CN114477119A - Method for enhancing recovery of phosphorus resources in municipal sludge hydrothermal carbonization liquid - Google Patents
Method for enhancing recovery of phosphorus resources in municipal sludge hydrothermal carbonization liquid Download PDFInfo
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- CN114477119A CN114477119A CN202210159560.6A CN202210159560A CN114477119A CN 114477119 A CN114477119 A CN 114477119A CN 202210159560 A CN202210159560 A CN 202210159560A CN 114477119 A CN114477119 A CN 114477119A
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- hydrothermal carbonization
- sludge hydrothermal
- phosphorus
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- 238000003763 carbonization Methods 0.000 title claims abstract description 48
- 239000010802 sludge Substances 0.000 title claims abstract description 46
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000011574 phosphorus Substances 0.000 title claims abstract description 43
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000007788 liquid Substances 0.000 title claims abstract description 32
- 238000011084 recovery Methods 0.000 title claims abstract description 24
- 230000002708 enhancing effect Effects 0.000 title claims description 8
- 238000002425 crystallisation Methods 0.000 claims abstract description 23
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 23
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 23
- 230000008025 crystallization Effects 0.000 claims abstract description 22
- 239000000126 substance Substances 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 108091005804 Peptidases Proteins 0.000 claims abstract description 12
- 239000004365 Protease Substances 0.000 claims abstract description 12
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 claims abstract description 12
- 239000000413 hydrolysate Substances 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001448 ferrous ion Inorganic materials 0.000 claims abstract description 7
- 230000014759 maintenance of location Effects 0.000 claims abstract description 7
- 230000001105 regulatory effect Effects 0.000 claims abstract description 6
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 5
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 5
- 238000009287 sand filtration Methods 0.000 claims abstract description 5
- 230000007065 protein hydrolysis Effects 0.000 claims abstract description 4
- 238000005728 strengthening Methods 0.000 claims abstract description 4
- 108010009736 Protein Hydrolysates Proteins 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 4
- 102000004142 Trypsin Human genes 0.000 claims description 3
- 108090000631 Trypsin Proteins 0.000 claims description 3
- 238000004132 cross linking Methods 0.000 claims description 3
- 230000001965 increasing effect Effects 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 239000012588 trypsin Substances 0.000 claims description 3
- 239000013618 particulate matter Substances 0.000 claims description 2
- 230000000536 complexating effect Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000010865 sewage Substances 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910010710 LiFePO Inorganic materials 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- CKMXBZGNNVIXHC-UHFFFAOYSA-L ammonium magnesium phosphate hexahydrate Chemical compound [NH4+].O.O.O.O.O.O.[Mg+2].[O-]P([O-])([O-])=O CKMXBZGNNVIXHC-UHFFFAOYSA-L 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 230000003100 immobilizing effect Effects 0.000 description 1
- 229910052816 inorganic phosphate Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 229910052567 struvite Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
Classifications
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- 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
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention discloses a method for strengthening recovery of phosphorus resources in municipal sludge hydrothermal carbonization liquid. The method comprises the following steps: s1, preparing immobilized protease; s2, removing suspended solids from the sludge hydrothermal carbonization liquid through sand filtration; s3, adding immobilized protease into the filtered sludge hydrothermal carbonization liquid in a protein hydrolysis unit, and fully hydrolyzing to obtain sludge hydrothermal carbonization hydrolysate; s4, determining the phosphorus concentration and the residual protein substance concentration of the sludge hydrothermal carbonization hydrolysate in a crystallization reaction unit, adding ferrous salt according to the molar ratio of Fe to P being 1.5: 1, and performing crystallization reaction by regulating the pH value and the hydraulic retention time according to the residual protein substance concentration to obtain the ferrocyanide. According to the invention, the immobilized protease is used for fully hydrolyzing the protein in the sludge hydrothermal carbonization liquid, so that the complexing effect of the protein on ferrous ions is effectively reduced, the phosphorus removal efficiency of the sludge hydrothermal carbonization hydrolysate is improved, and the recovery of effective phosphorus resources is promoted.
Description
Technical Field
The invention belongs to the technical field of wastewater treatment, and particularly relates to a method for strengthening recovery of phosphorus resources in municipal sludge hydrothermal carbonization liquid.
Background
Phosphorus resources are non-metallic mineral resources that are difficult to regenerate and irreplaceable in the world. In recent years, the exploitation of a large amount of phosphorus ore resources and the development of technologies for recycling phosphorus resources have been slow, resulting in the present situation of depletion of phosphorus resources. Meanwhile, excessive accumulation of phosphorus in water can lead to eutrophication of water. Therefore, the development of an effective phosphorus resource recovery technology has become one of the main tasks facing municipal sewage plants in the future.
At present, phosphorus-containing sewage/wastewater phosphorus removal methods comprise a chemical precipitation method, a biological method, a crystallization method and the like. Among these processes, phosphorus crystallization is a promising process for phosphorus recovery, and products thereof include calcium phosphate, struvite, and hematite. Wherein, ferroconite (Fe)3(PO4)2·8H2O) crystallization is a new technology for recovering phosphorus from wastewater with application prospect. The ferroconite is a colorless inorganic phosphate crystal mineral, is widely concerned due to the near-neutral crystallization condition and good economy, can be used as a fertilizer to provide phosphorus and iron for plants, and can also be used as an energy storage material, namely lithium iron phosphate (LiFePO)4) The synthesis of (2) is one of the main synthetic raw materials of the power lithium ion battery. The cycocite crystal is used as a new technology for removing and recycling phosphate in sewage/wastewater, and the crystallization process is simple and easy to implement, has low cost and has good application prospect.
In the process of the ferrocyanide crystallization technology, phosphorus in municipal sewage is enriched in excess sludge after being treated by a biological unit of a sewage plant. Hydrothermal carbonization, as an effective sludge reduction technology, has the potential of simultaneously controlling pollution and promoting resource recovery. After the hydrothermal carbonization treatment, a large amount of recoverable orthophosphate is transferred from the sludge into the hydrothermal carbonization liquid. However, the sludge hydrothermal carbonization liquid contains a large amount of proteins derived from activated sludge microbial cells, and has a wide variety of types and complicated components. These proteins can bind ferrous ions, resulting in a reduction in available free ferrous ions, reducing supersaturation levels, and thus reducing phosphorus removal efficiency by reducing driving forces to interfere with ferrocyanite crystallization. Therefore, the influence of protein substances on the crystallization process of the ferrocyanide is reduced by adopting effective means, and the method has important significance on resource recycling of phosphorus in the sludge hydrothermal carbonization liquid.
Disclosure of Invention
The invention aims to solve the problems in the prior art and solve the problems of high-efficiency removal and recovery of a large amount of phosphorus resources in the sludge hydrothermal carbonization liquid. Provides a method for strengthening the recovery of phosphorus resources in municipal sludge hydrothermal carbonization liquid. The technical scheme of the invention is realized in such a way, and comprises the following steps:
s1, preparing immobilized protease;
s2, removing suspended solids from the sludge hydrothermal carbonization liquid through sand filtration;
s3, in the protein hydrolysis unit, adding the immobilized protease into the filtered sludge hydrothermal carbonization liquid, and fully hydrolyzing under proper temperature and pH conditions to obtain sludge hydrothermal carbonization hydrolysate;
s4, in a crystallization reaction unit, measuring the phosphorus concentration and the concentration of residual protein substances in the sludge hydrothermal carbonization hydrolysate, adding ferrous salt according to the molar ratio of Fe to P being 1.5: 1, and regulating the pH value and hydraulic retention time according to the concentration of the residual protein substances to enable ferrous ions and phosphate ions to generate crystallization reaction, thereby obtaining the phosphorus recovery product ferroconite.
Preferably, D151 resin is used as a carrier for immobilizing trypsin, and an adsorption-microwave assisted crosslinking method is adopted to prepare the immobilized protease.
Preferably, the suspended solid in S2 includes particulate matter and part of colloidal matter including proteinaceous organic matter.
Preferably, the suitable temperature in S3 is 25-45 ℃, the suitable pH is 5.0-5.5.
Preferably, the pH value in S4 is regulated within the range of 6.0-7.0 according to the concentration of residual protein substances in the sludge hydrothermal carbonization hydrolysate, and the optimal pH value is increased along with the increase of the concentration of the residual protein substances.
Preferably, the hydraulic retention time of the ferroconite crystallization reaction process in S4 is controlled to be 1-2 h.
The invention has the following advantages:
the method has the advantages that proteins in the sludge hydrothermal carbonization liquid are fully hydrolyzed, the complexing effect of the proteins on ferrous ions is effectively reduced, and the influence of the proteins on the phosphorus removal efficiency is eliminated; secondly, the phosphorus removal efficiency in the sludge hydrothermal carbonization hydrolysate is improved, and meanwhile, the recovery of effective phosphorus resources is promoted.
Drawings
FIG. 1 is a schematic flow chart of a method for enhancing recovery of phosphorus resources from municipal sludge hydrothermal carbonization liquid.
Detailed Description
The following detailed description of the patent embodiments refers to the accompanying drawings.
A phosphorus recovery method for partition regulation of ferrocyanite crystals by a fluidized bed comprises the following steps:
s1, preparing immobilized protease by taking D151 resin as a carrier of the immobilized trypsin through an adsorption-microwave-assisted crosslinking method;
s2, removing suspended solids from the sludge hydrothermal carbonization liquid through sand filtration, wherein the suspended solids are particulate matters and partial colloidal substances including protein organic matters;
s3, in a protein hydrolysis unit, adding immobilized protease into the filtered sludge hydrothermal carbonization liquid, and fully hydrolyzing at 25-45 ℃ and pH 5.0-5.5 to obtain sludge hydrothermal carbonization hydrolysate;
s4, in a crystallization reaction unit, measuring the phosphorus concentration and the concentration of residual protein substances in the sludge hydrothermal carbonization hydrolysate, adding ferrous salt according to the molar ratio of Fe to P of 1.5 to 1, regulating and controlling the pH and hydraulic retention time within 1-2h within the range of 6.0-7.0 according to the concentration of the residual protein substances, and increasing the optimal pH value along with the increase of the concentration of the residual protein substances to enable the ferrous ions and the phosphate ions to perform crystallization reaction to obtain a phosphorus recovery product, namely ferroconite.
Example 1
PO in carbonization liquid generated by hydrothermal carbonization process of sludge of certain municipal sewage treatment plant4-a concentration of 128mg/L of P; the concentration of TP is 199 mg/L; the TN concentration is 1810 mg/L; BOD58950 mg/L; COD is 19200mg/L, suspended solids in the carbonization liquid are removed by sand filtration, and the carbonization liquid enters an immobilized protease hydrolysis unit and is fully hydrolyzed under the conditions of temperature of 30 ℃ and pH value of 5.0 to obtain the sludge hydrothermal carbonization hydrolysis liquid. Mixing 128mg/L PO4Pumping the sludge hydrothermal carbonization hydrolysate of the P and a ferrous salt solution of 69.4g/L into a ferroconite crystallization reaction unit at the flow rates of 500L/h and 2.5L/h respectively to enable the molar ratio of Fe (II)/P to be 1.5; the pH value in the crystallization reaction unit is monitored in real time through a pH control system, and 1mol/L sodium hydroxide solution is continuously injected into the ferrocyanide crystallization reaction unit to regulate and control the ferrocyanide crystalsThe pH value in the crystal unit is 6; the hydraulic retention time in the ferrocyanide crystallization reaction unit is 1 h; and a crystal discharge port is arranged at the bottom of the ferrocyanide crystallization reaction unit, and the ferrocyanide crystals are collected. After the sludge carbonization liquid reinforced phosphorus resource recovery technology is operated, the effluent PO4the-P stability is lower than 25.6mg/L, and the high-efficiency recovery of phosphorus in the sludge hydrothermal carbonization liquid is realized.
Claims (6)
1. A method for strengthening recovery of phosphorus resources in municipal sludge hydrothermal carbonization liquid is characterized by comprising the following steps: the method comprises the following steps:
s1, preparing immobilized protease;
s2, removing suspended solids from the sludge hydrothermal carbonization liquid through sand filtration;
s3, in the protein hydrolysis unit, adding the immobilized protease into the filtered sludge hydrothermal carbonization liquid, and fully hydrolyzing under proper temperature and pH conditions to obtain sludge hydrothermal carbonization hydrolysate;
s4, in a crystallization reaction unit, measuring the phosphorus concentration and the concentration of residual protein substances in the sludge hydrothermal carbonization hydrolysate, adding ferrous salt according to the molar ratio of Fe to P being 1.5: 1, and regulating the pH value and hydraulic retention time according to the concentration of the residual protein substances to enable ferrous ions and phosphate ions to generate crystallization reaction, thereby obtaining the phosphorus recovery product ferroconite.
2. The method for enhancing the recovery of phosphorus resources from the municipal sludge hydrothermal carbonization liquid according to claim 1, wherein the method comprises the following steps: d151 resin is used as a carrier of immobilized trypsin, and an adsorption-microwave-assisted crosslinking method is adopted to prepare the immobilized protease.
3. The method for enhancing the recovery of phosphorus resources from the municipal sludge hydrothermal carbonization liquid according to claim 1, wherein the method comprises the following steps: the suspended solid in S2 comprises particulate matter and partial colloidal substances including protein organic matters.
4. The method for enhancing the recovery of phosphorus resources from the municipal sludge hydrothermal carbonization liquid according to claim 1, wherein the method comprises the following steps: the appropriate temperature in S3 is 25-45 deg.C, and the appropriate pH is 5.0-5.5.
5. The method for enhancing the recovery of phosphorus resources from the municipal sludge hydrothermal carbonization liquid according to claim 1, wherein the method comprises the following steps: the pH value in S4 should be regulated and controlled within the range of 6.0-7.0 according to the concentration of residual protein substances in the sludge hydrothermal carbonization hydrolysate, and the optimal pH value is increased along with the increase of the concentration of the residual protein substances.
6. The method for enhancing the recovery of phosphorus resources from the municipal sludge hydrothermal carbonization liquid according to claim 1, wherein the method comprises the following steps: the hydraulic retention time of the ferroconite crystallization reaction process in the S4 is controlled to be 1-2 h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210159560.6A CN114477119A (en) | 2022-02-18 | 2022-02-18 | Method for enhancing recovery of phosphorus resources in municipal sludge hydrothermal carbonization liquid |
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| CN202210159560.6A CN114477119A (en) | 2022-02-18 | 2022-02-18 | Method for enhancing recovery of phosphorus resources in municipal sludge hydrothermal carbonization liquid |
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| NL2028955A (en) * | 2020-11-30 | 2022-01-13 | Univ Suzhou Sci & Technology | Process for enriching phosphorus and recovering vivianite by biofilm method |
| WO2022022090A1 (en) * | 2020-07-29 | 2022-02-03 | 同济大学 | Method for recovering vivianite from sludge incineration ash |
-
2022
- 2022-02-18 CN CN202210159560.6A patent/CN114477119A/en active Pending
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