CN104311337B - A kind of method of utilizing glutamic acid wastewater to produce liquid fertilizer - Google Patents
A kind of method of utilizing glutamic acid wastewater to produce liquid fertilizer Download PDFInfo
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- CN104311337B CN104311337B CN201410558744.5A CN201410558744A CN104311337B CN 104311337 B CN104311337 B CN 104311337B CN 201410558744 A CN201410558744 A CN 201410558744A CN 104311337 B CN104311337 B CN 104311337B
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/80—Soil conditioners
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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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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F7/00—Fertilisers from waste water, sewage sludge, sea slime, ooze or similar masses
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- Life Sciences & Earth Sciences (AREA)
- Soil Sciences (AREA)
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Abstract
The invention belongs to Amino Acid Fermentation Wastewater process field, a kind of method of utilizing glutamic acid wastewater to produce liquid fertilizer is disclosed, comprise the steps, step 1) filtering fermentation liquor, step 2) decolour, concentrate and crystallization, step 3) separates ammonia sulfate crystal, step 4) hydrolysis, and step 5) is prepared fertilizer. The method has been used paddy base acid fermentation waste water, greatly reduces fertilizer production cost, realized and having turned waste into wealth, and effect of fertilizer is better than market like product.
Description
Technical field
The invention belongs to Amino Acid Fermentation Wastewater process field, be specifically related to a kind of method of utilizing glutamic acid wastewater to produce liquid fertilizer.
Background technology
Glutamic acid is a kind of acidic amino acid. Molecule includes two carboxyls, and chemical name is alpha-amido glutaric acid. Glutamic acid is that inner Suo Xun finds for 1856, is clear crystal, has delicate flavour, is present in a large number in grain protein, and in animal brain, content is also more. In glutamic acid protein metabolism process in vivo, account for critical role, participate in the many important chemical reaction in animal, plant and microorganism. Sodium glutamate is commonly called as monosodium glutamate, is important tasty agents, and fragrance is had to humidification. Sodium glutamate is widely used in food flavor, both can be used alone, and can also use with other amino acid etc. again. For in food, there is flavouring effect.
Along with the development of amino acid fermentation technology, China has become the production and consumption big country of monosodium glutamate, but the wastewater flow rate discharging in glutamate production process is large, fermented gournet powder liquid through etc. electricity extract the mother liquor discharging after glutamic acid and have that CODCr is high, BOD5 is high, thalline content is high, content is high, ammonia-nitrogen content is high and the feature of pH value (1.5-3.2) low " five high low " for sulfate radical (using instead before sulfuric acid is adjusted pH is chlorion). It is the industrial wastewater that a kind of difficulty of governance is very large. Owing to can not effectively administering gourmet powder waste water, many Gourmet Powder Factories are put into the row of national major polluting sources unit, and the improvement of gourmet powder waste water has become the great difficult problem of restriction glutamate production enterprise development. The a large amount of thalline that contain in waste water, it is a kind of single cell protein, contains rich in protein.
The development of China's fertilizer and application history, be to be Main Stage from farm manure to using inorganic fertilizer, and because farm manure pollution sources are many, freight volume is large, in operation, wastes time and energy and effect is not obvious especially; And inorganic fertilizer composition is single, utilization rate is lower, and tends to cause soil compaction and follow soil erosion polluted source, influence ecological environment. The defects such as at present, market adopts the inorganic composite fertilizer of Nitrogen-and Phosphorus-containing potassium etc. more, and the fertilizer efficiency of this composite fertilizer is comprehensive, but also exists fertilizer efficiency not lasting, easy loss; The more important thing is, the price of composite fertilizer is higher at present, brings larger burden to peasant, how to reduce fertilizer cost, and improving farmers' income is the agricultural modernization technical issues that need to address.
Summary of the invention
In order to overcome the defect of prior art, the invention provides a kind of method of utilizing glutamic acid wastewater to produce liquid fertilizer, the method has been used Amino Acid Fermentation Wastewater, greatly reduces fertilizer production cost, realized and having turned waste into wealth, and fertilization effect is better than market like product.
For achieving the above object, the present invention is by the following technical solutions:
Utilize glutamic acid wastewater to produce a method for liquid fertilizer, the method comprises the steps: step 1) filtering fermentation liquor, step 2) to decolour, concentrate and crystallization, step 3) separates ammonia sulfate crystal, step 4) hydrolysis, and step 5) is prepared fertilizer;
Particularly, described method comprises the steps:
Step 1) filtering fermentation liquor: glutami acid fermentation liquor, through micro-filtrate membrane filtration degerming, is collected respectively trapped substance and filtered solution; Then filtered solution is proceeded to ultrafiltration membrance filter, collect concentrate and penetrating fluid; Above-mentioned trapped substance and concentrate are merged into feed liquid A for subsequent use; Wherein, micro-filtration membrane is inorganic ceramic membrane, and molecular cut off is 2000MW, and micro-filtration temperature is 40 DEG C; Milipore filter molecular cut off is 300MW, and ultrafiltration temperature is 40 DEG C;
Step 2) decolouring, concentrated and crystallization: step 1) gained penetrating fluid pumps into the bleacher processing of decolouring, in bleacher, add the active carbon of penetrating fluid quality 0.5%, the temperature of controlling in bleacher is 45 DEG C, after decolouring 30min, plate-frame filtering is removed active carbon, then concentrated, crystallization, last centrifugal acquisition glutamic acid crystal and mother liquor; Described concentrated parameter is: temperature 60 C, and vacuum is-0.1kpa;
Step 3) separates ammonia sulfate crystal: by step 2) the mother liquid obtained evaporation and concentration of carrying out, temperature is controlled at 65 DEG C, stream adds liquefied ammonia simultaneously, make pH value of solution be controlled at 4.0, evaporation and concentration was to 1/3 o'clock of mother liquor volume, be cooled to 40 DEG C and separate out ammonia sulfate crystal, centrifugation obtains ammonia sulfate crystal and concentrated mother liquor;
Step 4) hydrolysis: feed liquid A is dried, pulverizer is ground into Powdered, then be placed in reactor, add the hydrochloric acid of 6-8mol/L, not have raw material to be as the criterion, at 60 DEG C of temperature, stir hydrolysis 12-16 hour, mixing speed is turn/min of 100-200, after reaction terminating, use in potassium hydroxide and remaining hydrochloric acid, obtain amino acid solution, then the ratio that is 3:1 according to the mol ratio of amino acid and metal ion is added metal ion, control temperature is 40-50 DEG C, time is 30-40min, pH carries out chelatropic reaction 7.0, finally that chelating product is concentrated, be dried and pulverize, obtain amino-acid chelate,
Step 5) is prepared fertilizer: amino-acid chelate, shitosan, humic acid, urea, potassium dihydrogen phosphate and step 3) gained concentrated mother liquor are added in agitator tank according to the mass ratio of 1-2:5-9:8-15:30-50:35-50:100-150,100-200 rev/min is stirred 10-20 minute, to obtain final product;
Described metal ion is formed according to the mixed in molar ratio of 1:1:1 by copper ion, calcium ion and zinc ion.
The invention also discloses the fertilizer of preparation according to the method described above.
The beneficial effect that the present invention obtains mainly comprises:
1. the present invention separates the ammonium sulfate in mother liquor, avoids sulfate ion and calacareous soil to form calcium sulfate, causes soil knot tying, has also avoided sulfate radical to be reduced into hydrogen sulfide in water logging situation, and Crop Root is damaged.
2. in the filtration trapped substance of glutami acid fermentation liquor and concentrate, contain a large amount of fermentation thalline and albumen, the present invention, produce amino acid whose mycoprotein and the mother liquor of having utilized simultaneously, has saved mother liquid disposal process, reduces production costs, realize and having turned waste into wealth, increased substantially the utilization rate of resource;
3. the present invention, by utilizing mycoprotein to be prepared into chelating amino acid, avoids using expensive protein raw materials, and has greatly improved fertilizer;
4. the present invention adds potassium hydroxide as nertralizer, and the sylvite of its generation can be used as composite fertilizer's potassium nutrient;
5. the present invention has added the humic acid of appropriate amount, with physics and chemistry bonding mode complexing nutrient, delays nutrient and discharges speed, realizes fast delaying of fertilizer efficiency and has both, and improves fertilizer conservation, water holding capacity, pins nutrient control and runs off;
6. preparation method's simple possible of the present invention, is applicable to large-scale industrial production.
Detailed description of the invention
In order to make those skilled in the art person understand better the technical scheme in the application, below in conjunction with the application's specific embodiment, the present invention is described more clearly and completely, obviously, described embodiment is only some embodiments of the present application, instead of whole embodiment. Based on the embodiment in the application, those of ordinary skill in the art, not making the every other embodiment obtaining under creative work prerequisite, should belong to the scope of protection of the invention.
Embodiment 1
Utilize glutamic acid wastewater to produce a method for liquid fertilizer, it comprises the steps:
Step 1) filtering fermentation liquor: glutami acid fermentation liquor, through micro-filtrate membrane filtration degerming, is collected respectively trapped substance and filtered solution; Then filtered solution is proceeded to ultrafiltration membrance filter, collect concentrate and penetrating fluid; Above-mentioned trapped substance and concentrate are merged into feed liquid A for subsequent use; Wherein, micro-filtration membrane is inorganic ceramic membrane, and molecular cut off is 2000MW, and micro-filtration temperature is 40 DEG C; Milipore filter molecular cut off is 300MW, and ultrafiltration temperature is 40 DEG C;
Step 2) decolouring, concentrated and crystallization: step (1) gained penetrating fluid pumps into the bleacher processing of decolouring, in bleacher, add the active carbon of penetrating fluid quality 0.5%, the temperature of controlling in bleacher is 45 DEG C, after decolouring 30min, plate-frame filtering is removed active carbon, then concentrated, crystallization, last centrifugal acquisition glutamic acid crystal and mother liquor; Described concentrated parameter is: temperature 60 C, and vacuum is-0.1kpa;
Step 3) is prepared ammonia sulfate crystal: mother liquor is carried out to evaporation and concentration, and temperature is controlled at 65 DEG C, and stream adds liquefied ammonia simultaneously, make solution PH be controlled at 4.0, evaporation and concentration, to 1/3 o'clock of stoste volume, is cooled to 40 DEG C and separates out ammonia sulfate crystal, and centrifugation obtains ammonia sulfate crystal and concentrated mother liquor;
Step 4) hydrolysis: feed liquid A is dried, pulverizer is ground into Powdered, then be placed in reactor, add the hydrochloric acid of 8mol/L, not have raw material to be as the criterion, at 60 DEG C of temperature, stir hydrolysis 12 hours, mixing speed is 100 turn/min, after reaction terminating, use in potassium hydroxide and remaining hydrochloric acid, obtain amino acid solution, then the ratio that is 3:1 according to the mol ratio of amino acid and metal ion is added metal ion, controlling temperature is 40 DEG C, time is 30min, pH carries out chelatropic reaction 7.0, finally that chelating product is concentrated, be dried and pulverize, obtain amino-acid chelate, described metal ion is by copper ion (Cu＋2), calcium ion (Ca＋2) and zinc ion (Zn＋2) form according to the mixed in molar ratio of 1:1:1;
Step 5) is prepared fertilizer: amino-acid chelate, shitosan, humic acid, urea, potassium dihydrogen phosphate and step 3) gained concentrated mother liquor are added in agitator tank according to the mass ratio of 1:5:8:30:35:100,200 revs/min are stirred 10 minutes, to obtain final product.
Embodiment 2
Utilize glutamic acid wastewater to produce a method for liquid fertilizer, it comprises the steps:
Step 1) filtering fermentation liquor: glutami acid fermentation liquor, through micro-filtrate membrane filtration degerming, is collected respectively trapped substance and filtered solution; Then filtered solution is proceeded to ultrafiltration membrance filter, collect concentrate and penetrating fluid; Above-mentioned trapped substance and concentrate are merged into feed liquid A for subsequent use; Wherein, micro-filtration membrane is inorganic ceramic membrane, and molecular cut off is 2000MW, and micro-filtration temperature is 40 DEG C; Milipore filter molecular cut off is 300MW, and ultrafiltration temperature is 40 DEG C;
Step 2) decolouring, concentrated and crystallization: step (1) gained penetrating fluid pumps into the bleacher processing of decolouring, in bleacher, add the active carbon of penetrating fluid quality 0.5%, the temperature of controlling in bleacher is 45 DEG C, after decolouring 30min, plate-frame filtering is removed active carbon, then concentrated, crystallization, last centrifugal acquisition glutamic acid crystal and mother liquor; Described concentrated parameter is: temperature 60 C, and vacuum is-0.1kpa;
Step 3) is prepared ammonia sulfate crystal: mother liquor is carried out to evaporation and concentration, and temperature is controlled at 65 DEG C, and stream adds liquefied ammonia simultaneously, make solution PH be controlled at 4.0, evaporation and concentration, to 1/3 o'clock of stoste volume, is cooled to 40 DEG C and separates out ammonia sulfate crystal, and centrifugation obtains ammonia sulfate crystal and concentrated mother liquor;
Step 4) hydrolysis: feed liquid A is dried, pulverizer is ground into Powdered, then be placed in reactor, add the hydrochloric acid of 6mol/L, not have raw material to be as the criterion, at 60 DEG C of temperature, stir hydrolysis 16 hours, mixing speed is 200 turn/min, after reaction terminating, use in potassium hydroxide and remaining hydrochloric acid, obtain amino acid solution, then the ratio that is 3:1 according to the mol ratio of amino acid and metal ion is added metal ion, controlling temperature is 50 DEG C, time is 40min, pH carries out chelatropic reaction 7.0, finally that chelating product is concentrated, be dried and pulverize, obtain amino-acid chelate, described metal ion is by copper ion (Cu＋2), calcium ion (Ca＋2) and zinc ion (Zn＋2) form according to the mixed in molar ratio of 1:1:1;
Step 5) is prepared fertilizer: amino-acid chelate, shitosan, humic acid, urea, potassium dihydrogen phosphate and step 3) gained concentrated mother liquor are added in agitator tank according to the mass ratio of 2:9:15:50:50:150,100 revs/min are stirred 20 minutes, to obtain final product.
Embodiment 3
The manure trial of fertilizer of the present invention
One, taking tomato as example:
Liquid fertilizer prepared by the embodiment of the present invention 1 impact on tomato yield and quality. Test group is appended and is sprayed preparation of the present invention, and control group is with spray equivalent clear water, and tomato variety is that gingko is rich by force, every mu of ground 100kg, and two groups of other planting conditions are identical. Result is as shown in table 1, can increase tomato yield after using this product, shortens Time To Market, strengthens tomato resistance against diseases, can also improve fruit quality, increases the economic worth of tamato fruit.
Table 1
Two, taking cucumber as example:
The impact of the liquid fertilizer of the embodiment of the present invention 1 on cucumber yield and quality. Spring plastic tent cucumber experimental cultivar is Tianjin spring No. 3, adopt high furrow ridge culture, wide-and narrow-row cultivation, 1 mu of ground of community area, liquid fertilizer (test group 1) prepared by foliage-spray embodiment 1 and commercially available Kang Piao Liquid Fertilizer (test group 2), connect and spray 3 times, to spray clear water as contrast, measure its early yield (contrast reaches and begins to receive the output in after date 15d), every community is got 100 strains and is observed the increment in its 15d. Result is as shown in table 2, can promote cucumber growth after using fertilizer of the present invention, strengthens cucumber resistance against diseases, improves cucumber yield and product quality. On indices, be all better than commercially available conventional liquid fertilizer.
Table 2
Although, above with general explanation and detailed description of the invention, this case being done to detailed explanation, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art. Therefore, the amendment done without departing from theon the basis of the spirit of the present invention or improvement, all belong to the scope of protection of present invention.
Claims (2)
1.OnePlant and utilize glutamic acid wastewater to produce the method for liquid fertilizer, it is characterized in that, described method comprises the steps:
Step 1) filtering fermentation liquor: glutami acid fermentation liquor, through micro-filtrate membrane filtration degerming, is collected respectively trapped substance and filtered solution; Then filtered solution is proceeded to ultrafiltration membrance filter, collect concentrate and penetrating fluid; Above-mentioned trapped substance and concentrate are merged into feed liquid A for subsequent use; Wherein, micro-filtration membrane is inorganic ceramic membrane, and molecular cut off is 2000MW, and micro-filtration temperature is 40 DEG C; Milipore filter molecular cut off is 300MW, and ultrafiltration temperature is 40 DEG C;
Step 2) decolouring, concentrated and crystallization: step 1) gained penetrating fluid pumps into the bleacher processing of decolouring, in bleacher, add the active carbon of penetrating fluid quality 0.5%, the temperature of controlling in bleacher is 45 DEG C, after decolouring 30min, plate-frame filtering is removed active carbon, then concentrated, crystallization, last centrifugal acquisition glutamic acid crystal and mother liquor; Described concentrated parameter is: temperature 60 C, and vacuum is-0.1kpa;
Step 3) separates ammonia sulfate crystal: by step 2) the mother liquid obtained evaporation and concentration of carrying out, temperature is controlled at 65 DEG C, stream adds liquefied ammonia simultaneously, make pH value of solution be controlled at 4.0, evaporation and concentration was to 1/3 o'clock of mother liquor volume, be cooled to 40 DEG C and separate out ammonia sulfate crystal, centrifugation obtains ammonia sulfate crystal and concentrated mother liquor;
Step 4) hydrolysis: feed liquid A is dried, pulverizer is ground into Powdered, then be placed in reactor, add the hydrochloric acid of 6-8mol/L, not have raw material to be as the criterion, at 60 DEG C of temperature, stir hydrolysis 12-16 hour, mixing speed is turn/min of 100-200, after reaction terminating, use in potassium hydroxide and remaining hydrochloric acid, obtain amino acid solution, then the ratio that is 3:1 according to the mol ratio of amino acid and metal ion is added metal ion, control temperature is 40-50 DEG C, time is 30-40min, pH carries out chelatropic reaction 7.0, finally that chelating product is concentrated, be dried and pulverize, obtain amino-acid chelate,
Step 5) is prepared fertilizer: amino-acid chelate, shitosan, humic acid, urea, potassium dihydrogen phosphate and step 3) gained concentrated mother liquor are added in agitator tank according to the mass ratio of 1-2:5-9:8-15:30-50:35-50:100-150,100-200 rev/min is stirred 10-20 minute, to obtain final product;
Described metal ion is formed according to the mixed in molar ratio of 1:1:1 by copper ion, calcium ion and zinc ion.
2. the fertilizer of preparing in accordance with the method for claim 1.
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| CN104926419B (en) * | 2015-07-02 | 2018-01-02 | 湖北新生源生物工程有限公司 | A kind of preparation method of the shape of water-soluble powder containing amino acid fertilizer |
| CN105294319A (en) * | 2015-12-02 | 2016-02-03 | 江苏远山生物技术有限公司 | Method for preparing liquid fertilizer by using beneficial microorganism fermentation liquor |
| CN106045701B (en) * | 2016-06-07 | 2019-07-23 | 内蒙古阜丰生物科技有限公司 | The compound fertilizer prepared using Threonine Fermentation waste |
| CN106631279B (en) * | 2016-12-28 | 2021-03-23 | 贵州大学 | Method for preparing sulfur-containing liquid fertilizer by using barium sulfate factory wastewater |
| CN107129372A (en) * | 2017-06-01 | 2017-09-05 | 内蒙古沃丰农业发展有限公司 | The method that potassium glutamate is produced using the glutamic acid mother liquor after corn fermentation |
| CN107417368A (en) * | 2017-06-20 | 2017-12-01 | 峨眉山市龙腾生物科技有限公司 | A kind of production method of the water soluble fertilizer containing amino acid |
| CN109970488A (en) * | 2017-12-28 | 2019-07-05 | 许传高 | The liquid fertilizer made using amino acid fermentation tail washings |
| CN109987614A (en) * | 2017-12-30 | 2019-07-09 | 许传高 | A method of extracting ammonium sulfate from glutamic acid fermentation tail washings |
| CN110407388B (en) * | 2019-08-16 | 2020-09-04 | 江南大学 | Recycling treatment method of glutamic acid concentrated isoelectric extraction waste liquid |
| CN110734331B (en) * | 2019-10-28 | 2022-03-11 | 内蒙古阜丰生物科技有限公司 | Compound fertilizer prepared by utilizing glutamic acid fermentation waste |
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| CN1161324A (en) * | 1996-06-25 | 1997-10-08 | 无锡轻工大学 | Method for extracting glutamic acid from fermentation liquor |
| CN101337729A (en) * | 2007-07-03 | 2009-01-07 | 长春大成实业集团有限公司 | Processing process for fermentation waste liquid of lysine |
| CN102173881A (en) * | 2010-12-29 | 2011-09-07 | 菱花集团有限公司 | Production method of amino acid plant nutrient solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS5392258A (en) * | 1977-01-17 | 1978-08-12 | Takeda Chemical Industries Ltd | Method for producing solids from fermentation wastes |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1161324A (en) * | 1996-06-25 | 1997-10-08 | 无锡轻工大学 | Method for extracting glutamic acid from fermentation liquor |
| CN101337729A (en) * | 2007-07-03 | 2009-01-07 | 长春大成实业集团有限公司 | Processing process for fermentation waste liquid of lysine |
| CN102173881A (en) * | 2010-12-29 | 2011-09-07 | 菱花集团有限公司 | Production method of amino acid plant nutrient solution |
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