CN110759453B - Method for removing ammonia nitrogen from biogas slurry - Google Patents
Method for removing ammonia nitrogen from biogas slurry Download PDFInfo
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- CN110759453B CN110759453B CN201910725927.4A CN201910725927A CN110759453B CN 110759453 B CN110759453 B CN 110759453B CN 201910725927 A CN201910725927 A CN 201910725927A CN 110759453 B CN110759453 B CN 110759453B
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/586—Treatment of water, waste water, or sewage by removing specified dissolved compounds by removing ammoniacal nitrogen
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
- C01B25/451—Phosphates containing plural metal, or metal and ammonium containing metal and ammonium
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Abstract
The invention discloses a method for removing ammonia nitrogen from biogas slurry, which comprises the steps of regulating pH of the biogas slurry, feeding the biogas slurry into a first liquid mixer, adding magnesium salt to form crystal nuclei, and growing the crystal nuclei in at least two parallel liquid mixers to generate struvite precipitate. The method can realize the online ammonia nitrogen concentration regulation and control of the biogas engineering, the obtained magnesium ammonium phosphate particles with large particle size can be separated by precipitation, and the online adding mode of the invention reduces the using amount of the medicament and reduces the cost.
Description
Technical Field
The invention belongs to the technical field of wastewater treatment and recycling, and particularly relates to a method for removing ammonia nitrogen in biogas slurry.
Background
Billions of tons of poor biomass are produced in China every year, the resource utilization rate is low, and various policies of China are developed to develop biogas engineering to solve the problems of poor biomass treatment and resource utilization. However, the problem of biogas slurry treatment is difficult to solve after the development of biogas engineering is more and more robust. The biogas slurry as anaerobic fermentation liquid has extremely many components and complex physical properties, and is mainly reflected in high enrichment of COD and ammonia nitrogen and residues of humic acid and heavy metals.
The biogas slurry has huge yield, billions of tons of annual output in China, is difficult to be absorbed by soil and has long-term harm to the soil when being directly returned to the field, and is directly and efficiently treated, the cost is extremely high, the treatment cost per ton reaches hundreds of yuan, and the common biogas engineering is difficult to bear. If high ammonia nitrogen in the biogas slurry is treated and reused in fermentation, the pressure for biogas slurry treatment can be greatly reduced, and nitrogen in the system can be effectively controlled and recovered.
The existing denitrification technology comprises a biological method, an air stripping method, an ion exchange method, a breakpoint chlorination method and a chemical precipitation method, and the methods have advantages and disadvantages and different application conditions. The biological method has large occupied area and higher requirements on temperature and pH; the addition amount of alkali liquor in the stripping method is too large, and a certain heat source is required; the material usage of the ion exchange method is too large; the breakpoint chlorination method has high treatment efficiency, but only aims at the wastewater with low ammonia nitrogen concentration. Aiming at the biogas slurry with high ammonia nitrogen concentration (500-.
The application of the prior magnesium ammonium phosphate precipitation method in engineering practice has great problems, mainly the dosing cost is high, and imperfect problems exist in a crystallization device and a process flow, so that the efficiency of recovering ammonia nitrogen in biogas slurry is influenced. In many patents related to struvite precipitation (struvite), synthetic ammonia wastewater is treated by a struvite cyclic crystallization method (Chinese patent 201110260178.6), struvite is recovered from sludge (Chinese patent 201620118743.3), ammonia nitrogen wastewater is treated by a coagulation precipitation and struvite crystallization combined method (Chinese patent 201620118743.3) and the like, and ammonia nitrogen process is not regulated and controlled from the kinetic angle of nucleation and crystallization growth, so that the ammonia nitrogen removal rate in the actual application process is not high, and ideal crystal particle size distribution is difficult to obtain. The particle size and the crystal solubility are closely related, and the removal rate of ammonia nitrogen and the crystal quality are indirectly influenced. The smaller the crystal particle size, the greater the solubility. Therefore, the particle size in the precipitation process of magnesium ammonium phosphate is effectively controlled, and the key points of reducing the addition of the medicament, namely reducing the treatment cost and improving the removal rate of ammonia nitrogen are achieved.
Disclosure of Invention
The invention aims to provide a method for removing ammonia nitrogen from biogas slurry, which is used for solving the problems that the existing biogas slurry is difficult to treat and the magnesium ammonium phosphate precipitation method is difficult to industrially apply.
The invention is realized by the following technical scheme:
a method for removing ammonia nitrogen from biogas slurry comprises the steps of regulating pH of the biogas slurry, feeding the biogas slurry into a first liquid mixer, adding magnesium salt to form crystal nuclei, and growing the crystal nuclei in at least two liquid mixers connected in parallel to generate struvite precipitate.
According to the invention, the nucleation growth kinetics of a struvite precipitation method is accurately regulated and controlled by the first liquid mixer, then the at least two parallel liquid mixers and the form of connecting the struvite mixers in series and then connecting the struvite mixers in parallel, so that the multilevel precipitation of struvite is realized, magnesium ammonium phosphate particles with the particle size of more than 50% and more than 100 micrometers are obtained, and the ammonia nitrogen concentration of the biogas slurry subjected to single circulation treatment is reduced to 90-95% of the original ammonia nitrogen concentration. The magnesium ammonium phosphate particles are applied as a slow release fertilizer, a certain particle size requirement needs to be met, the larger average particle size reduces the contact area between the particles and the soil and the atmosphere, the nutrient loss in the interaction process of the particles and the soil is reduced or delayed, the diffusion range and the fertilizer supply strength are influenced by the overlarge particle size, and the 100-micron struvite precipitate formed by the method is the size of the applicable magnesium ammonium phosphate slow release fertilizer. In addition, the uniform particle size distribution also enables the nutrient supply in the fertilization process to be smooth and is an important index for evaluation of the slow release fertilizer, and the particle size distribution formed by the method is uniform.
In one embodiment, a part of the biogas slurry after the crystal nucleus growth can flow back to the fermentation system to be used as fermentation water, and the other part of the biogas slurry can flow out to be used as organic fertilizer.
In one embodiment, the number of the liquid mixers connected in parallel is 2 to 5, preferably 2 to 3.
In one embodiment, the residence time of the biogas slurry in the first liquid mixer is controlled to be 15-30 seconds, the flow rate of the biogas slurry is controlled to be 0.25-0.5 m/s, and the Reynolds number Re is controlled to be more than 3500, preferably more than 4000, more preferably 4000-6000, and further preferably 4000-5000. The low residence time and high turbulence in the first liquid mixer allow a significant increase in the nucleation rate of the crystals.
In one embodiment, the residence time in at least two parallel liquid mixers is controlled to be 50-60 seconds, the biogas slurry flow rate is controlled to be 0.1-0.2 m/s, and the Reynolds number Re is controlled to be less than 2000, preferably 1000-2000. In the stage, the growth of the crystal is slowly regulated, and the supersaturation degree of the reaction is controlled through the regulation of kinetic parameters, so that the crystal effectively grows, and secondary nucleation can be avoided.
In one embodiment, the pH is adjusted to be 8-9, preferably 8.5. The pH value in the first liquid mixer and the liquid mixers connected in parallel is 8-10, preferably 9.0, and the alkali for adjusting the pH value can be alkali commonly used in the field, such as one or more of sodium hydroxide, calcium hydroxide or quicklime.
In one embodiment, the magnesium salt is added in an amount of 3-4 kg/t. The invention can effectively control the particle size in the precipitation process of magnesium ammonium phosphate, thereby reducing the addition of the medicament, namely reducing the treatment cost.
The magnesium salt added in the invention can be a magnesium salt commonly used in the art, and in one embodiment, can be one or more of magnesium sulfate, magnesium chloride or magnesium hydroxide.
In one embodiment, when the biogas slurry passes through at least two liquid mixers connected in parallel, the circulation ratio of the biogas slurry is 0.6-0.8. The circulation ratio is the ratio of the amount of the circulating material to the amount of the fresh raw material, and R is VR/V0。
The invention also provides a device for removing ammonia nitrogen from biogas slurry, which comprises a fermentation tank, a buffer tank, a first liquid mixer and at least two liquid mixers connected in parallel; the inlet of the buffer pool is connected with the liquid outlet of the fermentation tank, the outlet of the buffer pool is connected with the first liquid mixer, and the outlet of the first liquid mixer is connected with at least two liquid mixers connected in parallel.
The main flow of the ammonia nitrogen removal of the biogas slurry in the device is that the biogas slurry from a fermentation tank can enter a buffer tank through a conventional mode such as a water pump, after the pH and the medicament are regulated and controlled in the buffer tank, introducing the biogas slurry into a first liquid mixer, adding a small amount of magnesium salt into the liquid mixer to form a large amount of crystal nuclei in the biogas slurry, then carrying out crystal nucleus growth in two subsequent liquid mixers to generate large-particle struvite sediment, wherein one part of the treated biogas slurry can flow back into a fermentation tank to be used as fermentation water, and the other part of the treated biogas slurry can flow out of a system to be used as an organic fertilizer, the method is characterized in that a plurality of liquid mixers are connected in series and then in parallel, so that the nucleation growth dynamics of a struvite precipitation method is accurately regulated and controlled, the multistage precipitation of struvite is realized, more than 60% of magnesium ammonium phosphate particles with the particle size of more than 100 micrometers are obtained, and the ammonia nitrogen concentration of the biogas slurry subjected to single circulation treatment is reduced to 90-95% of the original ammonia nitrogen concentration. The magnesium ammonium phosphate particles are applied as a slow release fertilizer, a certain particle size requirement needs to be met, the larger average particle size reduces the contact area between the particles and the soil and the atmosphere, the nutrient loss in the interaction process of the particles and the soil is reduced or delayed, the diffusion range and the fertilizer supply strength are influenced by the overlarge particle size, and the struvite sediment with the particle size of 100 micrometers prepared by the invention is the particle size of the applicable magnesium ammonium phosphate slow release fertilizer. In addition, the uniform particle size distribution also enables the nutrient supply in the fertilization process to be smooth, and the uniform particle size distribution is an important index for evaluation of the slow release fertilizer.
The equipment provided by the invention can also be provided with a pH on-line monitor and an ammonia nitrogen on-line monitor in the buffer tank, and a pH agent dosing pump, a pH regulator storage tank, a phosphate dosing pump and a phosphate storage tank, and can regulate and control the biogas slurry through the pH agent dosing pump, the pH regulator storage tank, the phosphate dosing pump and the phosphate storage tank, so that the purpose of subsequent crystallization of the biogas slurry is achieved.
In the invention, a pH on-line monitor and an ammonia nitrogen on-line monitor can be arranged in the first liquid mixer and the liquid mixers connected in parallel, a pH agent dosing pump and a pH regulator storage tank are arranged, and alkali liquor can be added in front of each mixer according to the ammonia nitrogen concentration and the pH value of the biogas slurry through the pH agent dosing pump and the pH regulator storage tank.
In one embodiment, the first liquid mixer of the present invention is further provided with a magnesium salt dosing pump and a magnesium salt storage tank, and magnesium salt can be added to form crystal nuclei.
In one embodiment, the parallel liquid mixers of the present invention may be connected to a settling tank.
The first liquid mixer and the parallel liquid mixers in the invention can be enumerated by the types including but not limited to one or more of a porous cross-flow jet mixer, a hydrodynamic cavitation mixer, a micro-fluidic chip rapid mixer, a self-suction liquid mixer, a high-viscosity liquid mixer, a regular hexagon twisted tube mixer or a hydrodynamic liquid mixer.
In one embodiment, when the biogas slurry flows through the first liquid mixer, the residence time of the biogas slurry in the liquid mixer is controlled to be 15-30 seconds, the flow rate of the biogas slurry is controlled to be 0.25-0.5 m/s, and the Reynolds number Re is controlled to be more than 3500, preferably more than 4000, more preferably 4000-6000, and further preferably 4000-5000. The low residence time and high turbulence provide a significant increase in the nucleation rate of the crystals.
In one embodiment, when biogas slurry flows through the parallel liquid mixers, the residence time of the biogas slurry in the parallel liquid mixers is controlled to be 50-60 seconds, the flow rate of the biogas slurry is controlled to be 0.1-0.2 m/s, and the Reynolds number Re is controlled to be below 2000, preferably 1000-2000. The growth of the crystal is slowly regulated, and the supersaturation degree of the reaction is controlled through the regulation of kinetic parameters, so that the crystal effectively grows, and secondary nucleation is avoided.
In one embodiment, when biogas slurry flows through the parallel liquid mixers, the circulation ratio of the biogas slurry is 0.6-0.8. The circulation ratio is the ratio of the amount of the circulating material to the amount of the fresh raw material, and R is VR/V0。
The high ammonia nitrogen in the biogas slurry is efficiently removed by an ammoniomagnesium phosphate precipitation method after the biogas slurry is treated by the parallel liquid mixers, so that the treated biogas slurry can be directly reused for fermentation or can flow out to be applied as an organic fertilizer.
The invention has the beneficial effects that:
(1) in the biogas slurry ammonia nitrogen regulation and control process, the concentration of ammonia nitrogen in biogas slurry subjected to single-cycle treatment is reduced to 90-95% of the original concentration.
(2) In the biogas slurry ammonia nitrogen regulation and control process, more than 60% of magnesium ammonium phosphate particles with the particle size of more than 100 microns can be finally obtained.
(3) In the ammonia nitrogen regulation and control process of the biogas slurry, the high ammonia nitrogen in the biogas slurry can be greatly reduced, the high ammonia nitrogen in the biogas slurry is recycled, and the fermentation water is reduced.
(4) The online ammonia nitrogen concentration regulation and control of the biogas engineering can be realized, the obtained magnesium ammonium phosphate particles with large particle size can be separated through precipitation, and the online adding mode of the invention reduces the usage amount of the medicament and reduces the cost.
Drawings
FIG. 1 is a flow chart of a biogas slurry ammonia nitrogen regulation system process;
FIG. 2 is a graph showing a particle size distribution of an struvite precipitate;
FIG. 3 is an electron micrograph of an struvite precipitate;
FIG. 4 is an XRD diffractogram of the struvite precipitate.
Detailed Description
The present invention will be further described with reference to the following examples, which are intended to illustrate the present invention and not to limit the scope of the present invention, and all simple modifications of the preparation method of the present invention based on the idea of the present invention are within the scope of the present invention. The following examples are experimental methods without specifying specific conditions, and generally follow the methods known in the art. The test materials used in the following examples were purchased from a conventional biochemical reagent store unless otherwise specified.
Example 1
The implementation provides a device for removing ammonia nitrogen from biogas slurry, which comprises a fermentation tank 1, a buffer tank 3, a first liquid mixer 4, and at least two liquid mixers 5 and 6 connected in parallel; the inlet of the buffer pool 3 is connected with the liquid outlet of the fermentation tank 1 through a water pump 2, the outlet of the buffer pool 3 is connected with a first liquid mixer 4, and the outlet of the first liquid mixer 4 is connected with at least two liquid mixers 5 and 6 which are connected in parallel (figure 1).
The serial-parallel connection mode of the liquid mixers is that two liquid mixers are connected in parallel behind a single liquid mixer, the biogas slurry residence time in the front-stage process is 15 seconds, the Reynolds number Re is 4800, the biogas slurry residence time in the rear-stage process is 55 seconds, the Reynolds number Re is 2000, and the circulation ratio is 0.6.
Struvite is a crystallization process in which magnesium protophosphate and nitrogen protophosphate form magnesium ammonium phosphate crystals under certain conditions, i.e., struvite. Crystallization mainly includes two processes of nucleation and growth, and when the supersaturation in the liquid phase reached the crystal and appeared required solubility product, the crystal nucleus will appear, then the inverse relation of supersaturation and crystal nucleus size, and the supersaturation is big more, and the crystal nucleus is less, and the crystal nucleus quantity is more for the size of crystal is difficult to grow up, consequently needs to have accurate regulation and control to its supersaturation of nucleation growth to the amplification technology of guano stone method. This patent is through the process of the series-parallel connection of a plurality of liquid state blenders separately regulation and control of nucleation and growth, realizes a large amount of nucleation through high turbulence degree and short dwell time in the front section technology, and the back section technology is shunted through natural pond liquid and is circulated realization high dwell time, and control crystal nucleus is grown.
And (3) characterizing the treated biogas slurry under the condition, and analyzing the residual ammonia nitrogen concentration in the biogas slurry by using an ammonia nitrogen online monitor, thereby obtaining the ammonia nitrogen removal rate of the biogas slurry. The precipitate magnesium ammonium phosphate was analyzed for particle size to obtain an average particle size, the results are shown in FIG. 2; and the results are shown in figure 3 and figure 4 through the characterization of SEM and XRD.
TABLE 1 operating conditions and characterization results for the examples
As can be seen from the above table, in examples 1 to 7, a plurality of experiments were performed by adjusting the process parameters of the liquid mixer and the hydrodynamic parameters in biogas slurry treatment, and the results found that different lengths of the liquid mixer, the retention time of the biogas slurry and the reynolds number Re have different effects on the biogas slurry treatment effect, and are directly reflected in the changes of the final ammonia nitrogen removal rate and the particle size distribution, and the optimal process conditions are that, in the serial-parallel connection mode of the liquid mixers, the retention time of the biogas slurry in the front stage is 20 seconds, the reynolds number Re is 4200, the retention time of the biogas slurry in the rear stage is 60 seconds, the reynolds number Re is 1200, and the circulation ratio is 0.8, but the ammonia nitrogen removal rate can be up to 91% or more, the percentage of particles with a particle size greater than 100 μm is 61% or more, and the effect is significantly better than that of the comparative example.
Comparative example 1 and example, it can be seen that the effect of a single liquid mixer is much less than the series-parallel connection of multiple mixers, because it is difficult to precisely control the nucleation and growth of crystals by a single liquid mixer, and different supersaturations required for nucleation and growth cannot be provided, resulting in low ammonia nitrogen removal rate and difficult growth of crystal particles. In the same way as in comparative example 2, in the crystal growth stage, the low supersaturation degree needs to be controlled, and the crystal growth effect is influenced due to the fact that the low supersaturation degree needs to be controlled and the low supersaturation degree can not be achieved due to simple series connection.
Comparative examples 3 to 4, the parallel connection of a plurality of liquid mixers, or the parallel connection and the serial connection are not beneficial to the nucleation process of crystallization, so that the local supersaturation degree can not meet the requirement of mass nucleation, and the obtained effect is lower than that of the examples.
Comparative example 5 is traditional kettle-type crystallization mixer, and the effect is poor, and the energy consumption is big, mainly reflects in mixing inhomogeneous, very easily appears the local supersaturation too big, the problem of excessive nucleation, finally leads to the ammonia nitrogen clearance low, and the average particle size of crystal is little, is difficult to separate.
Although the invention has been described in detail with respect to the general description and the specific embodiments, it will be apparent to those skilled in the art that modifications or improvements may be made thereto without departing from the spirit of the invention.
Claims (16)
1. A method for removing ammonia nitrogen from biogas slurry is characterized in that the biogas slurry enters a first liquid mixer after pH regulation, magnesium salt is added to form crystal nuclei, and then the crystal nuclei grow in at least two parallel liquid mixers to generate struvite sediment; the residence time of the biogas slurry in the first liquid mixer is controlled to be 15-30 seconds, the flow rate of the biogas slurry is controlled to be 0.25-0.5 m/s, and the Reynolds number Re is controlled to be more than 3500; the residence time in at least two parallel liquid mixers is controlled to be 50-60 seconds, the flow rate of the biogas slurry is controlled to be 0.1-0.2 m/s, and the Reynolds number Re is controlled to be below 2000.
2. The method according to claim 1, wherein the number of the liquid mixers connected in parallel is 2 to 5.
3. The method according to claim 2, wherein the number of the liquid mixers connected in parallel is 2 to 3.
4. The method as claimed in claim 1, wherein the reynolds number Re of the biogas slurry in the first liquid mixer is controlled to 4000 or more.
5. The method as claimed in claim 4, wherein the Reynolds number Re of the biogas slurry in the first liquid mixer is controlled to 4000 to 6000.
6. The method as claimed in claim 5, wherein the Reynolds number Re of the biogas slurry in the first liquid mixer is controlled to 4000 to 5000.
7. The method of claim 1, wherein the Reynolds number Re is controlled to be 1000 to 2000 in at least two liquid mixers connected in parallel.
8. The method according to claim 1, wherein the pH is adjusted to a pH of 8 to 9; the pH value of the first liquid mixer and the liquid mixers connected in parallel is 8-10, and the alkali for adjusting the pH value is one or more of sodium hydroxide, calcium hydroxide or quick lime; adding 3-4 kg/t of magnesium salt; the magnesium salt is one or more of magnesium sulfate or magnesium chloride; when the biogas slurry passes through at least two liquid mixers connected in parallel, the circulation ratio of the biogas slurry is 0.6-0.8.
9. The device for the method for removing ammonia nitrogen from biogas slurry according to claim 1, which is characterized by comprising a fermentation tank, a buffer tank, a first liquid mixer and at least two liquid mixers connected in parallel; the inlet of the buffer pool is connected with the liquid outlet of the fermentation tank, the outlet of the buffer pool is connected with the first liquid mixer, and the outlet of the first liquid mixer is connected with at least two liquid mixers connected in parallel.
10. The device according to claim 9, wherein the buffer tank is provided with an online pH monitor and an online ammonia nitrogen monitor, and is provided with a pH regulator dosing pump, a pH regulator storage tank, a phosphate dosing pump and a phosphate storage tank; a pH on-line monitor and an ammonia nitrogen on-line monitor are also arranged in the first liquid mixer and the liquid mixers connected in parallel, and a pH regulator dosing pump and a pH regulator storage tank are also arranged; the first liquid mixer is also provided with a magnesium salt dosing pump and a magnesium salt storage tank.
11. The apparatus of claim 9, wherein the first liquid mixer and the parallel liquid mixers are one or more of a porous cross-flow jet ejector mixer, a hydrodynamic cavitation mixer, a microfluidic chip flash mixer, a self-priming liquid mixer, a high viscosity liquid mixer, a regular hexagonal twisted tube mixer, or a hydrodynamic liquid mixer.
12. The apparatus as claimed in claim 9, wherein the reynolds number Re of the biogas slurry in the first liquid mixer is controlled to be more than 4000.
13. The apparatus as claimed in claim 12, wherein the Reynolds number Re of the biogas slurry in the first liquid mixer is controlled to 4000-6000.
14. The apparatus as claimed in claim 13, wherein the Reynolds number Re of the biogas slurry in the first liquid mixer is controlled to 4000-5000.
15. The apparatus of claim 9, wherein the Reynolds number Re is controlled to be 1000 to 2000 in at least two liquid mixers connected in parallel.
16. The apparatus of claim 9, wherein the parallel liquid mixers are connected to a settling tank; when biogas slurry flows through the parallel liquid mixers, the circulation ratio of the biogas slurry is 0.6-0.8.
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