L in the mother liquor with the second tertiary iron phosphate
3Solution makes the Fe of system
3+Concentration and PO
4 3-Concentration identical,
The 4th step, in well-beaten situation, heighten the first tertiary iron phosphate of processing through the 3rd step with NaOH solution and separate mother liquor separates the making of mother liquor pH and second step with the second tertiary iron phosphate preparation mother liquor pH, when pH adjusts to 2.5～4.5, the tawny precipitation all appears in three kinds of solution, the centrifugation sedimentable matter, and be the rinsed with deionized water three times of 10 times of throw outs with volume, in 105 ℃ of baking ovens, dry 24h, obtain pure solid precipitation
The 5th step, adopt Fourier transform infrared spectroscopy, scanning electron microscope and X-ray diffraction analysis sedimentable matter essential property, determine that product is tertiary iron phosphate.
2. a kind of tertiary iron phosphate method that reclaims in mud according to claim 1 is characterized in that, may further comprise the steps:
The first step first through cracking pre-treatment, is carried out centrifugation to cracking the mixed solution that pre-treatment obtains with mud, obtains solid residue, and 80 ℃ of lower oven dry 12 hours,
Second step is dissolved in the solid residue after the oven dry in the hydrochloric acid of 1.5mol/L, and the quality of solid residue and the volume ratio of hydrochloric acid are 1g: 60mL, and centrifugation behind the Turning motion 24h is got supernatant liquor and separated mother liquor as the first tertiary iron phosphate; Simultaneously, in 600 ℃ retort furnace, be dissolved in the solid residue after the oven dry in the hydrochloric acid of 1.5mol/L behind the calcination 1h, the quality of solid residue and the volume ratio of hydrochloric acid are 1g: 60mL, and centrifugation behind the Turning motion 24h is got supernatant liquor and separated mother liquor as the second tertiary iron phosphate; With analytically pure FeCl
3And H
3PO
4Preparation PO
4 3-And Fe
3+Concentration is the supersaturated solution of 0.01mol/L as the preparation mother liquor,
In the 3rd step, separate mother liquor to the first tertiary iron phosphate and separate the FeCl that adds 0.01mol/L in the mother liquor with the second tertiary iron phosphate
3Solution makes the Fe of system
3+Concentration and PO
4 3-Concentration identical,
The 4th step, in well-beaten situation, heighten the first tertiary iron phosphate of processing through the 3rd step with NaOH solution and separate mother liquor separates the making of mother liquor pH and second step with the second tertiary iron phosphate preparation mother liquor pH, when pH adjusts to 2.5, the tawny precipitation all appears in three kinds of solution, the centrifugation sedimentable matter, and be the rinsed with deionized water three times of 10 times of throw outs with volume, in 105 ℃ of baking ovens, dry 24h, obtain pure solid precipitation
The 5th step, adopt Fourier transform infrared spectroscopy, scanning electron microscope and X-ray diffraction analysis sedimentable matter essential property, determine that product is tertiary iron phosphate.
3. a kind of tertiary iron phosphate method that reclaims in mud according to claim 1 is characterized in that, may further comprise the steps:
The first step first through cracking pre-treatment, is carried out centrifugation to cracking the mixed solution that pre-treatment obtains with mud, obtains solid residue, and 95 ℃ of lower oven dry 11 hours,
Second step is dissolved in the solid residue after the oven dry in the hydrochloric acid of 2mol/L, and the quality of solid residue and the volume ratio of hydrochloric acid are 1g: 60mL, and centrifugation behind the Turning motion 24h is got supernatant liquor and separated mother liquor as the first tertiary iron phosphate; Simultaneously, in 600 ℃ retort furnace, be dissolved in the solid residue after the oven dry in the hydrochloric acid of 2mol/L behind the calcination 2h, the quality of solid residue and the volume ratio of hydrochloric acid are 1g: 60mL, and centrifugation behind the Turning motion 24h is got supernatant liquor and separated mother liquor as the second tertiary iron phosphate; With analytically pure FeCl
3And H
3PO
4Preparation PO
4 3-And Fe
3+Concentration is the supersaturated solution of 0.01mol/L as the preparation mother liquor,
In the 3rd step, separate mother liquor to the first tertiary iron phosphate and separate the FeCl that adds 0.01mol/L in the mother liquor with the second tertiary iron phosphate
3Solution makes the Fe of system
3+Concentration and PO
4 3-Concentration identical,
The 4th step, in well-beaten situation, heighten the first tertiary iron phosphate of processing through the 3rd step with NaOH solution and separate mother liquor separates the making of mother liquor pH and second step with the second tertiary iron phosphate preparation mother liquor pH, when pH adjusts to 3.0, the tawny precipitation all appears in three kinds of solution, the centrifugation sedimentable matter, and be the rinsed with deionized water three times of 10 times of throw outs with volume, in 105 ℃ of baking ovens, dry 24h, obtain pure solid precipitation
The 5th step, adopt Fourier transform infrared spectroscopy, scanning electron microscope and X-ray diffraction analysis sedimentable matter essential property, determine that product is tertiary iron phosphate.
4. a kind of tertiary iron phosphate method that reclaims in mud according to claim 1 is characterized in that, may further comprise the steps:
The first step first through cracking pre-treatment, is carried out centrifugation to cracking the mixed solution that pre-treatment obtains with mud, obtains solid residue, and 105 ℃ of lower oven dry 10 hours,
Second step is dissolved in the solid residue after the oven dry in the hydrochloric acid of 3mol/L, and the quality of solid residue and the volume ratio of hydrochloric acid are 1g: 60mL, and centrifugation behind the Turning motion 24h is got supernatant liquor and separated mother liquor as the first tertiary iron phosphate; Simultaneously, in 600 ℃ retort furnace, be dissolved in the solid residue after the oven dry in the hydrochloric acid of 3mol/L behind the calcination 3h, the quality of solid residue and the volume ratio of hydrochloric acid are 1g: 60mL, and centrifugation behind the Turning motion 24h is got supernatant liquor and separated mother liquor as the second tertiary iron phosphate; With analytically pure FeCl
3And H
3PO
4Preparation PO
4 3-And Fe
3+Concentration is the supersaturated solution of 0.01mol/L as the preparation mother liquor,
In the 3rd step, separate mother liquor to the first tertiary iron phosphate and separate the FeCl that adds 0.01mol/L in the mother liquor with the second tertiary iron phosphate
3Solution makes the Fe of system
3+Concentration and PO
4 3-Concentration identical,
The 4th step, in well-beaten situation, heighten the first tertiary iron phosphate of processing through the 3rd step with NaOH solution and separate mother liquor separates the making of mother liquor pH and second step with the second tertiary iron phosphate preparation mother liquor pH, when pH adjusts to 4.5, the tawny precipitation all appears in three kinds of solution, the centrifugation sedimentable matter, and be the rinsed with deionized water three times of 10 times of throw outs with volume, in 105 ℃ of baking ovens, dry 24h, obtain pure solid precipitation
The 5th step, adopt Fourier transform infrared spectroscopy, scanning electron microscope and X-ray diffraction analysis sedimentable matter essential property, determine that product is tertiary iron phosphate.
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| CN 201110375682 CN102503060B (en) | 2011-11-23 | 2011-11-23 | Method for recovering ferric phosphate from sludge |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110375682 CN102503060B (en) | 2011-11-23 | 2011-11-23 | Method for recovering ferric phosphate from sludge |
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| CN102503060A CN102503060A (en) | 2012-06-20 |
| CN102503060B true CN102503060B (en) | 2013-03-06 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE537780C2 (en) | 2013-05-02 | 2015-10-13 | Easymining Sweden Ab | Production of phosphate compounds from materials containing phosphorus and at least one of iron and aluminum |
| CN104609630B (en) * | 2015-01-19 | 2016-08-24 | 深圳市华虹清源环保科技有限公司 | Iron phosphate waste water treatment and reclamation devices and methods therefor |
| CN105772484B (en) * | 2016-03-23 | 2017-12-19 | 武汉纺织大学 | A kind of recovery method of municipal sludge incineration residue innoxious process for treating and phosphorus compound |
| CN111646674A (en) * | 2020-04-30 | 2020-09-11 | 中国环境科学研究院 | Method for releasing and recovering phosphorus in sludge |
| CN112551502A (en) * | 2020-12-21 | 2021-03-26 | 长沙工研院环保有限公司 | Method for recycling ferroelectrolytic phosphorus removal precipitate |
| CN113401887B (en) * | 2021-07-12 | 2022-07-19 | 湖北云翔聚能新能源科技有限公司 | Method for preparing iron phosphate by using municipal sludge incineration ash and battery-grade iron phosphate |
| CN116924378B (en) * | 2023-09-18 | 2023-12-12 | 内蒙古大学 | Method for directionally cleaning and recycling phosphorus in sludge through acid-regulated hydrothermal carbonization reforming treatment |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6503293B1 (en) * | 1999-06-25 | 2003-01-07 | Paul Dempsey | Process for the extraction of copper |
| CN101654238A (en) * | 2009-09-11 | 2010-02-24 | 华东理工大学 | Method for recovering phosphonium compound from phosphorous excess sludge of urban sewage treatment plant |
| CN101695999A (en) * | 2009-10-23 | 2010-04-21 | 宁波工程学院 | Method for recovering nutritive materials of phosphorus and nitrogen from sewage and sludge |
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2011
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6503293B1 (en) * | 1999-06-25 | 2003-01-07 | Paul Dempsey | Process for the extraction of copper |
| CN101654238A (en) * | 2009-09-11 | 2010-02-24 | 华东理工大学 | Method for recovering phosphonium compound from phosphorous excess sludge of urban sewage treatment plant |
| CN101695999A (en) * | 2009-10-23 | 2010-04-21 | 宁波工程学院 | Method for recovering nutritive materials of phosphorus and nitrogen from sewage and sludge |
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