CN109593001A - A kind of method of leather waste water efficient denitrification production efficient compound fertilizer - Google Patents
A kind of method of leather waste water efficient denitrification production efficient compound fertilizer Download PDFInfo
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- CN109593001A CN109593001A CN201811502582.8A CN201811502582A CN109593001A CN 109593001 A CN109593001 A CN 109593001A CN 201811502582 A CN201811502582 A CN 201811502582A CN 109593001 A CN109593001 A CN 109593001A
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- waste water
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- magnesium
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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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Abstract
The present invention relates to a kind of method of leather waste water efficient denitrification production efficient compound fertilizer, it is characterized in that including the following steps: that the biological carbon material for loading magnesium and phosphate anion is placed in H by (1)3PO4After impregnating 12h in solution, activated material is obtained after being filtered, washed, drying, it is spare；(2) activated material of step (1) preparation is added into waste water, after stirring 1h, precipitating, dry product are collected in filtering；(3) product that step (2) obtains is uniformly mixed with ammonium magnesium phosphate with mass ratio 1:3-1:5 to get efficient compound fertilizer.
Description
Technical field
The invention belongs to wastewater treatments to recycle field, and in particular to a kind of leather waste water efficient denitrification production high efficiency composition
The method of fertilizer.
Background technique
The ammonia and nitrogen pollution that leather waste water treatment process generates is mainly from two aspects first is that being added in process
Various ammonium salts；Second is that be transformed by leather organic nitrogen itself.Process in waste water containing ammonia nitrogen have immersion, depilation, tanning, in
With the processes such as dyeing, wherein in deashing and softening using ammonium sulfate, ammonium chloride etc. in and dyeing process also uses ammonium hydrogen carbonate
And liquefied ammonia；And the ammonia nitrogen in pickling and tanning processes then in leather ammonium salt residue continuous release.Due to process hides raw material
In Animal Skin itself with many ammonia nitrogens, the Some Animals protein in processing in original skin will divide in process
It separates out and, constantly decompose and generate more ammonia nitrogen.The processing method of leather-making waste water mostly uses greatly materialization, biochemistry or both at present
The process flow combined.It is wherein added into nitrogen-containing wastewater and contains Mg2+、PO4 3-Reagent, produce MgNH4PO4, but should
Method is to Mg2+、NH4 +、PO4 3-Ratio have a strict demand, reagent dosage is few, cannot be removed effectively the ammonia nitrogen in waste water,
Additional amount will cause secondary pollution.Therefore, developing a kind of can be released effectively Mg2+、PO4 3-Biological carbon material be used for waste water
Denitrogenation becomes a problem.
Summary of the invention
The present invention provides a kind of method of waste water high-efficiency denitrogenation production efficient compound fertilizer, it is characterised in that including walking as follows
It is rapid:
(1) activation of the biological carbon material of magnesium and phosphate anion is loaded:
The biological carbon material for loading magnesium and phosphate anion is placed in H3PO4After impregnating 12h in solution, it is filtered, washed, does
Activated material is obtained after dry, it is spare；
(2) activated material of step (1) preparation is added into waste water, after stirring 1h, precipitating is collected in filtering, so dry that produce
Product；
(3) product that step (2) obtains is uniformly mixed with ammonium magnesium phosphate with mass ratio 1:3-1:5 to get high efficiency composition
Fertilizer.
H described in step (1)3PO4The concentration of solution is 3-6mol/L；Waste water described in step (2) is nitrogen-containing wastewater,
The dosage of activated material is that 200mg activated material is used in every 100mL waste water.
Another embodiment of the present invention provides a kind of efficient compound fertilizer, it is characterised in that the efficient compound fertilizer is by ingredient
1 and ammonium magnesium phosphate be mixed with mass ratio 1:3-1:5；The preparation method of the ingredient 1 includes the following steps:
(1) activation of the biological carbon material of magnesium and phosphate anion is loaded:
The biological carbon material for loading magnesium and phosphate anion is placed in H3PO4After impregnating 12h in solution, it is filtered, washed, does
Activated material is obtained after dry, it is spare；
(2) activated material of step (1) preparation is added into waste water, after stirring 1h, precipitating is collected in filtering, it is dry at
Divide 1.
H described in step (1)3PO4The concentration of solution is 3-6mol/L；Waste water described in step (2) is nitrogen-containing wastewater,
The dosage of activated material is that 200mg activated material is used in every 100mL waste water.
The preparation method of the biological carbon material of load magnesium and phosphate anion of the present invention includes the following steps:
(1) dried yeast powder and glucose are dissolved in deionized water, after cultivating 0.5-1.0h at 30-35 DEG C, are centrifuged, go
Ion water washing obtains saccharomycete；
(2) MgCl is added in the saccharomycete that step (1) obtains2Solution and H3PO4Solution after stirring 0.5h, rises at room temperature
Temperature is to 170-180 DEG C, and after reacting 5-8h, centrifugation, drying, grinds to obtain presoma at deionized water washing；
(3) presoma that step (2) obtains is placed in tube furnace, under nitrogen protection, with the heating speed of 10 DEG C/min
After rate rises to 800 DEG C of calcining 4h, restore the biological carbon material to room temperature to get the load magnesium and phosphate anion.
The preferred 1:2 of the mass ratio of dried yeast powder and glucose in step (1), every gram of dried yeast powder use 100mL deionization
Water；
MgCl in step (2)2Solution and H3PO4The concentration of solution is 1mol/L, and dosage is that every gram of dried yeast powder uses
MgCl2Solution 100mL, uses H3PO4Solution 100mL；The reaction of step (2) preferably carries out in a high pressure reaction kettle.
Another embodiment of the present invention provides the biological carbon material of above-mentioned load magnesium and phosphate anion in denitrogenation of waste water
Produce the application in efficient compound fertilizer.
Compared with the prior art, the advantages of the present invention are as follows: (1) present invention using spherical or elliposoidal saccharomycete as template
Agent and biological carbon source, yeast cell wall are made of a large amount of protein and polysaccharide, so that saccharomycete has big point of many biologies
Son and surface charge, these large biological molecules and surface charge and metal ion or charged ion faciation interaction, excitation deposition,
The core site of orientation is provided, fixed ion ultimately forms microspheroidal structure.The COOH of cell wall and cell interior?、OH?、NH4 +
With hydrophily, the mineralization ability of saccharomycete can be improved, adjust the nucleation and growth of crystal, ferment is assembled by electrostatic interaction
Mother cell wall surface and cell interior；Calcining, H after hydro-thermal3PO4Solution impregnates can be released effectively Mg to obtain the final product2+、PO4 3-Biological carbon
Material.(2) ion load type biology carbon material prepared by the present invention is while denitrogenation of waste water, moreover it is possible to effective dephosphorization.(3) this hair
The precipitating obtained after the reason waste water of daylight can be used as additive and ammonium magnesium phosphate is mixed for preparing efficient compound fertilizer.
Specific embodiment
For the ease of a further understanding of the present invention, examples provided below has done more detailed description to it.But
It is that these embodiments are only not supposed to be a limitation to the present invention or implementation principle for better understanding invention, reality of the invention
The mode of applying is not limited to the following contents.Dried yeast powder used in the embodiment of the present invention is (high purchased from Angel Yeast Co., Ltd
Active dry yeast).
Embodiment 1
(1) dried yeast powder (100g) and glucose (200g) is dissolved in deionized water (10L), cultivates 1.0h at 30 DEG C
Afterwards, centrifugation, deionized water wash to obtain saccharomycete；
(2) MgCl is added in the saccharomycete that step (1) obtains2Solution (10L, 1mol/L) and H3PO4Solution (10L, 1mol/
L), at room temperature, after stirring 0.5h, 180 DEG C are warming up to, after reacting 5h, centrifugation, drying, grinds to obtain forerunner at deionized water washing
Body；
(3) presoma that step (2) obtains is placed in tube furnace, under nitrogen protection, with the heating speed of 10 DEG C/min
It is (following to get the biological carbon material of the load magnesium and phosphate anion after restoring to room temperature after rate rises to 800 DEG C of calcining 4h
Abbreviation product A).
Embodiment 2
(1) dried yeast powder (100g) and glucose (200g) is dissolved in deionized water (10L), cultivates 0.5h at 35 DEG C
Afterwards, centrifugation, deionized water wash to obtain saccharomycete；
(2) MgCl is added in the saccharomycete that step (1) obtains2Solution (10L, 1mol/L) and H3PO4Solution (10L, 1mol/
L), at room temperature, after stirring 0.5h, 170 DEG C are warming up to, after reacting 8h, centrifugation, drying, grinds to obtain forerunner at deionized water washing
Body；
(3) presoma that step (2) obtains is placed in tube furnace, under nitrogen protection, with the heating speed of 10 DEG C/min
It is (following to get the biological carbon material of the load magnesium and phosphate anion after restoring to room temperature after rate rises to 800 DEG C of calcining 4h
Abbreviation product B).
Embodiment 3
(1) dried yeast powder (100g) and glucose (200g) is dissolved in deionized water (10L), cultivates 1.0h at 30 DEG C
Afterwards, centrifugation, deionized water wash to obtain saccharomycete；
(2) MgCl is added in the saccharomycete that step (1) obtains2Solution (10L, 0.1mol/L) and H3PO4Solution (10L,
0.1mol/L), at room temperature, after stirring 0.5h, 180 DEG C are warming up to, after reacting 5h, centrifugation, deionized water washing, dry, grinding
Obtain presoma；
(3) presoma that step (2) obtains is placed in tube furnace, under nitrogen protection, with the heating speed of 10 DEG C/min
After rate rises to 800 DEG C of calcining 4h, after restoring to room temperature (hereinafter referred to as to get the biological carbon material of load magnesium and phosphate anion
Products C).
Embodiment 4 loads the activation of the biological carbon material of magnesium and phosphate anion
Product A (10g) is taken to be placed in H3PO4After impregnating 12h in solution (3mol/L), material must be activated after being filtered, washed, drying
Expect (hereinafter referred to as product a1)；
It takes product A (10g) to be placed in HCl solution (3mol/L) after immersion 12h, activated material is obtained after being filtered, washed, drying
(hereinafter referred to as product a2)；
Product B (10g) is taken to be placed in H3PO4After impregnating 12h in solution (6mol/L), material must be activated after being filtered, washed, drying
Expect (hereinafter referred to as product b)；
Products C (10g) is taken to be placed in H3PO4After impregnating 12h in solution (3mol/L), material must be activated after being filtered, washed, drying
Expect (hereinafter referred to as product c).
Embodiment 5
Waste water (secondary effluent for being derived from Jiangsu Leather Factory), ammonia nitrogen (NH4 +- N) measured using Nessler's reagent photometer,
Total phosphorus (TP) uses ion-chromatographic determination, and index is shown in Table.
| NH4 +-N(mg/L) | TP(mg/L) |
| 59.62±0.30 | 6.95±0.10 |
Example 1: taking waste water 1.0L that product A (2.0g) is added thereto, is stirred after 1h (no precipitating continues to generate) at room temperature, mistake
Filter (detects NH in filtrate4 +- N, TP indices), collect precipitating, dry product 1.
Example 2: taking waste water 1.0L that product B (2.0g) is added thereto, is stirred after 1h (no precipitating continues to generate) at room temperature, mistake
Filter (detects NH in filtrate4 +- N, TP indices), collect precipitating, dry product 2.
Example 3: taking waste water 1.0L that products C (2.0g) is added thereto, is stirred after 1h (no precipitating continues to generate) at room temperature, mistake
Filter (detects NH in filtrate4 +- N, TP indices), collect precipitating, dry product 3.
Example 4: taking waste water 1.0L that product a1 (2.0g) is added thereto, is stirred after 1h (no precipitating continues to generate) at room temperature,
Filtering (detects NH in filtrate4 +- N, TP indices), collect precipitating, dry product 4.
Example 5: taking waste water 1.0L that product a2 (2.0g) is added thereto, is stirred after 1h (no precipitating continues to generate) at room temperature,
Filtering (detects NH in filtrate4 +- N, TP indices), collect precipitating, dry product 5.
Example 6: taking waste water 1.0L that product b (2.0g) is added thereto, is stirred after 1h (no precipitating continues to generate) at room temperature, mistake
Filter (detects NH in filtrate4 +- N, TP indices), collect precipitating, dry product 6.
Example 7: taking waste water 1.0L that product c (2.0g) is added thereto, is stirred after 1h (no precipitating continues to generate) at room temperature, mistake
Filter (detects NH in filtrate4 +- N, TP indices), collect precipitating, dry product 7.
Example 8: waste water 1.0L is taken to be added thereto and NH4 +The MgCl of the amount of substance such as-N2·6H2O and Na2HPO4·12H2O,
After stirring 1h at room temperature, filtering (detects NH in filtrate4 +- N, TP indices).
NH in filtrate in example 1- example 84 +- N, TP index see the table below.
| Filtrate | NH4 +-N(mg/L) | TP(mg/L) |
| Example 1 | 42.25±0.30 | 6.32±0.10 |
| Example 2 | 43.50±0.30 | 6.35±0.10 |
| Example 3 | 46.20±0.30 | 6.43±0.10 |
| Example 4 | 5.16±0.10 | 2.20±0.10 |
| Example 5 | 35.26±0.30 | 6.25±0.10 |
| Example 6 | 5.48±0.10 | 2.31±0.10 |
| Example 7 | 24.69±0.30 | 4.58±0.10 |
| Example 8 | 27.82±0.30 | 22.42±0.30 |
The field experiment of the product 4, ammonium magnesium phosphate and its compound fertilizer that obtain after 6 present invention processing waste water of embodiment is using field
Between randomized block experiment, each plot area is 4.0m × 5.0m, and using the ammonium-magnesium compounded fertilizer of application of phosphoric acid as compareing, every group is applied
Fertilizer amount is 50Kg/ mus, and romaine lettuce kind is 4 season of Thailand；As a result such as following table.
Claims (8)
1. a kind of method of waste water high-efficiency denitrogenation production efficient compound fertilizer, it is characterised in that include the following steps:
(1) activation of the biological carbon material of magnesium and phosphate anion is loaded:
The biological carbon material for loading magnesium and phosphate anion is placed in H3PO4After impregnating 12h in solution, after being filtered, washed, drying
Activated material is obtained, it is spare；
(2) activated material of step (1) preparation is added into waste water, after stirring 1h, precipitating, dry product are collected in filtering；
(3) product that step (2) obtains is uniformly mixed with ammonium magnesium phosphate with mass ratio 1:3-1:5 to get efficient compound fertilizer.
2. method described in claim 1, it is characterised in that H described in step (1)3PO4The concentration of solution is 3-6mol/L.
3. the described in any item methods of claim 1-2, it is characterised in that waste water described in step (2) is nitrogen-containing wastewater, living
The dosage for changing material is that 200mg activated material is used in every 100mL waste water.
4. a kind of efficient compound fertilizer, it is characterised in that the efficient compound fertilizer is by ingredient 1 and ammonium magnesium phosphate with mass ratio 1:3-1:5
It is mixed with；The preparation method of the ingredient 1 includes the following steps:
(1) activation of the biological carbon material of magnesium and phosphate anion is loaded:
The biological carbon material for loading magnesium and phosphate anion is placed in H3PO4After impregnating 12h in solution, after being filtered, washed, drying
Activated material is obtained, it is spare；
(2) activated material of step (1) preparation is added into waste water, after stirring 1h, precipitating, dry ingredient 1 are collected in filtering.
5. efficient compound fertilizer as claimed in claim 4, it is characterised in that H described in step (1)3PO4The concentration of solution is 3-
6mol/L。
6. the described in any item efficient compound fertilizers of claim 4-5, it is characterised in that waste water described in step (2) is useless containing ammonia nitrogen
Water, the dosage of activated material are that 200mg activated material is used in every 100mL waste water.
7. the biological carbon material of load magnesium and phosphate anion of any of claims 1-6, it is characterised in that it is made
Preparation Method includes the following steps:
(1) dried yeast powder and glucose are dissolved in deionized water, after cultivating 0.5-1.0h at 30-35 DEG C, centrifugation, deionization
Water washing obtains saccharomycete；
(2) MgCl is added in the saccharomycete that step (1) obtains2Solution and H3PO4Solution after stirring 0.5h, is warming up at room temperature
170-180 DEG C, after reacting 5-8h, centrifugation, drying, grinds to obtain presoma at deionized water washing；
(3) presoma that step (2) obtains is placed in tube furnace, under nitrogen protection, with the heating rate liter of 10 DEG C/min
To 800 DEG C of calcining 4h, restore the biological carbon material to room temperature to get the load magnesium and phosphate anion.It is done in step (1)
The preferred 1:2 of the mass ratio of yeast powder and glucose, every gram of dried yeast powder use 100mL deionized water；MgCl in step (2)2It is molten
Liquid and H3PO4The concentration of solution is 1mol/L, and dosage is that every gram of dried yeast powder uses MgCl2Solution 100mL, uses H3PO4
Solution 100mL；The reaction of step (2) preferably carries out in a high pressure reaction kettle.
8. the biological carbon material of load magnesium as claimed in claim 7 and phosphate anion is in denitrogenation of waste water production efficient compound fertilizer
Application.
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|---|---|---|---|
| CN201811502582.8A CN109593001A (en) | 2018-12-09 | 2018-12-09 | A kind of method of leather waste water efficient denitrification production efficient compound fertilizer |
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| CN201811502582.8A CN109593001A (en) | 2018-12-09 | 2018-12-09 | A kind of method of leather waste water efficient denitrification production efficient compound fertilizer |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000264615A (en) * | 1999-03-18 | 2000-09-26 | Tokyo Gas Co Ltd | Yeasts, yeast-containing material and gas adsorbent |
| CN103523769A (en) * | 2013-10-08 | 2014-01-22 | 中国农业大学 | Composite charcoal, and preparation method and application thereof |
-
2018
- 2018-12-09 CN CN201811502582.8A patent/CN109593001A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000264615A (en) * | 1999-03-18 | 2000-09-26 | Tokyo Gas Co Ltd | Yeasts, yeast-containing material and gas adsorbent |
| CN103523769A (en) * | 2013-10-08 | 2014-01-22 | 中国农业大学 | Composite charcoal, and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 伦世仪 等: "《环境生物工程》", 31 May 2002, 化学工业出版社 * |
| 王正银 等: "《肥料研制与加工 第2版》", 31 December 2015, 中国农业大学出版社 * |
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