CN105036235A - Composite oxygen producer for adsorbing residual antibiotics in aquaculture water and preparation method thereof - Google Patents
Composite oxygen producer for adsorbing residual antibiotics in aquaculture water and preparation method thereof Download PDFInfo
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Abstract
The present invention belongs to the field of aquaculture technology, and discloses a method for preparing a composite oxygen producer for adsorbing residual antibiotics in aquaculture water. The composite oxygen producer is prepared from the following components by weight: 70-90 parts of an oxygen supply component, 15-25 parts of a traditional Chinese medicine compound, 42-68 parts of an adsorption component, 2 -5 parts of a coating agent, 1-3 parts of a stabilizer and 1.3-1.8 parts of a sustained co-solvent. The oxygen supply component comprises 50-60 parts of sodium peroxide and 20-30 parts of calcium peroxide; the traditional Chinese medicine compound includes celandine, Chinese angelica, Radix Astragali, nephelium lappaceum, receptaculum nelumbinis, fruticose breynia juvenile branchlet and leaf, Hydrangea aspera Don and yucca; the adsorption component comprises 20-30 parts of Chinese medical stone, 6 -10 parts of a polymer material, 9-15 parts of diatomaceous earth and 7-13 parts of silica powder. Through compounding of a plurality of effective components, the obtained product has good oxygenation function and residual antibiotic adsorption function.
Description
Technical field
The invention belongs to technical field of aquaculture, be specifically related to a kind of compound oxygenation agent and preparation method of adsorbing aquaculture water residual antibiotic.
Background technology
Along with the development of social economy and communications and transportation, a large amount of fishery products are transported to the north by south, drive the development of aquaculture.The large problem affecting aquaculture is exactly the quality of water body environment, and in recent years, microbiotic is widely applied in aquaculture, in order to prophylactic treatment and the organic growth promotion of disease.But microbiotic body absorption difference, by force water-soluble, (parent or meta-bolites) continues entered environment with people and livestock and poultry excretion, aquaculture and pharmacy waste water discharge often in an active, and final residue is in water body.Microbiotic residual and accumulation in the environment can cause many eco-toxicities such as microorganism species resistance, has a strong impact on human health and the eubiosis.In addition, the content of oxygen in water is the important indicator weighing water body self-purification ability.Oxygen in water will be consumed during aerobe decomposing pollutant in water, and dissolved oxygen constantly can be supplemented due to incorporating of oxygen in air with the photosynthesis of waterplant; But when water body is subject to Organic pollutants, oxygen consumption is serious, dissolved oxygen can not get supplementing in time, and in water, anerobe can breed very soon, and it is smelly that organic corruption makes water body turn black.Meanwhile, promote that in Sediments, pollutent, to the release rate in water body, increases the weight of water body eutrophication degree.
So aquaculture will solve the problem that water body environment worsens, and not only will increase the content of oxygen in water, also to residual microbiotic be removed.For the content increasing oxygen in water, at present, more water oxygenation mode is used to mainly contain aeration and add the methods such as oxygenation reagent, the method power consumption that mechanical aeration increases oxygen in water is huge, so great majority adopt add the method that chemical reagent (conventional ammonium persulphate, calcium peroxide, hydrogen peroxide etc.) increases dissolved oxygen in water.For microbiotic residual in water body, research mainly concentrate on advanced oxidation processes, absorption method, membrane separation technique and combination process etc., the high-level oxidation technology wherein based on free-radical oxidn obtains extensive concern, and technique generally selects O
3, H
2o
2in conjunction with illumination, or combination metal and semiconductor light-catalyst realize, but the method not only cost is high, and be difficult to realize mineralising in the antibiotic process of degraded, the intermediate metabolites that degraded produces often shows the eco-toxicity stronger than parent microbiotic, application is restricted, and absorption method, as a kind of non-demolition means, often show that cost is low, easy to operate, pollutant removing rate is high and cause extensive attention without advantages such as high toxicity metabolite risks.Therefore, water oxygenation is adsorbed with residual antibiotic and combines, fundamentally solve water quality deterioration problem, improve breeding environment, have great importance for aquaculture, but rarely have report about the concrete research be combined with residual antibiotic Adsorption Phase by water oxygenation at present.
Summary of the invention
In order to solve the shortcoming and defect part of above prior art, primary and foremost purpose of the present invention is to provide a kind of compound oxygenation agent adsorbing aquaculture water residual antibiotic.
Another object of the present invention is to the preparation method of the compound oxygenation agent that a kind of above-mentioned absorption aquaculture water residual antibiotic is provided.
The object of the invention is achieved through the following technical solutions:
Adsorb a compound oxygenation agent for aquaculture water residual antibiotic, be prepared from by the component of following weight part:
Oxygen-supplying component 70 ~ 90 parts, Chinese medicine composite parts 15 ~ 25 parts, adsorption component 42 ~ 68 parts, coating agent 2 ~ 5 parts, stablizer 1 ~ 3 part, slowly-releasing solubility promoter 1.3 ~ 1.8 parts;
Wherein, described oxygen-supplying component comprises 50 ~ 60 parts of sodium carbonate peroxides and 20 ~ 30 parts of calcium peroxides; Described Chinese medicine composite parts comprises pilewort, Radix Angelicae Sinensis, the Radix Astragali, nephelium lappaceum, lotus pod, Leaf and twig of Fruticose Breynia, Root of Sstrigose Hydrangea and yucca; Described adsorption component comprises 20 ~ 30 parts of medical stones, 6 ~ 10 parts of macromolecular materials, 9 ~ 15 parts of diatomite and 7 ~ 13 parts of micropowder silica gels.
The working substance content of pilewort in described Chinese medicine composite parts, Radix Angelicae Sinensis, the Radix Astragali, nephelium lappaceum, lotus pod, Leaf and twig of Fruticose Breynia, Root of Sstrigose Hydrangea and yucca is than being preferably 1:1.5:1:2:2:3:1:0.5.
Preferably, described coating agent is macromolecule film former or water-borne acrylic resin.
Preferably, described stablizer is acetanilide N, adipic acid or water glass.
Preferably, described slowly-releasing solubility promoter is sodium alginate or ethyl cellulose.
Preferably, described macromolecular material is polyaniline derivative macromolecular material.
The preparation method of the compound oxygenation agent of above-mentioned absorption aquaculture water residual antibiotic, comprises following preparation process:
Oxygen-supplying component, Chinese medicine composite parts and adsorption component are put into mixing machine after pretreatment, then adds coating agent, stablizer and slowly-releasing solubility promoter successively, mix, obtain oxygenation agent compound; By oxygenation agent compound through granulation, polishing, screening, oven dry, i.e. the compound oxygenation agent of obtained absorption aquaculture water residual antibiotic.
The preprocessing process of described oxygen-supplying component is as follows:
SPC-D process: SPC-D is placed in Universalpulverizer and pulverizes the SPC-D pulvis making particle fineness≤0.5 millimeter;
Calcium peroxide process: be evenly sprayed into the water relative to its weight 8% ~ 14% in calcium peroxide, mix, obtain calcium peroxide wet feed.
The preprocessing process of described Chinese medicine composite parts is as follows:
Pilewort process: complete for pilewort being placed in temperature is that the clear water of 30 ~ 40 DEG C cleans up, being placed on temperature is again toast 12 ~ 20min in the baking oven of 80 ~ 90 DEG C, then oven temperature to 120 ~ 140 DEG C are adjusted, continue baking 25 ~ 30min, pulverized with pulverizer by the pilewort of drying, cross 150 ~ 180 mesh sieves, the sieve end, continues to employ, compass screen surface returns pulverizer and pulverizes, and obtains pilewort powder;
Radix Angelicae Sinensis process: Radix Angelicae Sinensis is placed in warm water immersion treatment 40 ~ 60min that temperature is 35 ~ 55 DEG C, be placed in boiler again and decoct 90 ~ 150min under the temperature condition of 90 ~ 120 DEG C, cooled and filtered, obtain the aqueous extract of Radix Angelicae Sinensis, concentrating under reduced pressure becomes relative density under 80 degrees celsius to be the medicinal extract of 1.06 ~ 1.24, then spraying dry makes eumenol powder;
Radix Astragali process: the Radix Astragali being placed in temperature is process 20 ~ 30min at the temperature of 40 ~ 70 DEG C, being placed on temperature is again process 10 ~ 20min at the temperature of 70 ~ 90 DEG C, adjust again temperature be 130 ~ 180 DEG C by moisture content process to 1 ~ 3% in the Radix Astragali time, be placed on grinding machine for grinding powdered, can Milkvetch Root be obtained;
Nephelium lappaceum process: nephelium lappaceum tree root is placed in dryer and adopts temperature to be 80 ~ 90 DEG C to dry to moisture contents to be after 4 ~ 6%, then to be placed in pulverizer and to be ground into 130 ~ 140 object powder, nephelium lappaceum powder can be obtained;
Lotus pod process: cleaned by lotus pod and dry, be placed in slow fire in pot and be fired in coke yellow, cool taking-up, is placed on grinding machine for grinding powdered, can obtain lotus pod powder;
Leaf and twig of Fruticose Breynia process: the Leaf and twig of Fruticose Breynia branches and leaves of drying are placed in dryer and dry to moisture content to be 2 ~ 4%, and to be placed in pulverizer and to be ground into 150 ~ 180 object powder, Leaf and twig of Fruticose Breynia powder can be obtained;
Root of Sstrigose Hydrangea process: Root of Sstrigose Hydrangea is cleaned up, being immersed in concentration is in the alcohol of 50 ~ 70%, the weight of alcohol used is 8 ~ 14 times of Root of Sstrigose Hydrangea weight, after immersion treatment 6 ~ 10h, take out, then be placed in frying pan, slow fire is fried slowly, to frying thoroughly completely, finally grinding powdered into powder, obtaining Root of Sstrigose Hydrangea powder;
Yucca process: fresh yucca is placed in baking oven and dries, pulverize through pulverizer, cross 60 mesh sieves, obtain dry yucca powder, be the ethanolic soln that 1:60 ~ 70 add 75 ~ 80% according to solid-to-liquid ratio, be placed in microwave oven and carry out microwave extraction, microwave power is 300W, extraction time is 20 ~ 25s, then decompress filter, obtain the ethanolic soln of yucconin, further concentrating under reduced pressure, heating evaporation removes ethanol, be cooled to room temperature, distilled water and acetone soln is added in the ratio of 1:1:0.8 in above-mentioned gained concentrated solution, carry out separation and purification, concentrating under reduced pressure again, heating evaporation removes acetone and distilled water, obtain yucca extract solid particulate,
Gained pilewort powder, eumenol powder, Milkvetch Root, nephelium lappaceum powder, lotus pod powder, Leaf and twig of Fruticose Breynia powder, Root of Sstrigose Hydrangea powder and yucca extract solid particulate are mixed by weight for 1:1.5:1:2:2:3:1:0.5, obtains Chinese medicine composite parts.
The preprocessing process of described adsorption component is as follows:
Medical stone process: by natural medical stone through screening, pulverizes, and is processed into the maifanite powder of particle fineness≤1.5 millimeter with rubbing down nodulizer;
Diatomite process: acidic solution dipping 3 ~ 5h diatomite being placed in 50 ~ 55 DEG C, described acidic solution is nitric acid, sulfuric acid or hydrochloric acid, flood rear suction filtration, under the condition of 80 ~ 100 DEG C, be dried to water content be again less than 2%, then calcining furnace calcining 1 ~ 3h is placed in, calcining temperature controls, at 1000 ~ 1100 DEG C, to obtain pretreated diatomite;
Diatomite and micropowder silica gel co-grinding: above-mentioned pretreated diatomite is mixed with micropowder silica gel, is placed in pulverizer and is crushed to particle fineness≤1.2 millimeter, then add macromolecular material and mix.
In Chinese medicine composite parts of the present invention, effect of each traditional Chinese medicine ingredients is: pilewort is rich in the nutritive elements such as flavonoid volume vitamins C, and energy sterilization and disinfection; Radix Angelicae Sinensis anti-inflammatory, antibacterial, all has anti-microbial effect, preventing disease to external dysentery, typhoid fever, paratyphoid, intestinal bacteria, diphtheria corynebacterium, vibrio cholerae and a, B Hemolytic streptococcus etc.; The Radix Astragali has enhancing body immunologic function and anti-microbial effect more widely; Nephelium lappaceum shell, anti-inflammation and sterilization, strengthening immunity; Lotus pod promotes fishery products growth; Leaf and twig of Fruticose Breynia all has very strong bacteriostatic action to streptococcus aureus, Pseudomonas aeruginosa, intestinal bacteria, shigella flexneri, alpha streptococcus; Root of Sstrigose Hydrangea can be antiviral, and preventing disease is propagated; Yucca is healthy to promotion fishery products, high yield, improves its digestive tract environment and improves meat product quality, promote absorption of nutrient ingredients, improves efficiency of feed utilization etc. and has vital role.
Preparation method of the present invention and the product tool obtained have the following advantages and beneficial effect:
(1) product oxygen level of the present invention is high, it is long to put the oxygen time, oxygenation speed is fast, directly pond bottom can be sunk to after shedding, oxygenation is carried out to pond bottom and middle lower floor water body, rapid raising bottom dissolved oxygen amount, reaches the effect of " three-dimensional oxygenation ", really effectively solves bottom anoxic problem;
(2) product of the present invention is rich in Chinese medicine composite parts, has disinfection, promotes effect of absorption of nutrient ingredients bottom anerobe also can be suppressed to grow, stop the generation of the objectionable impurities such as ammonia nitrogen, hydrogen sulfide, fish shrimp crab appetite can be strengthened, improve food ration, thus improve aquatic animal output;
(3) product of the present invention adds sorbent material especially, good adsorption is have for residue in water antibiosis, and can purify water, medical stone in sorbent material contains 18 kinds of trace elements such as potassium, sodium, calcium, magnesium, phosphorus major element and zinc, iron, selenium, copper, strontium, iodine, fluorine, metasilicic acid, at typical condition, in medical stone dissolution fluid, four kinds of trace element (metasilicic acid, Sr, Zn, F) content reaches or close to national potable mineral water standard, useful and harmless to fishery products, supplement water body mineral matter nutritional source, improve fishery products quality; Polyaniline derivative Polymer materialspreparation technique in sorbent material is simple, and raw material is cheap and easy to get, and cost is low, and chemical stability is good simultaneously, better for microbiotic adsorption effect, can not cause secondary pollution to environment;
(4) coating agent of the present invention adopts water-borne acrylic resin, has that price is low, use safety, and saving resource and the energy, reduce the advantage of environmental pollution;
(5) in preparation method of the present invention by diatomite and micropowder silica gel co-grinding, not only make pulverizing more easily carry out, solid dispersal to a certain extent can also be formed.
Accompanying drawing explanation
Fig. 1 is the experimental group of the compound oxygenation agent of the absorption aquaculture water residual antibiotic used respectively in the embodiment of the present invention 1 ~ 3 and the mean body weight growth pattern figure of control group cultivation circle carp.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
A kind of compound oxygenation agent adsorbing aquaculture water residual antibiotic of the present embodiment, is prepared from by the component of following weight part:
Oxygen-supplying component 70 parts, Chinese medicine composite parts 15 parts, adsorption component 42 parts, macromolecule film former 2 parts, acetanilide N 1 part, sodium alginate 1.3 parts; Wherein, described oxygen-supplying component comprises 50 parts of sodium carbonate peroxides, 20 parts of calcium peroxides; Described Chinese medicine composite parts is prepared from by pilewort, Radix Angelicae Sinensis, the Radix Astragali, nephelium lappaceum, lotus pod, Leaf and twig of Fruticose Breynia, Root of Sstrigose Hydrangea and yucca; Described adsorption component comprises 20 parts of medical stones, 6 parts of polyaniline derivative macromolecular materials, 9 parts of diatomite and 7 parts of micropowder silica gels.
Its concrete preparation method is as follows:
(1) oxygen-supplying component pre-treatment:
A. SPC-D process: SPC-D is placed in Universalpulverizer pulverizing and makes the SPC-D pulvis that particle fineness is 0.3 millimeter, stand-by;
B. calcium peroxide process: be evenly sprayed into the water relative to its weight 8% in calcium peroxide, mix, obtain calcium peroxide wet feed, stand-by;
(2) Chinese medicine composite parts pre-treatment:
A. pilewort process: complete for pilewort being placed in temperature is that the clear water of 30 DEG C cleans up, being placed on temperature is again toast 12min in the baking oven of 80 DEG C, then oven temperature to 120 DEG C is adjusted, continue baking 25min, the pilewort of drying is pulverized with pulverizer, cross 150 mesh sieves, the sieve end, continues to employ, compass screen surface returns pulverizer and pulverizes, and obtains pilewort powder, stand-by;
B. Radix Angelicae Sinensis process: Radix Angelicae Sinensis is placed in the warm water immersion treatment 40min that temperature is 35 DEG C, being placed in boiler again under the temperature condition of 90 DEG C decocts 90min, cooled and filtered, obtain the aqueous extract of Radix Angelicae Sinensis, concentrating under reduced pressure becomes relative density under 80 degrees celsius to be the medicinal extract of 1.06, spraying dry makes eumenol powder again, stand-by;
C. Radix Astragali process: the Radix Astragali being placed in temperature is process 20min at the temperature of 40 DEG C, being placed on temperature is again process 10min at the temperature of 70 DEG C, adjust again temperature be 130 DEG C by moisture content process to 1% in the Radix Astragali time, be placed on grinding machine for grinding powdered, can Milkvetch Root be obtained, stand-by;
D. nephelium lappaceum process: nephelium lappaceum tree root is placed in dryer and adopts temperature to be 80 DEG C to dry to moisture contents to be after 4%, then to be placed in pulverizer and to be ground into 130 object powder, nephelium lappaceum powder can be obtained, stand-by;
E. lotus pod process: cleaned by lotus pod and dry, be placed in slow fire in pot and be fired in coke yellow, cool taking-up, is placed on grinding machine for grinding powdered, can obtain lotus pod powder;
F. Leaf and twig of Fruticose Breynia process: the Leaf and twig of Fruticose Breynia branches and leaves of drying are placed in dryer and dry to moisture content to be 2%, and to be placed in pulverizer and to be ground into 150 object powder, Leaf and twig of Fruticose Breynia powder can be obtained, stand-by;
G. Root of Sstrigose Hydrangea process: Root of Sstrigose Hydrangea is cleaned up, being immersed in concentration is in the alcohol of 50%, and the weight of alcohol used is 8 times of Root of Sstrigose Hydrangea weight, after immersion treatment 6h, take out, then be placed in frying pan, slow fire is fried slowly, to frying thoroughly completely, finally grind powdered into powder, obtain Root of Sstrigose Hydrangea powder, stand-by;
H. yucca process: fresh yucca is placed in baking oven and dries, pulverize through pulverizer, cross 60 mesh sieves, obtain dry yucca powder, be the ethanolic soln that 1:60 adds 75% according to solid-to-liquid ratio, be placed in microwave oven and carry out microwave extraction, microwave power is 300W, extraction time is 20s, then decompress filter, obtain the ethanolic soln of yucconin, further concentrating under reduced pressure, heating evaporation removes ethanol, be cooled to room temperature, distilled water and acetone soln is added in the ratio of 1:1:0.8 in above-mentioned gained concentrated solution, carry out separation and purification, concentrating under reduced pressure again, heating evaporation removes acetone and distilled water, obtain yucca extract solid particulate, stand-by,
Gained pilewort powder, eumenol powder, Milkvetch Root, nephelium lappaceum powder, lotus pod powder, Leaf and twig of Fruticose Breynia powder, Root of Sstrigose Hydrangea powder and yucca extract solid particulate are mixed by weight for 1:1.5:1:2:2:3:1:0.5, obtains Chinese medicine composite parts.
(3) adsorption component pre-treatment:
A. medical stone process: by natural medical stone through screening, pulverize, be processed into maifanite powder with rubbing down nodulizer, its particle fineness is 1.3 millimeters, stand-by;
B. diatomite process: acidic solution diatomite being placed in 50 DEG C floods 3h, described acidic solution is nitric acid, sulfuric acid or hydrochloric acid, flood rear suction filtration, under the condition of 80 DEG C, be dried to water content be again less than 2%, then be placed in calcining furnace and calcine 1h, calcining temperature controls, at 1000 DEG C, to obtain pretreated diatomite, stand-by;
C. diatomite and micropowder silica gel co-grinding: above-mentioned pretreated diatomite is mixed with micropowder silica gel, being placed in pulverizer, to be crushed to particle fineness be 1.0 millimeters, then add polyaniline derivative macromolecular material, mixing, stand-by;
(4) mixing granulation:
Oxygen-supplying component good for step (1) to (3) pre-treatment, Chinese medicine composite parts, adsorption component are placed in mixing machine, add macromolecule film former, stablizer acetanilide N and sustained release dosage sodium alginate more successively, mix, obtain oxygenation agent compound; By oxygenation agent compound through granulation, polishing, screening, oven dry, i.e. the compound oxygenation agent of obtained absorption aquaculture water residual antibiotic.
Embodiment 2
A kind of compound oxygenation agent adsorbing aquaculture water residual antibiotic of the present embodiment, is prepared from by the component of following weight part:
Oxygen-supplying component 80 parts, Chinese medicine composite parts 20 parts, adsorption component 55 parts, water-borne acrylic resin 3.5 parts, adipic acid 2 parts, sodium alginate 1.55 parts; Wherein, described oxygen-supplying component comprises 55 parts of sodium carbonate peroxides, 25 parts of calcium peroxides; Described Chinese medicine composite parts is prepared from by pilewort, Radix Angelicae Sinensis, the Radix Astragali, nephelium lappaceum, lotus pod, Leaf and twig of Fruticose Breynia, Root of Sstrigose Hydrangea and yucca; Described adsorption component comprises 25 parts of medical stones, 8 parts of polyaniline derivative macromolecular materials, 12 parts of diatomite and 10 parts of micropowder silica gels.
Its concrete preparation method is as follows:
(1) oxygen-supplying component pre-treatment:
A. SPC-D process: SPC-D is placed in Universalpulverizer pulverizing and makes the SPC-D pulvis that particle fineness is 0.4 millimeter, stand-by;
B. calcium peroxide process: be evenly sprayed into the water relative to its weight 11% in calcium peroxide, mix, obtain calcium peroxide wet feed, stand-by;
(2) Chinese medicine composite parts pre-treatment:
A. pilewort process: complete for pilewort being placed in temperature is that the clear water of 35 DEG C cleans up, being placed on temperature is again toast 16min in the baking oven of 85 DEG C, then oven temperature to 130 DEG C is adjusted, continue baking 27.5min, the pilewort of drying is pulverized with pulverizer, cross 165 mesh sieves, the sieve end, continues to employ, compass screen surface returns pulverizer and pulverizes, and obtains pilewort powder, stand-by;
B. Radix Angelicae Sinensis process: Radix Angelicae Sinensis is placed in the warm water immersion treatment 50min that temperature is 45 DEG C, being placed in boiler again under the temperature condition of 105 DEG C decocts 120min, cooled and filtered, obtain the aqueous extract of Radix Angelicae Sinensis, concentrating under reduced pressure becomes relative density under 80 degrees celsius to be the medicinal extract of 1.15, spraying dry makes eumenol powder again, stand-by;
C. Radix Astragali process: the Radix Astragali being placed in temperature is process 25min at the temperature of 55 DEG C, being placed on temperature is again process 15min at the temperature of 80 DEG C, adjust again temperature be 155 DEG C by moisture content process to 2% in the Radix Astragali time, be placed on grinding machine for grinding powdered, can Milkvetch Root be obtained, stand-by;
D. nephelium lappaceum process: nephelium lappaceum tree root is placed in dryer and adopts temperature to be 85 DEG C to dry to moisture contents to be after 5%, then to be placed in pulverizer and to be ground into 135 object powder, nephelium lappaceum powder can be obtained, stand-by;
E. lotus pod process: cleaned by lotus pod and dry, be placed in slow fire in pot and be fired in coke yellow, cool taking-up, is placed on grinding machine for grinding powdered, can obtain lotus pod powder;
F. Leaf and twig of Fruticose Breynia process: the Leaf and twig of Fruticose Breynia branches and leaves of drying are placed in dryer and dry to moisture content to be 3%, and to be placed in pulverizer and to be ground into 165 object powder, Leaf and twig of Fruticose Breynia powder can be obtained, stand-by;
G. Root of Sstrigose Hydrangea process: Root of Sstrigose Hydrangea is cleaned up, being immersed in concentration is in the alcohol of 60%, and the weight of alcohol used is 11 times of Root of Sstrigose Hydrangea weight, after immersion treatment 8h, take out, then be placed in frying pan, slow fire is fried slowly, to frying thoroughly completely, finally grind powdered into powder, obtain Root of Sstrigose Hydrangea powder, stand-by;
H. yucca process: fresh yucca is placed in baking oven and dries, pulverize through pulverizer, cross 60 mesh sieves, obtain dry yucca powder, be the ethanolic soln that 1:65 adds 77.5% according to solid-to-liquid ratio, be placed in microwave oven and carry out microwave extraction, microwave power is 300W, extraction time is 22.5s, then decompress filter, obtain the ethanolic soln of yucconin, further concentrating under reduced pressure, heating evaporation removes ethanol, be cooled to room temperature, distilled water and acetone soln is added in the ratio of 1:1:0.8 in above-mentioned gained concentrated solution, carry out separation and purification, concentrating under reduced pressure again, heating evaporation removes acetone and distilled water, obtain yucca extract solid particulate, stand-by,
Gained pilewort powder, eumenol powder, Milkvetch Root, nephelium lappaceum powder, lotus pod powder, Leaf and twig of Fruticose Breynia powder, Root of Sstrigose Hydrangea powder and yucca extract solid particulate are mixed by weight for 1:1.5:1:2:2:3:1:0.5, obtains Chinese medicine composite parts.
(3) adsorption component pre-treatment:
A. medical stone process: by natural medical stone through screening, pulverize, be processed into maifanite powder with rubbing down nodulizer, its particle fineness is 1.4 millimeters, stand-by;
B. diatomite process: acidic solution diatomite being placed in 52.5 DEG C floods 4h, described acidic solution is nitric acid, sulfuric acid or hydrochloric acid, flood rear suction filtration, under the condition of 90 DEG C, be dried to water content be again less than 2%, then be placed in calcining furnace and calcine 2h, calcining temperature controls, at 1050 DEG C, to obtain pretreated diatomite, stand-by;
C. diatomite and micropowder silica gel co-grinding: above-mentioned pretreated diatomite is mixed with micropowder silica gel, being placed in pulverizer, to be crushed to particle fineness be 1.1 millimeters, then add polyaniline derivative macromolecular material, mixing, stand-by;
(4) mixing granulation:
Oxygen-supplying component good for step (1) to (3) pre-treatment, Chinese medicine composite parts, adsorption component are placed in mixing machine, add coating agent water-borne acrylic resin, stablizer adipic acid and sustained release dosage sodium alginate more successively, mix, obtain oxygenation agent compound; By oxygenation agent compound through granulation, polishing, screening, oven dry, i.e. the compound oxygenation agent of obtained absorption aquaculture water residual antibiotic.
Embodiment 3
A kind of compound oxygenation agent adsorbing aquaculture water residual antibiotic of the present embodiment, is prepared from by the component of following weight part:
Oxygen-supplying component 90 parts, Chinese medicine composite parts 25 parts, adsorption component 68 parts, water-borne acrylic resin 5 parts, water glass 3 parts, ethyl cellulose 1.8 parts; Wherein, described oxygen-supplying component comprises 60 parts of sodium carbonate peroxides, 30 parts of calcium peroxides; Described Chinese medicine composite parts is prepared from by pilewort, Radix Angelicae Sinensis, the Radix Astragali, nephelium lappaceum, lotus pod, Leaf and twig of Fruticose Breynia, Root of Sstrigose Hydrangea and yucca; Described adsorption component comprises 30 parts of medical stones, 10 parts of polyaniline derivative macromolecular materials, 15 parts of diatomite and 13 parts of micropowder silica gels.
Its concrete preparation method is as follows:
(1) oxygen-supplying component pre-treatment:
A. SPC-D process: SPC-D is placed in Universalpulverizer pulverizing and makes the SPC-D pulvis that particle fineness is 0.5 millimeter, stand-by;
B. calcium peroxide process: be evenly sprayed into the water relative to its weight 14% in calcium peroxide, mix, obtain calcium peroxide wet feed, stand-by;
(2) Chinese medicine composite parts pre-treatment:
A. pilewort process: complete for pilewort being placed in temperature is that the clear water of 40 DEG C cleans up, being placed on temperature is again toast 20min in the baking oven of 90 DEG C, then oven temperature to 140 DEG C is adjusted, continue baking 30min, the pilewort of drying is pulverized with pulverizer, cross 180 mesh sieves, the sieve end, continues to employ, compass screen surface returns pulverizer and pulverizes, and obtains pilewort powder, stand-by;
B. Radix Angelicae Sinensis process: Radix Angelicae Sinensis is placed in the warm water immersion treatment 60min that temperature is 55 DEG C, being placed in boiler again under the temperature condition of 120 DEG C decocts 150min, cooled and filtered, obtain the aqueous extract of Radix Angelicae Sinensis, concentrating under reduced pressure becomes relative density under 80 degrees celsius to be the medicinal extract of 1.24, spraying dry makes eumenol powder again, stand-by;
C. Radix Astragali process: the Radix Astragali being placed in temperature is process 30min at the temperature of 70 DEG C, being placed on temperature is again process 20min at the temperature of 90 DEG C, adjust again temperature be 180 DEG C by moisture content process to 3% in the Radix Astragali time, be placed on grinding machine for grinding powdered, can Milkvetch Root be obtained, stand-by;
D. nephelium lappaceum process: nephelium lappaceum tree root is placed in dryer and adopts temperature to be 90 DEG C to dry to moisture contents to be after 6%, then to be placed in pulverizer and to be ground into 140 object powder, nephelium lappaceum powder can be obtained, stand-by;
E. lotus pod process: cleaned by lotus pod and dry, be placed in slow fire in pot and be fired in coke yellow, cool taking-up, is placed on grinding machine for grinding powdered, can obtain lotus pod powder;
F. Leaf and twig of Fruticose Breynia process: the Leaf and twig of Fruticose Breynia branches and leaves of drying are placed in dryer and dry to moisture content to be 4%, and to be placed in pulverizer and to be ground into 180 object powder, Leaf and twig of Fruticose Breynia powder can be obtained, stand-by;
G. Root of Sstrigose Hydrangea process: Root of Sstrigose Hydrangea is cleaned up, being immersed in concentration is in the alcohol of 70%, and the weight of alcohol used is 14 times of Root of Sstrigose Hydrangea weight, after immersion treatment 10h, take out, then be placed in frying pan, slow fire is fried slowly, to frying thoroughly completely, finally grind powdered into powder, obtain Root of Sstrigose Hydrangea powder, stand-by;
H. yucca process: fresh yucca is placed in baking oven and dries, pulverize through pulverizer, cross 60 mesh sieves, obtain dry yucca powder, be the ethanolic soln that 1:70 adds 80% according to solid-to-liquid ratio, be placed in microwave oven and carry out microwave extraction, microwave power is 300W, extraction time is 25s, then decompress filter, obtain the ethanolic soln of yucconin, further concentrating under reduced pressure, heating evaporation removes ethanol, be cooled to room temperature, distilled water and acetone soln is added in the ratio of 1:1:0.8 in above-mentioned gained concentrated solution, carry out separation and purification, concentrating under reduced pressure again, heating evaporation removes acetone and distilled water, obtain yucca extract solid particulate, stand-by,
Gained pilewort powder, eumenol powder, Milkvetch Root, nephelium lappaceum powder, lotus pod powder, Leaf and twig of Fruticose Breynia powder, Root of Sstrigose Hydrangea powder and yucca extract solid particulate are mixed by weight for 1:1.5:1:2:2:3:1:0.5, obtains Chinese medicine composite parts.
(3) adsorption component pre-treatment:
A. medical stone process: by natural medical stone through screening, pulverize, be processed into maifanite powder with rubbing down nodulizer, its particle fineness is 1.5 millimeters, stand-by;
B. diatomite process: acidic solution diatomite being placed in 55 DEG C floods 5h, described acidic solution is nitric acid, sulfuric acid or hydrochloric acid, flood rear suction filtration, under the condition of 100 DEG C, be dried to water content be again less than 2%, then be placed in calcining furnace and calcine 3h, calcining temperature controls, at 1100 DEG C, to obtain pretreated diatomite, stand-by;
C. diatomite and micropowder silica gel co-grinding: above-mentioned pretreated diatomite is mixed with micropowder silica gel, being placed in pulverizer, to be crushed to particle fineness be 1.2 millimeters, then add polyaniline derivative macromolecular material, mixing, stand-by;
(4) mixing granulation:
Oxygen-supplying component good for step (1) to (3) pre-treatment, Chinese medicine composite parts, adsorption component are placed in mixing machine, add coating agent water-borne acrylic resin, stablizer water glass and sustained release dosage ethyl cellulose more successively, mix, obtain oxygenation agent compound; By oxygenation agent compound through granulation, polishing, screening, oven dry, i.e. the compound oxygenation agent of obtained absorption aquaculture water residual antibiotic.
The measure of merit of the compound oxygenation agent of embodiment 1 ~ 3 gained absorption aquaculture water residual antibiotic is as follows:
1. experimental subjects: choose the carp culture circle that 4 place's conditions are identical, average depth 3.0-3.5m, fry weight in average is 100g/ head, and density is at 14-18 head/m
3.1,2, No. 3 circles are experimental group (the compound oxygenation agent of the absorption aquaculture water residual antibiotic using the present invention to prepare), and No. 4 circles are control group (the compound oxygenation agent of the absorption aquaculture water residual antibiotic not using the present invention to prepare).
2. experimental technique: experimental group 1,2,3 is except the compound oxygenation agent of the absorption aquaculture water residual antibiotic prepared by embodiment 1,2,3 of regularly splashing respectively, and feed mode is the same with control group with management process.Experimental period be in August, 2014 to October, 60 days by a definite date, experimental group was splashed 1 time every 3 days, and the amount of splashing is 200g/m
3, experimental session, periodic detection water quality, observes carp and to ingest situation, every 15 all over the world water touch spy, measure carp body weight.
3. experimental data:
(1) the water quality data index extracting experimental group and control group the 30th day and the 60th day is respectively as shown in table 1:
Table 1: each every water-quality guideline data cultivating circle the 30th day and the 60th day
(2) the mean body weight growth pattern of experimental session experimental group and control group cultivation circle carp as shown in Figure 1.
Result as can be seen from table 1 and Fig. 1: the compound oxygenation agent of absorption aquaculture water residual antibiotic of the present invention, can fast and stably oxygenation, remove the microbiotic in water body, obvious decontamination effect improving is had to the water quality of aquaculture water, significantly can reduce the content of the objectionable impuritiess such as ammonia nitrogen, nitrite, hydrogen sulfide, improve the Quality and yield of aquatic animal.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (7)
1. adsorb a compound oxygenation agent for aquaculture water residual antibiotic, it is characterized in that: be prepared from by the component of following weight part:
Oxygen-supplying component 70 ~ 90 parts, Chinese medicine composite parts 15 ~ 25 parts, adsorption component 42 ~ 68 parts, coating agent 2 ~ 5 parts, stablizer 1 ~ 3 part, slowly-releasing solubility promoter 1.3 ~ 1.8 parts;
Wherein, described oxygen-supplying component comprises 50 ~ 60 parts of sodium carbonate peroxides and 20 ~ 30 parts of calcium peroxides; Described Chinese medicine composite parts comprises pilewort, Radix Angelicae Sinensis, the Radix Astragali, nephelium lappaceum, lotus pod, Leaf and twig of Fruticose Breynia, Root of Sstrigose Hydrangea and yucca; Described adsorption component comprises 20 ~ 30 parts of medical stones, 6 ~ 10 parts of macromolecular materials, 9 ~ 15 parts of diatomite and 7 ~ 13 parts of micropowder silica gels.
2. a kind of compound oxygenation agent adsorbing aquaculture water residual antibiotic according to claim 1, is characterized in that: the content of pilewort in described Chinese medicine composite parts, Radix Angelicae Sinensis, the Radix Astragali, nephelium lappaceum, lotus pod, Leaf and twig of Fruticose Breynia, Root of Sstrigose Hydrangea and yucca is than being 1:1.5:1:2:2:3:1:0.5.
3. a kind of compound oxygenation agent adsorbing aquaculture water residual antibiotic according to claim 1, is characterized in that: described coating agent is macromolecule film former or water-borne acrylic resin; Described stablizer is acetanilide N, adipic acid or water glass; Described slowly-releasing solubility promoter is sodium alginate or ethyl cellulose; Described macromolecular material is polyaniline derivative macromolecular material.
4. a kind of preparation method of adsorbing the compound oxygenation agent of aquaculture water residual antibiotic described in any one of claims 1 to 3, is characterized in that comprising following preparation process:
Oxygen-supplying component, Chinese medicine composite parts and adsorption component are put into mixing machine after pretreatment, then adds coating agent, stablizer and slowly-releasing solubility promoter successively, mix, obtain oxygenation agent compound; By oxygenation agent compound through granulation, polishing, screening, oven dry, i.e. the compound oxygenation agent of obtained absorption aquaculture water residual antibiotic.
5. a kind of preparation method of adsorbing the compound oxygenation agent of aquaculture water residual antibiotic according to claim 4, is characterized in that described oxygen-supplying component before use through following pre-treatment:
SPC-D process: SPC-D is placed in Universalpulverizer and pulverizes the SPC-D pulvis making particle fineness≤0.5 millimeter;
Calcium peroxide process: be evenly sprayed into the water relative to its weight 8% ~ 14% in calcium peroxide, mix, obtain calcium peroxide wet feed.
6. a kind of preparation method of adsorbing the compound oxygenation agent of aquaculture water residual antibiotic according to claim 4, is characterized in that described Chinese medicine composite parts prepares by the following method:
Pilewort process: complete for pilewort being placed in temperature is that the clear water of 30 ~ 40 DEG C cleans up, being placed on temperature is again toast 12 ~ 20min in the baking oven of 80 ~ 90 DEG C, then oven temperature to 120 ~ 140 DEG C are adjusted, continue baking 25 ~ 30min, pulverized with pulverizer by the pilewort of drying, cross 150 ~ 180 mesh sieves, the sieve end, continues to employ, compass screen surface returns pulverizer and pulverizes, and obtains pilewort powder;
Radix Angelicae Sinensis process: Radix Angelicae Sinensis is placed in warm water immersion treatment 40 ~ 60min that temperature is 35 ~ 55 DEG C, be placed in boiler again and decoct 90 ~ 150min under the temperature condition of 90 ~ 120 DEG C, cooled and filtered, obtain the aqueous extract of Radix Angelicae Sinensis, concentrating under reduced pressure becomes relative density under 80 degrees celsius to be the medicinal extract of 1.06 ~ 1.24, then spraying dry makes eumenol powder;
Radix Astragali process: the Radix Astragali being placed in temperature is process 20 ~ 30min at the temperature of 40 ~ 70 DEG C, being placed on temperature is again process 10 ~ 20min at the temperature of 70 ~ 90 DEG C, adjust again temperature be 130 ~ 180 DEG C by moisture content process to 1 ~ 3% in the Radix Astragali time, be placed on grinding machine for grinding powdered, can Milkvetch Root be obtained;
Nephelium lappaceum process: nephelium lappaceum tree root is placed in dryer and adopts temperature to be 80 ~ 90 DEG C to dry to moisture contents to be after 4 ~ 6%, then to be placed in pulverizer and to be ground into 130 ~ 140 object powder, nephelium lappaceum powder can be obtained;
Lotus pod process: cleaned by lotus pod and dry, be placed in slow fire in pot and be fired in coke yellow, cool taking-up, is placed on grinding machine for grinding powdered, can obtain lotus pod powder;
Leaf and twig of Fruticose Breynia process: the Leaf and twig of Fruticose Breynia branches and leaves of drying are placed in dryer and dry to moisture content to be 2 ~ 4%, and to be placed in pulverizer and to be ground into 150 ~ 180 object powder, Leaf and twig of Fruticose Breynia powder can be obtained;
Root of Sstrigose Hydrangea process: Root of Sstrigose Hydrangea is cleaned up, being immersed in concentration is in the alcohol of 50 ~ 70%, the weight of alcohol used is 8 ~ 14 times of Root of Sstrigose Hydrangea weight, after immersion treatment 6 ~ 10h, take out, then be placed in frying pan, slow fire is fried slowly, to frying thoroughly completely, finally grinding powdered into powder, obtaining Root of Sstrigose Hydrangea powder;
Yucca process: fresh yucca is placed in baking oven and dries, pulverize through pulverizer, cross 60 mesh sieves, obtain dry yucca powder, be the ethanolic soln that 1:60 ~ 70 add 75 ~ 80% according to solid-to-liquid ratio, be placed in microwave oven and carry out microwave extraction, microwave power is 300W, extraction time is 20 ~ 25s, then decompress filter, obtain the ethanolic soln of yucconin, further concentrating under reduced pressure, heating evaporation removes ethanol, be cooled to room temperature, distilled water and acetone soln is added in the ratio of 1:1:0.8 in above-mentioned gained concentrated solution, carry out separation and purification, concentrating under reduced pressure again, heating evaporation removes acetone and distilled water, obtain yucca extract solid particulate,
Gained pilewort powder, eumenol powder, Milkvetch Root, nephelium lappaceum powder, lotus pod powder, Leaf and twig of Fruticose Breynia powder, Root of Sstrigose Hydrangea powder and yucca extract solid particulate are mixed by weight for 1:1.5:1:2:2:3:1:0.5, obtains Chinese medicine composite parts.
7. a kind of preparation method of adsorbing the compound oxygenation agent of aquaculture water residual antibiotic according to claim 4, is characterized in that described adsorption component before use through following pre-treatment:
Medical stone process: by natural medical stone through screening, pulverizes, and is processed into the maifanite powder of particle fineness≤1.5 millimeter with rubbing down nodulizer;
Diatomite process: acidic solution dipping 3 ~ 5h diatomite being placed in 50 ~ 55 DEG C, described acidic solution is nitric acid, sulfuric acid or hydrochloric acid, flood rear suction filtration, under the condition of 80 ~ 100 DEG C, be dried to water content be again less than 2%, then calcining furnace calcining 1 ~ 3h is placed in, calcining temperature controls, at 1000 ~ 1100 DEG C, to obtain pretreated diatomite;
Diatomite and micropowder silica gel co-grinding: above-mentioned pretreated diatomite is mixed with micropowder silica gel, is placed in pulverizer and is crushed to particle fineness≤1.2 millimeter, then add macromolecular material and mix.
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