CN107601793B - Device and method for simultaneously preparing protein intercalated hydrotalcite material by sludge protein extraction - Google Patents
Device and method for simultaneously preparing protein intercalated hydrotalcite material by sludge protein extraction Download PDFInfo
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- 239000010802 sludge Substances 0.000 title claims abstract description 127
- 108090000623 proteins and genes Proteins 0.000 title claims abstract description 86
- 102000004169 proteins and genes Human genes 0.000 title claims abstract description 86
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 71
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 70
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 70
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- 239000000498 cooling water Substances 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
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- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims description 3
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- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
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- 238000005336 cracking Methods 0.000 abstract description 9
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- 238000004064 recycling Methods 0.000 abstract description 6
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Abstract
The invention discloses a device and a method for extracting sludge protein and simultaneously preparing a protein intercalated hydrotalcite material, belonging to the technical field of excess sludge treatment. The method comprises a reaction kettle, a horizontal centrifuge and a stainless steel barrel which are sequentially connected through a pipeline, and under the condition that no chemical agent is added, the high-efficiency cracking of reaction materials is achieved by means of acoustic cavitation and irradiation, and meanwhile, excessive damage of sludge protein and subsequent separation procedures caused by mixing of the chemical agent into the sludge protein are avoided; the sludge protein liquid enters a stainless steel barrel provided with a hydrotalcite filter, the protein intercalated hydrotalcite material is prepared by means of strong affinity of hydrotalcite and protein, and the structure of the protein intercalated hydrotalcite material can be regulated and controlled by regulating the temperature and pressure. The invention can not only realize the effective cracking of the residual sludge and the reduction treatment of the residual sludge, but also realize the recycling of the residual sludge. The device is novel in structure, environment-friendly, convenient to use and high in efficiency.
Description
Technical Field
The invention belongs to the technical field of excess sludge treatment, and relates to a device and a method for extracting sludge protein and simultaneously preparing a protein intercalated hydrotalcite material.
Background
With the increasing exhaustion of resources, the recycling of waste resources has become a worldwide development trend. Excess sludge (activated sludge discharged from a secondary sedimentation tank in an activated sludge system) is a waste which is solid, semi-solid and liquid and has huge content, and environmental pollution is serious. The investigation shows that the residual sludge contains a large amount of organic matters, nitrogen and phosphorus and other nutrients, heavy metals, pathogenic bacteria and the like, wherein the content of the organic matters is about 55% -60%, the highest content of the organic matters is microbial single-cell proteins, and the proteins have the advantages of good quality, complete amino acid types and the like, are not only excellent raw materials for developing foaming agents, but also can develop various chemical functional materials. The protein is obtained from the excess sludge, which accords with the sludge recycling policy and is one of the hot problems of the research at home and abroad at present.
If the sludge protein is to be extracted, the sludge must be first effectively broken to allow the cellular content to flow out into the aqueous phase, and then the protein is separated and purified in the aqueous phase. Currently common methods are chemical, biological, heat treatment, physical and combinations of these. Research results show that the methods can promote the cracking of the microbial cells of the excess sludge to a certain extent and accelerate the dissolution and release of intracellular organic matters. However, these methods have the problems of low efficiency, old equipment, long production period, complex secondary separation procedure, serious protein damage and the like, so that the sludge protein is difficult to popularize and apply widely.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a device and a method for extracting sludge protein and simultaneously preparing protein intercalated hydrotalcite material, the device has reasonable structural design and convenient use, and can realize effective cracking of residual sludge so as to achieve reduction treatment of the residual sludge; the method is simple to operate, and the protein intercalation hydrotalcite functional material can be prepared while the residual sludge protein is cracked.
The invention is realized by the following technical scheme:
the invention discloses a device for extracting sludge protein and simultaneously preparing protein intercalated hydrotalcite material, which comprises a reaction kettle, a horizontal centrifuge and a stainless steel barrel, wherein a discharge port of a surplus sludge tank is connected with the reaction kettle through a pipeline, and a first ball valve and a first screw pump are arranged on the pipeline; the discharge port of the reaction kettle is connected with the feed port of the horizontal centrifuge through a pipeline, and a second ball valve and a second screw pump are arranged on the pipeline; the liquid outlet of the horizontal centrifuge is connected with the liquid inlet of the stainless steel barrel through a pipeline, and a third ball valve is arranged on the pipeline; the filtrate outlet of the stainless steel barrel is connected to the residual sludge tank through a pipeline, and a fourth ball valve is arranged on the pipeline;
an ultrasonic unit capable of applying cavitation to the excess sludge is arranged at the upper end of the reaction kettle, and an electron accelerator capable of applying irradiation to the excess sludge is arranged at the lower end of the reaction kettle; a stainless steel barrel is filled with a plurality of layers of hydrotalcite filters.
Preferably, the ultrasonic unit is composed of an ultrasonic transducer and an ultrasonic generator, and the ultrasonic transducer and the ultrasonic generator are electrically connected; an ultrasonic amplitude transformer on the ultrasonic transducer can extend into the reaction kettle.
Further preferably, the ultrasonic transducer is further provided with a cooling water channel, and cooling water enters the cooling water channel through the cooling water inlet and flows out of the cooling water outlet to form a water cooling system.
Preferably, the stainless steel barrel further comprises a temperature control unit and a pressure control unit which are arranged outside the stainless steel barrel;
the temperature control unit comprises a heater and a temperature controller connected with the heater;
the pressure control unit comprises an argon steel cylinder connected with the stainless steel barrel through a pipeline, and a fifth ball valve and a flowmeter are arranged on the pipeline.
Preferably, a sludge discharge port for discharging sludge is arranged at the bottom of the horizontal centrifuge.
Preferably, the irradiation dose of the electron accelerator is below 30 kGy.
The invention also discloses a method for extracting sludge protein and simultaneously preparing protein intercalated hydrotalcite material by adopting the device, which comprises the following steps:
1) Opening a first ball valve and a first screw pump, conveying the residual sludge in the residual sludge tank to a reaction kettle, and adjusting the sludge feeding flow through the first ball valve;
2) Starting an ultrasonic unit and an electronic accelerator to carry out ultrasonic wave and irradiation treatment on the sludge, opening a second ball valve and a second screw pump after the sludge is fully broken, enabling a broken sludge solution to enter a horizontal centrifuge for solid-liquid separation, separating solid sludge from sludge supernatant under the action of centrifugal force, discharging sludge, and dissolving sludge protein into a water phase;
3) And starting the third ball valve to enable the sludge protein to enter the stainless steel barrel, enabling the sludge protein to enter a hydrotalcite structural gap under the adsorption and filtration effects of the hydrotalcite filter, opening the fourth ball valve to enable filtrate to flow out of the stainless steel barrel and return to a raw material inlet of the residual sludge tank, and collecting solids in the hydrotalcite filter, namely the protein intercalated hydrotalcite material.
Preferably, the spatial structure of the protein intercalated hydrotalcite material can be regulated and controlled by a temperature control unit and a pressure control unit arranged outside the stainless steel barrel.
Preferably, the hydrotalcite filter is prepared by the following method:
mixing magnesium aluminum hydrotalcite and polyvinyl alcohol according to a mass ratio of 1:3 to obtain a mixed solution; taking a plurality of sponges with the same inner diameter size of a stainless steel barrel, soaking the sponges in the mixed solution, taking out the sponges after the sponges are saturated, drying at 55+/-2 ℃, and repeatedly soaking and drying for 5 times; and (3) treating the sponge dried for the last time at 950+/-30 ℃ for 4 hours, and cooling to obtain the hydrotalcite filter.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the device for simultaneously preparing the protein intercalated hydrotalcite material by extracting the sludge protein, disclosed by the invention, the ultrasonic unit and the electron accelerator are arranged on the reaction kettle, so that the efficient cracking of reaction materials is achieved by means of acoustic cavitation and irradiation under the condition that no chemical agent is added, and meanwhile, the excessive damage of the sludge protein and the subsequent separation procedure caused by mixing of the chemical agent into the sludge protein are avoided. Meanwhile, the treated sludge protein liquid enters a stainless steel barrel provided with a hydrotalcite filter, and the protein intercalated hydrotalcite material can be prepared by virtue of stronger affinity of hydrotalcite and protein. The invention can realize the effective cracking of the residual sludge, the reduction treatment of the residual sludge, and the recycling of the residual sludge, and the prepared protein intercalated hydrotalcite material can be used as an adsorbent for wastewater treatment and a catalyst for energy conversion. And the stainless steel barrel discharges filtrate and can return to the raw material inlet of the surplus sludge tank, so that the surplus sludge can be diluted, the protein release rate is accelerated, no additional water is needed in the process, and a limited fresh water source is saved. The device has reasonable structural design, green and environment-friendly performance, convenient use, high efficiency and remarkable economic benefit.
Further, the device also comprises a temperature control unit and a pressure control unit which are arranged outside the stainless steel barrel, and the structure of the protein intercalated hydrotalcite material can be regulated and controlled by regulating the temperature and the pressure.
Further, a sludge discharge port for discharging sludge is arranged at the bottom of the horizontal centrifuge, and the discharged sludge is collected and then subjected to corresponding physical property adjustment according to a physical and chemical property analysis result, so that the sludge can be used as building materials or greening soil after adjustment.
Drawings
Fig. 1 is a schematic diagram of the structure of the excess sludge protein extraction device of the invention.
Wherein: 1 is a first ball valve; 2 is a first screw pump; 3 is an electron accelerator; 4 is a reaction kettle; 5 is an ultrasonic transducer; 6 is an ultrasonic generator; 7 is a second ball valve; 8 is a second screw pump; 9 is a horizontal centrifuge; 10 is a flowmeter; 11 is a fifth ball valve; 12 is an argon steel cylinder; 13 is a temperature controller; 14 is a heater; 15 is a hydrotalcite filter; 16 is a stainless steel barrel; 17 is a fourth ball valve; and 18 is a third ball valve.
Detailed Description
The invention is described in further detail below with reference to the attached drawing figures:
referring to fig. 1, the excess sludge protein extraction device disclosed by the invention comprises a reaction kettle 4, wherein excess sludge enters the reaction kettle 4 under the action of a screw pump 2, and the sludge flow is regulated by a first ball valve 1. An ultrasonic unit is arranged on the reaction kettle 4 and consists of an ultrasonic transducer 5 and an ultrasonic generator 6, and can apply acoustic cavitation to the residual sludge; an electron accelerator 3 is arranged below the reaction kettle 4 and can apply irradiation to the sludge. Under the combined action of acoustic cavitation and irradiation, the efficient cracking of the residual sludge is realized, and the release speed of sludge protein is accelerated. The cracked surplus sludge enters a horizontal centrifugal machine 9 under the action of a second screw pump 8 to carry out solid-liquid separation, and the flow is regulated by a second ball valve 7. The separated supernatant enters a stainless steel barrel 16, the flow rate is regulated by a third ball valve 18, a plurality of layers of hydrotalcite filters 15 are contained in the stainless steel barrel 16, and sludge protein enters the hydrotalcite material layers under the adsorption effect of the hydrotalcite material to form a protein intercalation hydrotalcite material. The spatial structure of the protein intercalated hydrotalcite material can be regulated by a temperature control unit and a pressure control unit, wherein the temperature control unit consists of a temperature controller 13 and a heater 14, and the pressure control unit consists of a flowmeter 10, a fifth ball valve 11 and an argon steel cylinder 12. The final filtrate is returned to the feed inlet and the flow is regulated by a fourth ball valve 17. All interfaces of the whole set of device are hermetically connected by a mechanical sealing component.
Wherein, an ultrasonic amplitude transformer is arranged on the ultrasonic transducer 5 and extends into the reaction kettle 4. The ultrasonic transducer 5 is provided with a cooling water channel, and cooling water enters the cooling water channel through a cooling water inlet and flows out of a cooling water outlet to form a water cooling system.
The irradiation dose of the electron accelerator 3 is 30kGy or less.
The bottom of the horizontal centrifuge 9 is provided with a sludge discharge port for discharging sludge and slag, and the separated sludge and slag are correspondingly regulated according to the physical and chemical property analysis result and can be used as building materials or greening soil after regulation.
The sludge protein contains-OH, -NH in the molecule 2 And polar functional groups such as-SH, which are easy to generate strong acting force with the hydrotalcite filter containing electrodeless cations and anions in the stainless steel barrel, so as to form the protein intercalated hydrotalcite material, wherein the acting force can be influenced by temperature and pressure rise and fall, and further the regulation and control of the spatial structure of the protein intercalated hydrotalcite material are realized.
The physical and chemical properties of the protein intercalated hydrotalcite material can be determined by analysis means such as XRD, FT-IR, SEM and the like, and the temperature control unit and the pressure control unit are adjusted according to the determination result.
The several layers of hydrotalcite filters provided in the stainless steel drum 16 of the present invention may be self-made by the following method:
mixing commercial magnesium aluminum hydrotalcite and polyvinyl alcohol according to a mass ratio of 1:3, taking a plurality of sponges with the inner diameter of a stainless steel barrel, soaking the sponges in the mixed solution, taking out the sponges after the sponges are saturated, drying at 55+/-2 ℃, soaking in the mixed solution, drying at 55+/-2 ℃ after the sponges are saturated, and repeating for 5 times; and finally, treating the dried sponge at 950+/-30 ℃ for 4 hours, and cooling to obtain the hydrotalcite filter.
The dye wastewater treatment device of the invention, when in use:
firstly, a first ball valve 1 is opened, a first screw pump 2 is started, excess sludge is conveyed into a reaction kettle 4 from an excess sludge tank, the sludge feeding flow is controlled by adjusting the first ball valve 1, then an ultrasonic generator 6 and an electronic accelerator 3 are started, ultrasonic wave and irradiation treatment are carried out on the sludge, a second ball valve 7 is opened after the sludge is fully broken, a second screw pump 8 is started, broken sludge solution enters a horizontal centrifuge 9 for solid-liquid separation, under the action of centrifugal force, solid sludge and sludge supernatant are separated, sludge is discharged from a sludge discharge port at the bottom of the horizontal centrifuge 9, sludge protein is dissolved into water phase, a third ball valve 18 is started, the sludge protein enters a stainless steel barrel 16, under the action of filtering by a hydrotalcite filter 15, the sludge protein enters a hydrotalcite structural gap, a fourth ball valve 17 is opened, filtrate flows out of a raw material inlet of the stainless steel barrel 16 and returns to the excess sludge tank (the whole device is subjected to rough washing after the excess sludge is diluted and the system stops running). The spatial structure of the protein intercalated hydrotalcite material can be regulated and controlled through a temperature controller 13, a heater 14, a flowmeter 10, a ball valve 11 and an argon steel cylinder 12, and the protein intercalated hydrotalcite material is subjected to XRD, FT-IR, SEM and other physicochemical property analysis, so that a temperature control unit and a pressure control unit are further regulated according to analysis results, and the required protein intercalated hydrotalcite material is obtained.
According to the invention, the stirring of the materials in the reaction kettle 4 is realized by ultrasonic waves, wherein an ultrasonic amplitude transformer is inserted under the material layer in the reaction kettle 4, so that the cracking rate is faster. During the reaction, the ultrasonic generator 6 is operated all the time to fully react the excess sludge.
According to the invention, the protein intercalated hydrotalcite material is prepared by extracting sludge protein, the temperature is controlled by a temperature controller 13 and a heater 14 on a stainless steel barrel 16, and the pressure is controlled by a flowmeter 10, a ball valve 11 and an argon steel cylinder 12, so that the spatial structure of the protein intercalated hydrotalcite material is regulated and controlled; and (3) through sampling and analyzing the protein intercalated hydrotalcite material, determining the working state in the stainless steel barrel according to the physical and chemical property analysis result of the material, and finally obtaining the required protein intercalated hydrotalcite functional material.
In summary, the invention has the following advantages:
1. according to the invention, excess sludge is taken as a raw material, the excess sludge is broken through the irradiation of ultrasonic waves and electron beams, sludge proteins are released, sludge proteins entering a water phase pass through a stainless steel barrel, and enter a hydrotalcite structure under the adsorption action of a hydrotalcite filter in the stainless steel barrel to form a protein intercalated hydrotalcite material, and the structure of the protein intercalated hydrotalcite material can be regulated and controlled by a temperature control system and a pressure regulating system. The device can achieve the cracking of the excess sludge and obtain the protein intercalated hydrotalcite functional material, which can be said to be double.
2. According to the invention, the sludge can be efficiently cracked without adding any chemical agent in the treatment process of the surplus sludge, the obtained sludge protein has low molecular damage degree, does not contain chemical agent, does not use complex subsequent separation procedures, and reduces environmental burden.
3. The device can realize the reduction treatment and the recycling of the excess sludge, the prepared protein intercalated hydrotalcite material can also increase the economic benefit of the treatment process, the treatment cost is obviously reduced, the device realizes the reduction, recycling and stabilization treatment of the excess sludge, and the device positively corresponds to the call of national energy conservation and emission reduction.
Claims (6)
1. The method for extracting sludge protein and simultaneously preparing protein intercalated hydrotalcite material is characterized by comprising a reaction kettle (4), a horizontal centrifuge (9) and a stainless steel barrel (16), wherein a discharge hole of a surplus sludge tank is connected with the reaction kettle (4) through a pipeline, and a first ball valve (1) and a first screw pump (2) are arranged on the pipeline; the discharge port of the reaction kettle (4) is connected with the feed port of the horizontal centrifuge (9) through a pipeline, and a second ball valve (7) and a second screw pump (8) are arranged on the pipeline; the liquid outlet of the horizontal centrifuge (9) is connected with the liquid inlet of the stainless steel barrel (16) through a pipeline, and a third ball valve (18) is arranged on the pipeline; the filtrate outlet of the stainless steel barrel (16) is connected to the residual sludge tank through a pipeline, and a fourth ball valve (17) is arranged on the pipeline;
an ultrasonic unit capable of applying cavitation to the residual sludge is arranged at the upper end of the reaction kettle (4), and an electron accelerator (3) capable of applying irradiation to the residual sludge is arranged at the lower end of the reaction kettle (4); a stainless steel barrel (16) is filled with a plurality of layers of hydrotalcite filters (15);
the hydrotalcite filter (15) is produced by the following method:
mixing magnesium aluminum hydrotalcite and polyvinyl alcohol according to a mass ratio of 1:3 to obtain a mixed solution; taking a plurality of sponges with the same inner diameter size of a stainless steel barrel, soaking the sponges in the mixed solution, taking out the sponges after the sponges are saturated, drying at 55+/-2 ℃, and repeatedly soaking and drying for 5 times; treating the sponge dried for the last time at 950+/-30 ℃ for 4 hours, and cooling to obtain a hydrotalcite filter (15);
the method for extracting sludge protein and simultaneously preparing the protein intercalated hydrotalcite material comprises the following steps:
1) Opening a first ball valve (1) and a first screw pump (2), conveying the residual sludge in the residual sludge tank to a reaction kettle (4), and regulating the sludge feeding flow through the first ball valve (1);
2) Starting an ultrasonic unit and an electron accelerator (3) to carry out ultrasonic wave and irradiation treatment on sludge, opening a second ball valve (7) and a second screw pump (8) after the sludge is fully broken, enabling a broken sludge solution to enter a horizontal centrifuge (9) for solid-liquid separation, separating solid sludge from sludge supernatant under the action of centrifugal force, discharging sludge, and dissolving sludge protein into a water phase;
3) And starting a third ball valve (18) to enable sludge protein to enter a stainless steel barrel (16), enabling the sludge protein to enter a hydrotalcite structural gap under the adsorption and filtration effects of a hydrotalcite filter (15), opening a fourth ball valve (17) to enable filtrate to flow out of the stainless steel barrel (16) and return to a raw material inlet of a residual sludge tank, and collecting solid matters in the hydrotalcite filter (15), namely protein intercalated hydrotalcite materials.
2. The method for extracting sludge proteins and simultaneously preparing protein intercalated hydrotalcite material according to claim 1, wherein a temperature control unit and a pressure control unit are arranged outside the stainless steel barrel (16);
the temperature control unit comprises a heater (14) and a temperature controller (13) connected with the heater (14);
the pressure control unit comprises an argon steel cylinder (12) connected with a stainless steel barrel (16) through a pipeline, and a fifth ball valve (11) and a flowmeter (10) are arranged on the pipeline;
the spatial structure of the protein intercalated hydrotalcite material can be regulated and controlled by a temperature control unit and a pressure control unit which are arranged outside the stainless steel barrel (16).
3. The method for extracting sludge proteins and simultaneously preparing protein intercalated hydrotalcite material according to claim 1, wherein the ultrasonic unit consists of an ultrasonic transducer (5) and an ultrasonic generator (6), and the ultrasonic transducer (5) and the ultrasonic generator (6) are electrically connected; an ultrasonic amplitude transformer on the ultrasonic transducer (5) can extend into the reaction kettle (4).
4. The method for extracting sludge proteins and simultaneously preparing protein intercalated hydrotalcite materials according to claim 3, wherein the ultrasonic transducer (5) is also provided with a cooling water channel, and the cooling water enters the cooling water channel through a cooling water inlet and flows out from a cooling water outlet to form a water cooling system.
5. The method for extracting sludge proteins and simultaneously preparing protein intercalated hydrotalcite materials according to claim 1, characterized in that a sludge discharge port for removing sludge is arranged at the bottom of the horizontal centrifuge (9).
6. The method for extracting sludge proteins and simultaneously preparing protein intercalated hydrotalcite material according to claim 1, wherein the irradiation dose of the electron accelerator (3) is below 30 kGy.
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| CN110950511B (en) * | 2018-09-26 | 2022-07-15 | 中国石油化工股份有限公司 | System and method for treating excess biochemical sludge |
| CN109233862B (en) * | 2018-11-09 | 2020-10-30 | 榆林学院 | Soil remediation agent and preparation method and use method thereof |
| CN110776925B (en) * | 2019-11-20 | 2021-10-08 | 榆林学院 | Water-retaining agent prepared from excess sludge, and preparation method and application method thereof |
| CN111099799A (en) * | 2020-01-07 | 2020-05-05 | 沧州信昌化工股份有限公司 | Preprocessing device for dirty oil sludge |
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