CN115304230A - Three-in-one method for sludge reduction, VFAs production and phosphorus recovery - Google Patents
Three-in-one method for sludge reduction, VFAs production and phosphorus recovery Download PDFInfo
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- CN115304230A CN115304230A CN202210868548.2A CN202210868548A CN115304230A CN 115304230 A CN115304230 A CN 115304230A CN 202210868548 A CN202210868548 A CN 202210868548A CN 115304230 A CN115304230 A CN 115304230A
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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
- C02F11/06—Treatment of sludge; Devices therefor by oxidation
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/06—Flash distillation
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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
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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
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B17/00—Other phosphatic fertilisers, e.g. soft rock phosphates, bone meal
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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- C02F2101/105—Phosphorus compounds
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- C02F2303/00—Specific treatment goals
- C02F2303/06—Sludge reduction, e.g. by lysis
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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
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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Abstract
The invention provides a three-in-one method for sludge decrement, VFAs production and phosphorus recovery, which comprises the steps of increasing VFAs and releasing phosphorus through sludge hydrothermal oxidation, solid-phase fluidization, fluidized gas washing, mixed liquid-phase flash evaporation and flow splitting, VFAs separation, phosphorus enrichment through a recovery agent and the like. According to the technical scheme, pathogenic microorganisms in the sludge are thoroughly eliminated through hydrothermal oxidation reaction, solid organic matters in the sludge are promoted to be converted into VFAs, the release of phosphorus in the solids is enhanced, the harmless effect of the sludge is achieved, and then the sludge is deeply dehydrated through solid-phase fluidization operation, so that the sludge reduction effect is achieved. After the adsorption operation is adopted to recover the VFAs in the liquid phase, the VFAs-removed residual liquid can be circularly matched with an acidic solution for use, and the phosphorus element in the liquid phase is recovered in an insoluble substance replacement mode, namely, the phosphorus element is recovered through a series of steps, the content of impurities and pollutants in the liquid phase is obviously reduced, the biochemical treatment pressure of subsequent liquid discharge is effectively reduced, and the phosphorus-rich recovery agent can be directly used as a phosphorus raw material, so that obvious economic benefits are brought.
Description
Technical Field
The invention relates to the technical field of environmental protection, in particular to a three-in-one method for sludge reduction, VFAs production and phosphorus recovery.
Background
Municipal sludge is a byproduct generated in the municipal sewage treatment process, has high water content and high organic matter content, also contains non-renewable resources such as phosphorus and the like, and has high treatment difficulty. Common sludge disposal methods include mixed landfill, landscaping mud, soil improvement mud, building material mud and the like, and the treatment process focuses on reduction treatment of the sludge, and the water content of the sludge needs to be deeply dehydrated from more than 80% to less than 60% or even lower. Although the treatment method is simple, toxic and harmful substances in the sludge are not removed, so that secondary pollution is brought to the environment such as soil, water and the like. In addition, valuable substances such as organic substances and phosphorus in the sludge cannot be recovered, and resource waste is caused.
Municipal sludge contains a large amount of organic matters, so that sludge resources are becoming an important development direction for sludge treatment and disposal. Among the numerous treatment techniques, anaerobic digestion of sludge is of great interest. The technology obtains products such as methane, hydrogen, volatile fatty acid and the like through anaerobic fermentation. Concentrating organic sludge until the solid content is 20-40 g/L, adding an additive calcium nitrite, controlling the pH value to be 4.0-6.0, and performing hydrolytic acidification reaction at 35-39 ℃; adjusting the pH value of the sludge after hydrolytic acidification to 6.0-6.5, then carrying out anaerobic digestion reaction, and collecting methane. However, the product methane has low additional value and belongs to greenhouse gas, which is not beneficial to energy conservation and emission reduction. Therefore, volatile Fatty Acids (VFAs) are produced by utilizing the sludge, products with relatively high added values can be obtained, and the VFAs are used as important raw materials of biomass energy and can be directly utilized by a sewage treatment plant as an external carbon source. In addition, in another method, the sludge is frozen at the temperature of-20 to 0 ℃, then the temperature is raised to 0 to 10 ℃, then the organic sludge, the deionized water and the hydrogen peroxide are added into a reactor according to a certain proportion for hydrothermal oxidation, the reactor is heated to 200 to 400 ℃ in a salt bath furnace under a high-pressure environment for reaction for 0.5 to 20min, and the reactor is immediately taken out after the reaction is finished and put into ice water at the temperature of 0 ℃ for quenching, so that the acetic acid is obtained; however, the method has strict requirements on reaction conditions such as temperature and the like, the energy consumption is too high, and the equivalent resources of phosphorus element cannot be effectively recovered.
Besides organic matters, municipal sludge also contains a large amount of phosphorus elements, and the recovery of phosphorus from sewage sludge becomes a key for constructing sustainable phosphorus cycle. In the prior art, sludge enters a dehydration device for dehydration, and the dehydrated sludge enters a sludge drying device for drying; the dried sludge enters a carbonization furnace for anoxic carbonization treatment, and sludge carbide is generated after the sludge is carbonized; transferring the sludge carbide into an acid reaction tank and adding an acid solution; after full reaction, substances in the acid reaction tank are poured into a filtering device for filtering, the filtered liquid is the obtained phosphorus resource product, and the filtered solid is subjected to neutralization and resource utilization; however, the above method has a large energy consumption and cannot effectively utilize organic matters in the sludge.
In the prior art, main process units such as transfer aggregation, precipitation separation, biomembrane and denitrification treatment, hydrothermal treatment, modification preparation and the like are also adopted. The municipal sewage is subjected to transfer aggregation and precipitation treatment, organic matters are concentrated and enriched into sludge to be removed, then the sludge enters a biomembrane unit, phosphorus is removed through aerobic operation absorption, and finally the effluent meets the discharge requirement through biological denitrification treatment. Performing hydrothermal treatment on part of sludge to obtain a water-soluble macromolecular polymer, and modifying the water-soluble macromolecular polymer to prepare a transfer aggregation medium for reuse in a transfer aggregation process of sewage; in the anaerobic operation of the biomembrane unit and the aerobic operation which are alternately carried out, the same recovery liquid is repeatedly used until the phosphorus in the recovery liquid is gradually increased to the limit concentration and then replaced, and a high-concentration phosphorus solution can be obtained; the hydrothermal treatment also allows the production of carbon sources for biofilm and biological denitrification. The redundant sludge and the hydrothermal treatment solid-phase product are convenient to recycle. The method mainly depends on a biological method, recovers organic matters and phosphorus from a sewage end, has higher requirements on water inlet and outlet conditions and operation and is limited by the operation duration.
In conclusion, at present, no method for reducing municipal sludge and producing VFAs and recovering phosphorus is available, and a three-in-one method for reducing sludge, producing VFAs and recovering phosphorus, which is simple in operation, low in cost and good in popularization, is developed, so that the sludge is harmlessly treated, valuable organic matters and phosphorus in the sludge are effectively recovered, and the dual purposes of environmental protection and resource utilization can be realized.
Disclosure of Invention
The invention aims to provide a three-in-one method for sludge reduction, VFAs production and phosphorus recovery, which is characterized by comprising the following steps of:
thermal oxidation of sludge water to increase VFAs and release phosphorus
1-1, adding a hydrothermal oxidant into the dewatered sludge;
1-2, adding a hydrothermal oxidation promoter into the mixture obtained in the step 1-1, and then mixing;
1-3) feeding the mixture obtained in the step 1-2 into a reaction kettle, and adding an acidic solution into the reaction kettle for reaction;
1-4, after the reaction in the step 1-3), carrying out solid-liquid separation on the reaction product, and then carrying out treatment of the step 2) and the step 3 in no sequence;
solid-phase fluidization and fluidization gas scrubbing
Fluidizing the solid phase separated in the step 1-4 to reduce the volume of the solid phase and recover VFAs in the solid phase;
flash separation of mixed liquid phase
Carrying out flash evaporation on the mixed solution obtained by the separation in the step 1-4 to separate a VFAs-rich liquid phase and a phosphorus-rich liquid phase, and then carrying out treatment in the step 4) and the step 5 in a non-sequential manner;
separation of VFAs
Separating VFAs from the VFAs-rich liquid phase in an adsorption mode;
enriching phosphorus with recovery agent
And adding a reclaiming agent into the phosphorus-rich liquid phase to reclaim the phosphorus element.
In the technical scheme of the invention, through simple process steps, the three purposes of harmless and quantitative reduction treatment of the sludge, improvement of the yield and quality of VFAs and efficient recovery of phosphorus can be realized, and the method has double benefits of environment and economy.
Further, in the step 1-1, the hydrothermal oxidant is industrial-grade ferrous sulfate heptahydrate; the mass ratio of the hydrothermal oxidant to the dry weight of the dewatered sludge is (1);
further, in the step 1-2, the hydrothermal oxidation accelerator is industrial grade calcium hypochlorite; the mass ratio of the hydrothermal oxidizing agent to the hydrothermal oxidation promoter is 1;
further, the acid solution in the step 1-3 is hydrochloric acid; the mass ratio of the dry weight of the dewatered sludge to the acid solution is 1.
Further, the pH of the acidic solution is 4.5 to 6.5. The acid solution can come from VFAs-removed residual liquid recovered in the step 4), and hydrochloric acid can be added for preparation, so that the pH value of the acid solution is 4.5-6.5;
furthermore, when the reaction kettle carries out hydrothermal oxidation reaction, protective gas needs to be introduced to maintain the reaction pressure at 0.5-3 Mpa, the hydrothermal oxidation temperature is set at 120-240 ℃, and the hydrothermal oxidation time is 30-120 min.
Further, the protective gas is industrial nitrogen with the volume fraction of more than or equal to 99.2%.
Further, in the step 2), during fluidization treatment, fluidizing gas with the temperature of 130-180 ℃ is introduced at the speed of 0.5-5 BV/min (empty volume/min) to maintain the solid phase in a fluidized state, the fluidizing time is 3-10 min, and the high-temperature fluidizing gas can gasify and carry out the residual liquid containing VFAs in the solid phase, so that the solid phase is deeply dehydrated and the volume of the solid phase is further reduced.
Further, the fluidizing gas in the step 2) is industrial nitrogen with the volume fraction of more than or equal to 99.2 percent.
Further, the fluidizing gas after the completion of the fluidization is subjected to gas washing from the liquid phase separated in the step 1-4, and then sent to the step 3). And (1) intercepting the residual liquid containing VFAs carried out by the fluidizing gas by the separated liquid phase in the step (1-4), absorbing the heat of the fluidizing gas at the same time, and forming a preheated mixed liquid phase, wherein the mixed liquid phase contains both VFAs and phosphorus elements, and the fluidizing gas after washing can be recycled after being dried.
Further, in the step 3), during flash evaporation, further heating the preheated mixed liquid phase in the step 2 to 90-100 ℃, setting the flash evaporation pressure to be 75-90 Kpa, maintaining the gasified part of the mixed liquid phase in a liquid state under the flash evaporation condition, gasifying VFAs and water, condensing to obtain a VFAs-rich liquid phase, and forming a phosphorus-rich liquid phase on the part which is not gasified;
further, step 4) comprises loading VFAs on the adsorbent, desorbing VFAs and regenerating the adsorbent;
wherein:
auxiliary agent loading VFAs: keeping the temperature of the VFAs-rich liquid phase obtained in the step 3) at 20-40 ℃ and the speed at 0.5-3 BV/h (bed volume/hour), separating the VFAs from the aqueous solution by utilizing the adsorption performance of the adsorbent through a tower type adsorption column filled with the adsorbent, treating the VFAs-rich liquid phase with 50-100 times of volume of the adsorbent in unit volume to form the VFAs-loaded adsorbent, recovering the VFAs-removed residual liquid flowing through the tower type adsorption column, adjusting the acid and recycling the VFAs-removed residual liquid, namely the VFAs-removed liquid phase serving as the acidic solution in the step 1);
desorbing and collecting VFAs and regenerating the adsorbent: and (3) carrying out thermal desorption on the VFAs-loaded adsorbent in the step (4) by using desorption gas at the temperature of 160-200 ℃ according to the speed of 0.1-0.5 BV/min, gasifying the VFAs by the high-temperature desorption gas to carry away the adsorbent, condensing the VFAs carried away by the gasification and collecting the VFAs in a liquid phase form, drying the desorption gas for recycling, regenerating the desorbed adsorbent, and directly using the collected VFAs as a high-quality carbon source for a sewage plant or further processing the VFAs for other use.
Further, the adsorbent is fresh or regenerated polystyrene-divinylbenzene resin;
further, the stripping gas is industrial nitrogen with the volume fraction of more than or equal to 99.2 percent.
Further, when the recycling agent is enriched with phosphorus in the step 5), adding alkali into the phosphorus-enriched liquid phase obtained in the step 3 to adjust the pH value, and then adding the light calcium carbonate recycling agent;
further, adding alkali to adjust the pH value, namely adjusting the pH value of the phosphorus-rich liquid phase to 7-9 by using a sodium hydroxide solution;
further, the mass ratio of the recovering agent to the phosphorus-rich liquid phase is 1; after adding the reclaiming agent, keeping the temperature at 50-80 ℃, stirring for 30-90 min to reclaim phosphorus elements in the phosphorus-rich liquid phase, separating to obtain a phosphorus-containing reclaiming agent in a solid phase and a dephosphorizing residual liquid in a liquid phase after stirring is finished, wherein the phosphorus-containing reclaiming agent is not treated, and the content of the phosphorus-containing reclaiming agent is still as follows: the mass ratio of the phosphorus-rich liquid phase is 1-200-1, the temperature is 50-80 ℃, the stirring is carried out for 30-90 min to recover the phosphorus element in the phosphorus-rich liquid phase obtained in the step 3), the phosphorus-containing recovery agent after solid-liquid separation is repeated for 20-50 times to fully enrich the phosphorus element in the recovery agent, the phosphorus-enriched recovery agent can be processed into high-quality phosphate fertilizer or used for other purposes, and the dephosphorized residual liquid can be further processed and discharged after reaching the standard or used for other purposes.
The technical (preferred) scheme of the invention mainly has the following partial or whole technical effects:
(1) The environmental benefit is high: according to the invention, firstly, pathogenic microorganisms in the sludge are thoroughly eliminated through hydrothermal oxidation reaction to achieve the effect of sludge harmlessness, then, the sludge is deeply dehydrated through solid-phase fluidization operation to achieve the effect of sludge reduction, and the harmless sludge after reduction has small environmental burden when being subjected to subsequent treatment. After the adsorption operation is adopted to recover the VFAs in the liquid phase, the VFAs-removed residual liquid can be circularly used in an acid solution, and after the insoluble substance replacement mode is adopted to recover the phosphorus element in the liquid phase, the content of impurities and pollutants in the liquid phase is obviously reduced, so that the biochemical treatment pressure of subsequent liquid discharge is effectively reduced.
(2) The economic benefit is good. According to the invention, organic matters in the sludge are promoted to be converted into VFAs through hydrothermal oxidation, the release of phosphorus in solids is enhanced, the recovery of the VFAs is realized through the steps of flash flow distribution, adsorption enrichment, desorption and the like, and the recovery of phosphorus elements is realized through the steps of flash flow distribution, phosphorus enrichment by a recovery agent and the like, so that the value resources in the sludge are efficiently recovered, the recovered VFAs can be used as a high-quality carbon source and directly used in a sewage plant, and the recovered phosphorus-rich recovery agent can be directly used as a phosphate fertilizer, thereby bringing obvious economic benefits.
(3) Simple operation, simple equipment, easy maintenance and convenient popularization and application. The steps of hot water oxidation, fluidization, flash evaporation and flow distribution, adsorption, phosphorus enrichment of a recovery agent and the like involved in the method have low requirements on operation and equipment, are easy to maintain and are convenient to popularize.
(4) The operation cost is low and the economical efficiency is good. The adsorbent, the recycling agent and the industrial nitrogen adopted by the method are easy to obtain and have lower price, more importantly, the adsorbent is easy to regenerate and can be recycled for multiple times, the recycling agent can be used for multiple times without being processed, and the industrial nitrogen plays multiple roles of shielding gas, fluidizing gas and desorption gas and can be utilized in a gradient manner, so that the operation cost of the method is reduced.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, but it should not be construed that the scope of the above-described subject matter is limited to the following examples. Various substitutions and alterations can be made without departing from the technical idea of the invention and the scope of the invention is covered by the present invention according to the common technical knowledge and the conventional means in the field.
Example 1:
a three-in-one method for sludge reduction, VFAs production and phosphorus recovery is characterized by comprising the following steps:
1 ] production of VFAs and release of phosphorus by hydrothermal oxidation of sludge
1-1, adding a hydrothermal oxidant into the dewatered sludge; the hydrothermal oxidant is industrial-grade ferrous sulfate heptahydrate; the mass ratio of the hydrothermal oxidant to the dry weight of the dewatered sludge is 1:12.5;
1-2, adding a hydrothermal oxidation promoter into the mixture obtained in the step 1-1, and mixing; the hydrothermal oxidation accelerator is industrial grade calcium hypochlorite; the mass ratio of the hydrothermal oxidizing agent to the hydrothermal oxidation promoter is 1;
1-3) feeding the mixture obtained in the step 1-2 into a reaction kettle, and adding an acidic solution into the reaction kettle for reaction; the acidic solution is hydrochloric acid; the mass ratio of the dry weight of the dewatered sludge to the acid solution is 1. The pH value of the acid solution is 5.5, and the acid solution can be from the VFAs-removed residual liquid recovered in the step 4);
1-4, after the reaction in the step 1-3 is finished, carrying out solid-liquid separation on the reaction product, and then carrying out the treatment of the step 2 and the step 3 in no sequence;
during the hydrothermal oxidation reaction, protective gas (99.2% industrial nitrogen) is required to be introduced to maintain the reaction pressure at 2Mpa, the hydrothermal oxidation temperature is set at 180 ℃, and the hydrothermal oxidation time is 60min.
Solid-phase fluidization and fluidization gas scrubbing
Fluidizing the solid phase separated in the step 1-4 to reduce the volume of the solid phase and recover VFAs in the solid phase; during fluidization treatment, fluidizing gas (99.2% of industrial nitrogen) with the temperature of 155 ℃ is introduced at the speed of 2.5BV/min (empty volume/min) to maintain the solid phase in a fluidized state, the fluidizing time is 6min, and the high-temperature fluidizing gas can gasify and carry out the residual liquid containing VFAs in the solid phase, so that the solid phase is deeply dehydrated and the volume of the solid phase is further reduced.
The fluidizing gas after the fluidization is washed with the liquid phase separated in the step 1-4, and then sent to the step 3). And (1) intercepting the residual liquid containing VFAs carried out by the fluidizing gas by the separated liquid phase, absorbing the heat of the fluidizing gas at the same time to form a preheated mixed liquid phase, wherein the mixed liquid phase contains both VFAs and phosphorus elements, and the fluidized gas after washing can be recycled after being dried.
Flash separation of mixed liquid phase
Carrying out flash evaporation on the mixed solution obtained by the separation in the step 1-4 to separate a VFAs-rich liquid phase and a phosphorus-rich liquid phase, and then carrying out treatment in the step 4) and the step 5 in a non-sequential manner;
when flash evaporation is carried out, the preheated mixed liquid phase in the step 2 is further heated to 95 DEG
And C, setting the flash pressure to be 82Kpa, maintaining the part of the mixed liquid phase gasified to be in a liquid state under the flash conditions, so that the VFAs and the water are gasified and condensed to be a VFAs-rich liquid phase, and forming a phosphorus-rich liquid phase in the part which is not gasified.
Separating VFAs from the VFAs-rich liquid phase in an adsorption mode; comprises loading VFAs on an adsorbent, desorbing VFAs and regenerating the adsorbent;
wherein:
auxiliary agent loading VFAs: keeping the temperature of the VFAs-rich liquid phase obtained in the step 3) at 30 ℃ and the speed of 1.5BV/h (bed volume/hour), separating the VFAs from the aqueous solution by utilizing the adsorption performance of the adsorbent through a tower-type adsorption column filled with the adsorbent (polystyrene-divinylbenzene resin), treating the VFAs-rich liquid phase with 80 times of volume of the adsorbent in unit volume to form the VFAs-loaded adsorbent, recovering the VFAs-removed residual liquid flowing through the tower-type adsorption column, adjusting the acid and recycling the VFAs-removed residual liquid, namely the VFAs-removed residual liquid serving as the acidic solution in the step 1);
de-absorption and collection of VFAs and regeneration of adsorbent: and (3) carrying out thermal stripping desorption on the VFAs-loaded adsorbent in the step (4) by using stripping gas (99.2 percent of industrial nitrogen) with the temperature of 180 ℃ according to the speed of 0.3BV/min, carrying out high-temperature desorption gasification on the VFAs to separate the adsorbent, condensing the VFAs separated by gasification, collecting the VFAs in a liquid phase form, drying the stripping gas to recycle, regenerating the desorbed adsorbent, and directly using the collected VFAs as a high-quality carbon source of a sewage plant or further processing the VFAs for other purposes.
Enriching phosphorus by recovery agent
Adding sodium hydroxide solution into the obtained phosphorus-rich liquid phase to adjust the pH value of the phosphorus-rich liquid phase to 8, and then adding a light calcium carbonate recovery agent;
the mass ratio of the reclaiming agent to the phosphorus-rich liquid phase is 1; after adding the reclaiming agent, keeping the temperature at 65 ℃, stirring for 60min to reclaim phosphorus elements in the phosphorus-rich liquid phase, separating to obtain a solid-phase phosphorus-containing reclaiming agent and a liquid-phase dephosphorizing residual liquid after stirring is finished, wherein the phosphorus-containing reclaiming agent is not treated, and the phosphorus-containing reclaiming agent is still prepared according to the following steps of: and (2) recycling phosphorus elements in the phosphorus-rich liquid phase obtained in the step (3) under the conditions that the mass ratio of the phosphorus-rich liquid phase is 1.
Example 2:
a three-in-one method for sludge reduction, VFAs production and phosphorus recovery is characterized by comprising the following steps:
thermal oxidation of sludge water to increase VFAs and release phosphorus
1-1, adding a hydrothermal oxidant into the dewatered sludge; the hydrothermal oxidant is industrial-grade ferrous sulfate heptahydrate; the mass ratio of the hydrothermal oxidant to the dry weight of the dewatered sludge is 1:5;
1-2, adding a hydrothermal oxidation promoter into the mixture obtained in the step 1-1, and mixing; the hydrothermal oxidation accelerator is industrial grade calcium chlorate; the mass ratio of the hydrothermal oxidizing agent to the hydrothermal oxidation promoter is 2;
1-3) feeding the mixture obtained in the step 1-2 into a reaction kettle, and adding an acidic solution into the reaction kettle for reaction; the acidic solution is hydrochloric acid; the mass ratio of the dry weight of the dewatered sludge to the acid solution is 1. The pH value of the acid solution is 6.5, and the acid solution can be from the VFAs-removed residual liquid recovered in the step 4);
1-4, after the reaction in the step 1-3 is finished, carrying out solid-liquid separation on the reaction product, and then carrying out the treatment of the step 2 and the step 3 in no sequence;
during the hydrothermal oxidation reaction, protective gas (99.2% industrial nitrogen) is required to be introduced to maintain the reaction pressure at 3Mpa, the hydrothermal oxidation temperature is set at 120 ℃, and the hydrothermal oxidation time is 30min.
Solid-phase fluidization and fluidization gas scrubbing
Fluidizing the solid phase separated in the step 1-4 to reduce the volume of the solid phase and recover VFAs in the solid phase; during fluidization treatment, fluidizing gas (99.2% of industrial nitrogen) with the temperature of 130 ℃ is introduced at the rate of 0.5BV/min (empty volume/min) to maintain the solid phase in a fluidized state, the fluidizing time is 10min, and the high-temperature fluidizing gas can gasify and carry out the residual liquid containing VFAs in the solid phase, so that the solid phase is deeply dehydrated and the volume of the solid phase is further reduced.
The fluidizing gas after the fluidization is washed with the liquid phase separated in the step 1-4, and then sent to the step 3). And (1) intercepting the residual liquid containing VFAs carried out by the fluidizing gas by the separated liquid phase, absorbing the heat of the fluidizing gas at the same time to form a preheated mixed liquid phase, wherein the mixed liquid phase contains both VFAs and phosphorus elements, and the fluidized gas after washing can be recycled after being dried.
Flash separation of mixed liquid phase
Carrying out flash evaporation on the mixed solution obtained by the separation in the step 1-4 to separate a VFAs-rich liquid phase and a phosphorus-rich liquid phase, and then carrying out treatment in the step 4) and the step 5 in a non-sequential manner;
and (3) during flash evaporation, further heating the preheated mixed liquid phase in the step (2) to 100 ℃, setting the flash evaporation pressure to be 90Kpa, maintaining the gasified part of the mixed liquid phase in a liquid state under the flash evaporation condition, gasifying the VFAs and water, condensing to obtain a VFAs-rich liquid phase, and forming a phosphorus-rich liquid phase in the unvaporized part.
Separating VFAs from the VFAs-rich liquid phase in an adsorption mode; comprises loading VFAs on an adsorbent, desorbing VFAs and regenerating the adsorbent;
wherein:
auxiliary agent loading VFAs: keeping the temperature of the VFAs-rich liquid phase obtained in the step 3) at 40 ℃ at the speed of 0.5BV/h (bed volume/hour), separating the VFAs from the aqueous solution by utilizing the adsorption performance of the adsorbent through a tower-type adsorption column filled with the adsorbent (polystyrene-divinylbenzene resin), treating the VFAs-rich liquid phase with the volume of 100 times that of the adsorbent in unit volume to obtain the VFAs-loaded adsorbent, recovering VFAs-removed residual liquid flowing through the tower-type adsorption column, adjusting the acid and recycling the residual liquid, namely the residual liquid used as the acidic solution in the step 1);
de-absorption and collection of VFAs and regeneration of adsorbent: and (3) carrying out thermal stripping desorption on the VFAs-loaded adsorbent in the step (4) by using desorption gas (99.2 percent of industrial nitrogen) at the temperature of 200 ℃ according to the speed of 0.5BV/min, carrying out high-temperature desorption gasification on the VFAs to separate the adsorbent, condensing the VFAs separated by gasification, collecting the VFAs in a liquid phase form, drying the desorption gas for recycling, regenerating the desorbed adsorbent, and directly using the collected VFAs as a high-quality carbon source of a sewage plant or further processing the VFAs for other purposes.
Enriching phosphorus by recovery agent
Adding sodium hydroxide solution into the obtained phosphorus-rich liquid phase to adjust the pH value of the phosphorus-rich liquid phase to 9.0, and then adding a light calcium carbonate recovery agent;
the mass ratio of the reclaiming agent to the phosphorus-rich liquid phase is 1; after adding the reclaiming agent, keeping the temperature at 80 ℃, stirring for 30min to reclaim phosphorus elements in the phosphorus-rich liquid phase, separating to obtain a solid-phase phosphorus-containing reclaiming agent and a liquid-phase dephosphorizing residual liquid after stirring is finished, wherein the phosphorus-containing reclaiming agent is not treated, and the phosphorus-containing reclaiming agent is still prepared according to the following steps of: and (3) recovering phosphorus element in the phosphorus-rich liquid phase obtained in the step (3) under the conditions of a mass ratio of the phosphorus-rich liquid phase of 1:200, a temperature of 80 ℃ and stirring for 30min, and repeating the operation for 50 times by using the phosphorus-containing recovering agent after solid-liquid separation so as to fully enrich the phosphorus element in the recovering agent, thereby obtaining the raw material of phosphorus products (phosphate fertilizers and the like).
Example 3:
a three-in-one method for sludge reduction, VFAs production and phosphorus recovery is characterized by comprising the following steps:
thermal oxidation of sludge water to increase VFAs and release phosphorus
1-1, adding a hydrothermal oxidant into the dewatered sludge; the hydrothermal oxidant is industrial-grade ferrous sulfate heptahydrate; the mass ratio of the hydrothermal oxidant to the dry weight of the dewatered sludge is 1:20;
1-2, adding a hydrothermal oxidation promoter into the mixture obtained in the step 1-1, and mixing; the hydrothermal oxidation accelerator is industrial grade calcium hypochlorite; the mass ratio of the hydrothermal oxidizing agent to the hydrothermal oxidation promoter is 1;
1-3) feeding the mixture obtained in the step 1-2 into a reaction kettle, and adding an acidic solution into the reaction kettle for reaction; the acidic solution is hydrochloric acid; the mass ratio of the dry weight of the dewatered sludge to the acid solution is 1. The pH value of the acid solution is 4.5, and the acid solution can be from the VFAs-removed residual liquid recovered in the step 4);
1-4, after the reaction in the step 1-3 is finished, carrying out solid-liquid separation on the reaction product, and then carrying out the treatment of the step 2 and the step 3 in no sequence;
during the hydrothermal oxidation reaction, protective gas (99.2% industrial nitrogen) is required to be introduced to maintain the reaction pressure at 0.5Mpa, the hydrothermal oxidation temperature is set at 240 ℃, and the hydrothermal oxidation time is 120min.
Solid-phase fluidization and fluidization gas scrubbing
Fluidizing the solid phase obtained in the step 1-4 to reduce the volume of the solid phase and recover VFAs in the solid phase; during fluidization, fluidizing gas (99.2% of industrial nitrogen) with the temperature of 180 ℃ is introduced at the rate of 5BV/min (empty volume/min) to maintain the solid phase in a fluidized state, the fluidizing time is 3min, and the high-temperature fluidizing gas can gasify and carry out the VFAs-containing residual liquid in the solid phase, so that the solid phase is deeply dehydrated and the volume of the solid phase is further reduced.
And (3) after the fluidization gas which finishes fluidization is subjected to gas washing by the liquid phase separated in the step (1-4), sending the gas to the step (3). And (1) intercepting the residual liquid containing VFAs carried out by the fluidizing gas by the separated liquid phase, absorbing the heat of the fluidizing gas at the same time to form a preheated mixed liquid phase, wherein the mixed liquid phase contains both VFAs and phosphorus elements, and the fluidized gas after washing can be recycled after being dried.
Flash separation of mixed liquid phase
Carrying out flash evaporation on the mixed solution obtained by the separation in the step 1-4 to separate a VFAs-rich liquid phase and a phosphorus-rich liquid phase, and then carrying out treatment in the step 4) and the step 5 in a non-sequential manner;
and (3) during flash evaporation, further heating the preheated mixed liquid phase in the step 2) to 90 ℃, setting the flash evaporation pressure to be 75Kpa, maintaining the gasified part of the mixed liquid phase in a liquid state under the flash evaporation condition, gasifying the VFAs and water, condensing to obtain a VFAs-rich liquid phase, and forming a phosphorus-rich liquid phase in the unvaporized part.
Separating VFAs from the VFAs-rich liquid phase in an adsorption mode; comprises loading VFAs on an adsorbent, desorbing VFAs and regenerating the adsorbent;
wherein:
auxiliary agent loading VFAs: keeping the temperature of the VFAs-rich liquid phase obtained in the step 3) at 20 ℃ and the speed of 3BV/h (bed volume/hour), separating the VFAs from the aqueous solution by utilizing the adsorption performance of the adsorbent through a tower-type adsorption column filled with the adsorbent (polystyrene-divinyl phenyl resin), treating the VFAs-rich liquid phase with 50 times of volume of the adsorbent in unit volume to form the VFAs-loaded adsorbent, recovering the VFAs-removed residual liquid flowing through the tower-type adsorption column, adjusting the acid and recycling the VFAs-removed residual liquid, namely the VFAs-removed liquid phase serving as the acidic solution in the step 1);
de-absorption and collection of VFAs and regeneration of adsorbent: and (3) carrying out hot stripping desorption on the VFAs-loaded adsorbent in the step (4) by using desorption gas (99.2 percent of industrial nitrogen) with the temperature of 160 ℃ at the rate of 0.1BV/min, desorbing and gasifying the VFAs at high temperature, then carrying out separation on the adsorbent, condensing the VFAs carried out by gasification, collecting the VFAs in a liquid phase form, drying the desorption gas, recycling, regenerating the desorbed adsorbent, and directly using the collected VFAs as a high-quality carbon source for a sewage plant or further processing the VFAs for other purposes.
Enriching phosphorus by recovery agent
Adding sodium hydroxide solution into the obtained phosphorus-rich liquid phase to adjust the pH value of the phosphorus-rich liquid phase to 7.0, and then adding a light calcium carbonate recovery agent;
the mass ratio of the reclaiming agent to the phosphorus-rich liquid phase is 1; after adding the reclaiming agent, keeping the temperature at 50 ℃, stirring for 90min to reclaim phosphorus elements in the phosphorus-rich liquid phase, separating to obtain a phosphorus-containing reclaiming agent in a solid phase and a dephosphorizing residual liquid in a liquid phase after stirring is finished, wherein the phosphorus-containing reclaiming agent is not treated, and the content of the phosphorus-containing reclaiming agent is still as follows: and (3) the mass ratio of the phosphorus-rich liquid phase is 1.
The results of the tests on the sludge reduction effect (in terms of water content), the VFAs increase effect, and the phosphorus recovery rate in examples 1 to 3 are shown in table 1:
Claims (10)
1. a three-in-one method for sludge reduction, VFAs production and phosphorus recovery is characterized by comprising the following steps:
thermal oxidation of the sludge water to increase VFAs and release phosphorus
1-1, adding a hydrothermal oxidant into the dewatered sludge;
1-2, adding a hydrothermal oxidation promoter into the mixture obtained in the step 1-1, and then mixing;
1-3) feeding the mixture obtained in the step 1-2 into a reaction kettle, and adding an acidic solution into the reaction kettle for reaction;
1-4, after the reaction in the step 1-3 is finished, carrying out solid-liquid separation on the reaction product, and then carrying out the treatment of the step 2 and the step 3 in no sequence;
solid-phase fluidization and fluidization gas washing
Fluidizing the solid phase obtained in the step 1-4 to reduce the volume of the solid phase and recover VFAs in the solid phase;
flash separation of mixed liquid phase
Carrying out flash evaporation on the mixed solution obtained by the separation in the step 1-4 to separate a VFAs-rich liquid phase and a phosphorus-rich liquid phase, and then carrying out treatment in the step 4) and the step 5 in a non-sequential manner;
separation of VFAs
Separating VFAs from the VFAs-rich liquid phase in an adsorption mode;
enriching phosphorus by recovery agent
Adding a reclaiming agent into the phosphorus-rich liquid phase to reclaim phosphorus elements.
2. The three-in-one method for sludge reduction-production of VFAs-recovery of phosphorus as claimed in claim 1, wherein:
in the step 1-1, the hydrothermal oxidant is industrial-grade ferrous sulfate heptahydrate; the mass ratio of the hydrothermal oxidant to the dry weight of the dewatered sludge is 1.
3. The three-in-one method for sludge reduction-production of VFAs-recovery of phosphorus as claimed in claim 1 or 2, wherein the method comprises the following steps: in step 1-3, the acidic solution can be from the VFAs-removed residual liquid recovered in step 4), and can be prepared by adding hydrochloric acid, so that the pH value of the acidic solution is 4.5-6.5.
4. The three-in-one method for sludge reduction-production of VFAs-recovery of phosphorus as claimed in claim 3, wherein: the protective gas is industrial nitrogen with the volume fraction of more than or equal to 99.2 percent.
5. The three-in-one method for sludge reduction-production of VFAs-recovery of phosphorus as claimed in claim 1 or 3, wherein:
in the step 2, during fluidization treatment, fluidizing gas with the temperature of 130-180 ℃ is introduced at the speed of 0.5-5 BV/min (empty volume/min) to maintain the solid phase in a fluidized state, the fluidizing time is 3-10 min, and the high-temperature fluidizing gas can gasify and take out the residual liquid containing VFAs in the solid phase, so that the solid phase is deeply dehydrated and the volume of the solid phase is further reduced.
6. The three-in-one method for sludge reduction-production of VFAs-recovery of phosphorus as claimed in claim 5, wherein:
and in the step 2), the fluidizing gas is industrial nitrogen with the volume fraction of more than or equal to 99.2 percent.
The fluidizing gas after the fluidization is washed with the liquid phase separated in the step 1-4, and then sent to the step 3).
7. The three-in-one method for sludge reduction-production of VFAs-recovery of phosphorus as claimed in claim 1, wherein:
and 3) when flash evaporation is carried out, heating the mixed liquid phase in the step 2 to 90-100 ℃, setting the flash evaporation pressure to be 75-90 Kpa, so that VFAs and water are gasified, condensing to obtain a VFAs-rich liquid phase, and forming a phosphorus-rich liquid phase at the part which is not gasified.
8. The three-in-one method for sludge reduction-production of VFAs-recovery of phosphorus as claimed in claim 1, wherein:
step 4, loading VFAs on the adsorbent, desorbing VFAs and regenerating the adsorbent;
loading of the adsorbent with VFAs: keeping the temperature of the VFAs-rich liquid phase obtained in the step 3) at 20-40 ℃ and the speed at 0.5-3 BV/h (bed volume/hour), separating the VFAs from the aqueous solution by utilizing the adsorption performance of the adsorbent through a tower type adsorption column filled with the adsorbent, treating the VFAs-rich liquid phase with 50-100 times of volume of the adsorbent in unit volume to form an adsorbent loaded with the VFAs, recovering the VFAs-removed residual liquid flowing through the tower type adsorption column, adding hydrochloric acid to adjust the pH value, and recycling the residual liquid, namely the acidic solution in the step 1);
de-absorption and collection of VFAs and regeneration of adsorbent: desorbing the adsorbent loaded with VFAs in the step 4) by using desorption gas at the temperature of 160-200 ℃ in a hot blowing way at the rate of 0.1-0.5 BV/min, gasifying the VFAs by the high-temperature desorption gas and then carrying the VFAs away from the adsorbent, and condensing the VFAs carried away by the gasification and then collecting the VFAs in a liquid phase.
9. The three-in-one method for sludge reduction-production of VFAs-recovery of phosphorus as claimed in claim 8, wherein:
the adsorbent is fresh or regenerated polystyrene-divinyl phenyl resin;
the stripping gas is industrial nitrogen with the volume fraction of more than or equal to 99.2 percent.
10. The three-in-one method for sludge reduction, VFAs production and phosphorus recovery as claimed in claim 1, wherein the method comprises the following steps:
adding alkali to the phosphorus-rich liquid phase obtained in the step 3) to adjust the pH value when the recycling agent enriches phosphorus, and then adding a light calcium carbonate recycling agent;
adding alkali to adjust the pH value, namely adjusting the pH value of the phosphorus-rich liquid phase to 7-9 by adopting a sodium hydroxide solution;
the mass ratio of the reclaiming agent to the phosphorus-rich liquid phase is 1; after the reclaiming agent is added, the temperature is kept between 50 and 80 ℃, and the mixture is stirred for 30 to 90min to reclaim the phosphorus element in the phosphorus-rich liquid phase.
And (4) separating to obtain a solid-phase phosphorus-containing recycling agent and a liquid-phase dephosphorizing residual liquid after stirring is finished, wherein the phosphorus-containing recycling agent is recycled as the recycling agent used in the step 5 without treatment and is repeatedly recycled for a plurality of times to be used as a phosphorus raw material.
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