CN1074203A - Compound organic fertilizer containing multiple bacterial spawns and method for making thereof - Google Patents

Compound organic fertilizer containing multiple bacterial spawns and method for making thereof Download PDF

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CN1074203A
CN1074203A CN93100027A CN93100027A CN1074203A CN 1074203 A CN1074203 A CN 1074203A CN 93100027 A CN93100027 A CN 93100027A CN 93100027 A CN93100027 A CN 93100027A CN 1074203 A CN1074203 A CN 1074203A
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containing multiple
organic fertilizer
fertilizer containing
spawns
compound organic
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CN1030761C (en
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郑国华
李元芳
卢浩余
许有森
任正柯
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A40/00Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
    • Y02A40/10Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
    • Y02A40/20Fertilizers of biological origin, e.g. guano or fertilizers made from animal corpses

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Abstract

What the present invention relates to is a kind of compound organic fertilizer containing multiple bacterial spawns, carry out the repeatedly cultivation of liquid-solid two-phase respectively by each bacterial classification, mix with organism, inorganic mineral and small amounts of water soluble salt with certain proportion then, form compound organic fertilizer containing multiple bacterial spawns at last, its advantage is antagonism not to take place, the viable count abundance, the improvement that helps environment also can provide and promote the raising of soil fertility.

Description

Compound organic fertilizer containing multiple bacterial spawns and method for making thereof
What the present invention relates to is a kind of biological organic complex fertilizer, and especially, biological organic complex fertilizer of the present invention is formed by many bacterial classifications; And the method for making above-mentioned biological organic complex fertilizer.
In the prior art, utilize the example of organic waste manufacturing composite bio-fertilizer as follows:
At CN91107966.1 on July 22nd, 92 disclosed specification sheets, the applicant has described a kind of complete compound fertilizer, it is that employing organic waste materials and agriculture and animal husbandry by-product waste material are main raw material, this patent particularly points out, in the fermenting process of raw material, there is multiple microorganism to participate in, in the fertilizer innocent treatment procedure, still has multiple microorganism.
At CN89108541.6 on October 3rd, 90 disclosed specification sheets, the applicant has mentioned a kind of biochemical compound fertilizer and method for making, it is that nitrobacteria and the rotten bacterium of potassium introduced in domestic refuse through enlarged culturing carry out decomposing and fermenting, a certain amount of inorganic fertilizer of refining back fusion.
In DE3800814.9, the applicant discloses a kind of utilize mud and some other waste material fusion, introduces microorganism where necessary, packs the pollution with preventing heavy metal then.
In CN90106002.X, the applicant has described a kind of composite bio-fertilizer and method for making thereof, it is to add a kind of vinelandii in common mixing fertilizer, granulation and coat phosphorus mixture then at particle surface, be characterized in stable storing, but it only is a kind of anaerobic nitrogen-fixation bacterium, and the kind of unexposed used vinelandii.
In CN92101990.4, the applicant has described a kind of production method of composite organic bacterial fertilizer, and what it adopted is fermentation and sterilization, and liquid phase adds vinelandii, last granulation.
In the described bio-feritlizer of prior art, exist following deficiency: 1) bacterial classification is single; 2) described bacterial classification does not have concrete subject, therefore can not embody whether used the most great-hearted bacterial classification, perhaps discloses insufficient; 3) generally all adopt single liquid phase to cultivate, can cause antagonism like this.
Main purpose of the present invention is to provide a kind of compound organic fertilizer containing multiple bacterial spawns of repeatedly cultivating through liquid-solid two-phase that can not produce antagonistic action.
Another object of the present invention is to provide a kind of can effectively utilize organic waste, and through the preparation of the method for the invention, it is the composite bio-fertilizer of organic waste that a kind of major ingredient is provided.
A further object of the invention provides a kind of method of making above-mentioned composite bio-fertilizer.
Simple procedure of the present invention is as follows: each bacterial classification is carried out liquid phase respectively cultivate, adsorb with the peat composed of rotten mosses then, to carry out solid phase with the inoculum agent of microorganism cultivates, in the solid-liquid two-phase is cultivated, can repeatedly enlarge, last organism and mineral substance and micro-water-soluble salt with through fermenting mixes, or with powdery, or with granular formation compound organic fertilizer containing multiple bacterial spawns of the present invention.
Be described in detail the present invention below.
Because industrial or agricultural and townie waste are more and more, how to handle these wastes and become the problem that those skilled in the relevant art in recent ten years make earnest efforts studying, present result of study shows, part-organic waste in these wastes can become useful thing after suitably handling, comprising fertilizer of the present invention.Described here can comprise animal excrement, biological residual body and Humus thereof as the raw material of fertilizer of the present invention, the nubbin of plant, particularly, they are animal excrement, fur, scale, bone meal, wheat bran, rice bran, domestic waste, the straw in rural area, corn cob, the weathered coal that nature exists, brown coal, turfy soil, marsh mud or the like.In composite fertilizer of the present invention, these organic wastes account for more than 60% of raw material total amount, and their roles are as the nutriment of inoculum agent solid culture and the energy, and play fertilizer.
In order to realize the multi-functional and efficient of this fertilizer; in making and using, play protection, suction, insulation simultaneously; also comprise the mineral additive that accounts for total amount 6-40% in composite fertilizer of the present invention, they are vermiculite, zeolite, diatomite, ground phosphate rock, potassium breeze, Wingdale and boron, molybdenum, zinc, magnesium and rare-earth mineral material.
In the manufacturing of biological organic complex fertilizer of the present invention or can play the chemical additive of stimulation or nutriment effect in using, they are boric acid, zinc sulfate, ammonium molybdate, potassium primary phosphate and agricultural rare-earth.
If use at special geology, also should add a small amount of corresponding additive, as in the arid area, can add a spot of wetting Agent for Printing Inks, they are macromolecular material normally, the High hydrophilous resin of making as treated starch etc.
Unless otherwise indicated, described herein per-cent and umber all are meant weight.
Before preparation composite bio-fertilizer of the present invention, to tackle various raw materials and carry out pre-treatment, this is to make raw material meet the step of service requirements, if raw material is satisfactory, this preprocessing process can partly or entirely be cancelled.
Organic pre-treatment comprised select materials, pulverize and sterilize.At first to select not mouldy organism, organic waste after selected are dried pulverizing, about 60~120 orders of the fineness of crushing rear material, except that fresh wheat bran, rice bran and slag, straw, corn cob and sawdust, other organic waste all will be handled to reach environmental protection requirement through sterilization, for example, the processing requirements of municipal wastes should reach " the agricultural control criterion of GB8172-87 townm refuse " that country formulates.
Employed inorganic mineral in biological composite of the present invention requires its fineness more than 120 orders, and wherein phosphorus, potassium and limestone mine should be thin as much as possible; Owing to need the potassium phosphorus composition in the composite bio-fertilizer of the present invention, therefore will select the high ore of those potassium phosphorus contents for use.Used vermiculite should pass through high temperature puffing.
After having finished above-mentioned preparation work, we will further specify detailed technology content of the present invention by preparation process.
At first, we are in the production technique of this narration inoculum agent.
What the present invention relates to is a kind of compound organic fertilizer containing multiple bacterial spawns, many bacterial classifications described here, at least comprise 5 bacterial classifications, as foregoing, many bacterial classifications and make that antagonism does not take place between them is principal character of the present invention, 5 bacterial classifications (bacterial classification described in the present invention provides by the Chinese Academy of Agricultural Sciences's clay fertilizer) used in the biological organic complex fertilizer of the present invention are meant:
A bacterium-Bacillus megatherium (Bacillus megatherium de Bary), code name 10010-88, its feature has:
1. big bacillus 5-6 * 1.8-2 micron
2. cell in pairs or chaining, do not move
3. can divide Jie's phosphatide and nucleic acid
4. can increase the content (reaching 9 milligrams Vanadium Pentoxide in FLAKES in the 100 gram soil) of soluble phosphoric acid in the soil
1 liter of consumption of a bacterium culture medium prescription
Glucose: 10g
NaCl: 0.3g
MnSO4·4H2O 0.03g
(NH4)2SO4 0.5g
KCl: 0.3g
FeSO4·7H2O: 0.03g
CaCO3: 5g
MgSO4·2H2O: 0.3g
Yelkin TTS: 0.2g
No. two bacterium-potassium bacteriums, its code name 10012-88 can carry out branch Jie, discharge potassium, phosphorus and other ash element, improve the nutritional condition of crop potassic manosil AS of mica, feldspar etc. in the soil and phosphatic rock, and it comprises:
Colloid bacillus (Bac.mucilaginosus)
Fixed nitrogen bacillus (Bac.Azotofaxans)
1. aerobic bacteria, the long 4-7 micron of thalline, wide 1 micron
2. pod membrane is arranged, have only one sometimes, 2-3 is arranged sometimes together with the long 7-10 micron of pod membrane, wide 5-6 micron, pod membrane.
3. Gram-negative
4. have Jie's potassium, Jie's phosphorus ability
5. has certain nitrogen fixing capacity (utilizing 1 gram sugar can fix 1.3 milligrams of nitrogen)
6. secretion physiologically active substance, promotion plant growth.
1 liter of consumption of No. two bacterium culture medium prescriptions
Sucrose: 5g
K2HPO4:?2
(NH4)2SO4: 1
MgSO4·2H2O: 0.5
FeCl3: 0.2
CaCO3: 0.1
Yeast powder: 0.2
PH 7.2-7.4
No. three bacterium-nitrogen-fixing rhizobias (Azorhizobium Caulinadans ORS571), its code name 571-89, its feature is as follows:
1. dialister bacterium 0.5-0.6 * 1.5-2.5 micron
2. gram negative reaction
3. can move, give birth to admittedly flagellum (solid culture) or adnation flagellum (liquid culture)
4. give birth to type, Dai Shiwei 3-6 hour soon
5. special nitrogen fixation efficiency is arranged, in nitrogen-free agar, with nitrogen in the air such as only nitrogen source well-grown, the fixed nitrogen rate be 300-400 nM ethene/milligram butt/hour.
1 liter of consumption of No. three bacterium culture medium prescriptions
Sodium.alpha.-hydroxypropionate: 10 grams
The K2HPO4:1.67 gram
The KH2PO4:0.87 gram
NaCl: 0.05g
CaCl2: 0.04g
FeCl3: 0.004g
MgSO4·2H2O: 0.1g
Yeast powder: 1g
No. four bacterium-azotobacters (azotobacter chroococcum Azotobacter Chroococcum), its code name 10087-88, its feature is as follows:
1. aerobic bacteria, rod-short are oval or approximate spherical
Peritrichous, can move actively
3. do not sprout born of the same parents, cymbidium Albert'stain Albert feminine gender
4. sticking thick-walled pod film can make colony color by chromogenesis
5. oxidation one gram energy matter can gather nearly 30 milligrams nitrogen
6. can secrete VITAMIN and growth system, stimulate crop growth and strengthen the vital movements of other rhizospheric microorganisms, promote the mineralization of soil organic substance, supply with plant ashes nutriment thereby impel
1 liter of consumption of No. four bacterium culture medium prescriptions
KH2PO4: 0.2g
MgSO4·2H2O: 0.2g
NaCl: 0.2g
CaSO4·2H2O: 0.1g
CaCO3: 5g
N.F,USP MANNITOL: 10g
No. five bacterium-combination azotobacters (Klebsiella pneumonial), its code name 549-89, its feature is as follows:
1. atrichia or a few cell have polar flagella
2. there is pod membrane that nitrogenase is had provide protection
3. can utilize monose, disaccharide as carbon source, be that growth is vigorous on the nitrogen-free agar of sole carbon source with glucose or sucrose
4. rely on the rhizospheric environment life, the growth development to crop produces certain influence again, and forms united symbiosis fixed nitrogen relation between the two with crop
1 liter of consumption of No. five culture medium prescriptions
Glucose: 5g
KH2PO4: 0.4g
K2HPO4: 0.1g
MgSO4·2H2O: 0.2g
NaCl: 0.1g
CaCl2: 0.02g
FeCl3: 0.01g
Yeast powder: 0.5g
Na2MoO4: 0.002g
These 5 test tube strains utilize separately culture medium culturing after 1~2 day in 25~20 ℃ shaking table, utilize fermentation to carry out deep liquid respectively again and cultivate, and adsorb with turfy soil then, have so just finished primary liquid phase and have cultivated.
Next the dissolved stimulant is added in wheat bran and other the unfermentable organism, add above-mentioned inoculum agent then separately, mix, mixture was cultivated 1-2 days under 25~30 ℃ condition, and Here it is, and solid fermentation is cultivated, in the cultivation of solid-liquid two-phase, can carry out repeatedly enlarged culturing, after finishing above-mentioned steps, add vermiculite absorbent respectively and stir, so just obtained containing material-microbial inoculum component of microorganism.
The organic preparation of another main component of the present invention is like this, with organic matter fermentation, mixing a certain amount of dissolved trace element stirs, in whipping process, add reodorant, if desired, can in abovementioned steps, add this operation of the grey bacterium of oven dry, the material after the oven dry is crushed to 60~120 orders.
In addition ground phosphate rock and other inorganic mineral also being crushed to certain fineness, is thin more good more in principle, should be higher than 120 orders usually.
Material, the fermented organic behind the drying and sterilizing and the inorganic mineral that will contain bacterial classification is by following mixed:
Organic content accounts for more than 60% of total amount;
Mineral substance accounts for the 6-40% of total amount;
Stimulant accounts for 0.15~0.2% of total amount.
In practice, also should add a spot of water-soluble inorganic salt, the add-on of water-soluble inorganic salt be about total amount 1.5% or still less.Because the existence of water-soluble inorganic salt can threaten the survival of bacterial classification, therefore, when mixing, bacterial classification and water-soluble inorganic salt should be adsorbed with adsorptive respectively, so just can avoid the injury of water-soluble inorganic salt pair bacterial classification, can make to allow to allocate into the more trace element of volume in the fertilizer.
In general formulation, the proportioning of organism each component is as follows:
Wheat bran about 10%;
Chicken manure about 20%;
Soya-bean cake about 5%;
Turfy soil about 30%;
The better proportioning of each component comprises in the inorganic mineral:
Ground phosphate rock about 15~25%;
The about 3-7% of vermiculite (protective material);
The about 2-5% of zeolite (reodorant);
Zinc sulfate about 0.1~0.3%.
Foregoing stimulant comprises the ammonium molybdate that accounts for total amount 0.04~0.06.%, about 0.08~0.12% potassium primary phosphate, and about 0.02~0.06% rare earth element.Stimulant can also use corresponding mineral substance, such as: can replace aforesaid ammonium molybdate, potassium primary phosphate and rare earth element with rare-earth mineral, molybdenum ore powder and ground phosphate rock.
Inoculum agent (peat composed of rotten mosses absorption) accounts for the 2-5% of total amount.
Be each concrete composition shared general ratio in composite bio-fertilizer of the present invention above, in addition, in needs, can add an amount of water, water is mainly used to dissolve stimulant and various element additive in composite bio-fertilizer of the present invention, also be used for regulating the water content of fermented product in addition, the ratio of concrete water consumption, those skilled in the art can determine according to prior art or experience.
The compound organic fertilizer containing multiple bacterial spawns of preparing as stated above under above-mentioned formulation principle instructs, through a large amount of trying out, obvious effect of increasing production specifically please be seen table 1, table 2 and table 3.
Solarium, Chinese Academy of Agricultural Sciences Beijing pot rice, millet test, observed and recorded the paddy seedling give birth to, tiller, Cheng Sui, biological character, output (comprising the upperground part biomass, harvesting time cauline leaf output, heavy, the seed ultimate production of fringe) reach significantly or utmost point remarkably influenced, gather in the crops grain yield at last and see Table 1:
Table 1
Paddy rice millet
Grain yield and CR contrast grain yield and CR contrast
(gram/basin) stimulation ratio (%) (gram/basin) stimulation ratio (%)
1. chemical fertilizer 289.98 27.87 51.38 9.32
2. green friendly 100kg/ mu+chemical fertilizer 314.76 38.80 57.88 23.15
3. green friendly 50kg/ mu+chemical fertilizer 313.49 38.24 56.28 19.75
4. green friendly 50kg/ mu+1/2N+P 304.76 34.38 55.25 17.55
5. green friendly 50kg/ mu+1/3N+P 285.98 26.10 51.38 9.33
6. green friendly 50kg/ mu+N+1/2P 281.41 24.09 51.38 9.33
7. green friendly 50kg/ mu+N+1/3P 265.14 16.91 51.18 8.89
8. green friendly 50kg/ mu 242.39 6.88 50.33 7.09
9.CK 226.78 47.00
Edge friend's fertilizer is used in hot spring agrotechnical station, Jiangpu, table 2. Nanjing and chemical fertilizer relatively influences output of cotton
Base manure output (jin/mu) stimulation ratio (%) of topdressing
1. chemical fertilizer (40 jin/mu 67.2 in 80 jin of/mu urea of carbon ammonium
50 jin/mu in phosphate fertilizer)
2. green friendly 100 jin/mu+1/3 chemical fertilizer the same 83.2 23.8
3. green friendly 200 jin/mu+1/2 chemical fertilizer the same 97.8 45.5
4. green friendly 300 jin/mu the same 111.2 65.5
The table 3. Fengtai District, Beijing City institute of agricultural sciences uses green friendly fertilizer in vegetables effect of increasing production cartogram
Cucumber eggplant Chinese cabbage radish
A B A B A B A B
Green friendly 100 kilograms/mu 2,055 35% 1,865 70.3% 12,793 19% 7,465 27.5%
Public fertile (NP) 1,780 17% 1,435 31% 11,793 9.7% 6,215 6.15% of equal value
CK (blank) 1,520 1,095 10,750 5855
* A is output (a jin/mu) in the table, and B is a stimulation ratio.
Compound organic fertilizer containing multiple bacterial spawns of the present invention is a kind of non-harmful biological activity fertilizer; because it contains abundant organic matter, natural mineral nutrient, beneficial trace elements and effective stimulant and protective material; and solid-liquid two-phase repeatedly enlarged culturing and the composite operation of final blending have been adopted; therefore, improve the soil physical chemistry performance, transform organic-inorganic nutriment stimulate crop to germinate and healthy and strong growth disease resistance enhancemen aspect all come effectively than the bio-fertilizer of other single culture.Surprisingly, adopt the present invention to mix seed dressing with the bacterial classification after the careless carbon absorption respectively, significant effect of increasing production is also arranged.
Technology of the present invention except above-mentioned rapid, also should satisfy following requirement:
1.5 the liquid of individual bacterial classification, solid culture all will be carried out respectively, all are aerobic fermentations.
2. each bacterial classification all is the special culture media that adopts respectively separately.The cultivation that solid fermentation is cultivated all is same organic matter, and inoculum agent production can also can be through the level Four fluid enlargement culture through three grades.
4. the fertilizer finished product is produced, only through the one-level solid culture.
5. in the solid culture stage, the dissolving water consumption of stimulant will reach the water content that makes its suitable fermentation in the adding organism, is about 1/4 of fermented product.
6. stimulant potassium primary phosphate, rare earth, ammonium molybdate will dissolve, add respectively organism respectively.Ammonium molybdate can add behind solid fermentation.
7. to require PH before connecing bacterium be 7 to the solid fermentation thing, and moisture is 25~30%.
8. the raw materials quality height can all lump together and carry out solid fermentation, even after the venting bags of can directly packing into lets alone freely to ferment, can use.
Following index should be strictly controlled in the detection of compound organic fertilizer containing multiple bacterial spawns of the present invention,
Effective total viable count 〉=200,000,000/gram;
Organic content 〉=35%;
Acidity-basicity ph value 6.5~7;
Moisture content 10-15%;
Effectively store 1 year.
Advantage of the present invention and technical characterictic are described in detail in front; technical characterictic of the present invention or protection domain embody in the claims; but; claim provided by the present invention is not as a limitation of the invention, everyly utilizes any work of being done of notion of the present invention all will be among protection scope of the present invention.

Claims (12)

1, a kind of compound organic fertilizer containing multiple bacterial spawns, it is made up of a plurality of bacterial classifications, organism, inorganic mineral and a small amount of additive, it is characterized in that containing at least in the described compound organic fertilizer containing multiple bacterial spawns 5 bacterial classifications, contain effective viable count greater than 200,000,000 in the every gram composite fertilizer, organic content should be more than or equal to 35%, the pH value of composite fertilizer is between 6-7, and water content is about 8-20%.
2, the described many strain bios of claim 1 composite fertilizer is characterized in that described bacterial classification comprises Bacillus megatherium, potassium bacterium, nitrogen-fixing rhizobia, azotobacter and combination azotobacter.
3, the described potassium bacterium of claim 2 is meant colloid bacillus and fixed nitrogen bacillus.
4, the described azotobacter of claim 2 is meant the brown vinelandii in garden.
5, the described compound organic fertilizer containing multiple bacterial spawns of claim 1 is characterized in that pH value is about 6.5-7.
6, the described compound organic fertilizer containing multiple bacterial spawns of claim 1 is characterized in that the moisture about 10-15% of this composite fertilizer.
7, the described compound organic fertilizer containing multiple bacterial spawns of claim 1 is characterized in that organic content accounts for more than 60% of total amount in the compound organic fertilizer containing multiple bacterial spawns, and mineral substance accounts for the 6-40% of total amount, and stimulant accounts for 0.15~0.2% of total amount; Described organism each component generally includes:
Wheat bran about 10%;
Chicken manure about 20%;
Soya-bean cake about 5%;
Turfy soil about 30%;
Described inorganic mineral generally includes:
Ground phosphate rock about 15~25%;
The about 3-7% of vermiculite (protective material);
The about 2-5% of zeolite (reodorant);
Zinc sulfate about 0.1~0.3%;
Foregoing stimulant comprises the ammonium molybdate that accounts for total amount 0.04~0.06.%, about 0.08~0.12% potassium primary phosphate, and about 0.02~0.06% rare earth element, and inoculum agent (peat composed of rotten mosses absorption) accounts for the 2-5% of total amount.
8, claim 1 or 7 described compound organic fertilizer containing multiple bacterial spawns, it is characterized in that the organism in the compound organic fertilizer containing multiple bacterial spawns also comprises animal excrement, fur, scale, bone meal, rice bran, domestic waste, the straw in rural area, corn cob, weathered coal, brown coal, marsh mud that nature exists
9, claim 1 or 7 described compound organic fertilizer containing multiple bacterial spawns is characterized in that mineral additive also comprises mineral substance such as diatomite, potassium breeze, Wingdale and boron, molybdenum, magnesium.
10, claim 1 or 7 described compound organic fertilizer containing multiple bacterial spawns is characterized in that stimulant also comprises boric acid, zinc sulfate.
11, claim 1 or 7 described compound organic fertilizer containing multiple bacterial spawns is characterized in that described additive also comprises a spot of High hydrophilous resin;
12, a kind of method of making the described many strain bios organic double compound of claim 1, comprise and in 25~30 ℃ shaking table, utilize separately culture medium culturing after 1~2 day each test tube strains, utilizing fermentation to carry out deep liquid respectively again cultivates, adsorb with turfy soil then, so just finished the liquid phase cultivation;
Next the dissolved stimulant is added in wheat bran and its unfermentable organism, add above-mentioned microbial inoculum then respectively, mix, mixture solid fermentation under 25~30 ℃ condition was cultivated 1~2 day, in the cultivation of solid-liquid two-phase, can carry out repeatedly enlarged culturing, after finishing above-mentioned steps, add vermiculite absorbent respectively and stir the microbial inoculum that obtains containing microorganism;
With another part organic matter fermentation, mix a certain amount of dissolved trace element and stir, in whipping process, add reodorant, if desired, can in abovementioned steps, add this operation of drying and sterilizing, the material after the oven dry is crushed to 60~120 orders;
In addition ground phosphate rock and other inorganic mineral also are crushed to more than 120 orders;
Material, the fermented organic behind the drying and sterilizing and inorganic mineral and other additive that will contain bacterial classification mix according to the above ratio.
CN93100027A 1993-01-03 1993-01-03 Compound organic fertilizer containing multiple bacterial spawns and preparation thereof Expired - Fee Related CN1030761C (en)

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