CN100566573C - Plant growth regulating antibiotic agent - Google Patents

Plant growth regulating antibiotic agent Download PDF

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Publication number
CN100566573C
CN100566573C CNB2007100248810A CN200710024881A CN100566573C CN 100566573 C CN100566573 C CN 100566573C CN B2007100248810 A CNB2007100248810 A CN B2007100248810A CN 200710024881 A CN200710024881 A CN 200710024881A CN 100566573 C CN100566573 C CN 100566573C
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molecular weight
glucan
less
shitosan
filtrate
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CNB2007100248810A
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CN101084757A (en
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郑典元
邵世光
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LIANYUNGANG HIGHER NORMAL SCHOOL
Lianyungang Normal College
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LIANYUNGANG HIGHER NORMAL SCHOOL
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Abstract

The present invention relates to the conditioning agent and the antibacterial agent of a plant growth, specifically form: sulfated chitosan 5-25 part by following components in part by weight; Sulfonation β-1,3 glucan 5-25 part; Molecular weight is less than shitosan 25-50 part of 50000; Molecular weight is less than β-1,3 glucan or crosslinked β-1,3 glucan 25-50 part of 50000; Superphosphate 5-15 part.This microbial inoculum inducing paddy rice, wheat effectively produces chitinase, β-1, the activity of 3 dextranases and enzyme can improve hundreds of to thousands of times, can effectively prevent and treat wheat, rice disease, remarkable for the early disease effect of preventing and treating wheat, paddy rice when using as seed dressing.

Description

Plant growth regulating antibiotic agent
Technical field
The present invention relates to the conditioning agent and the antibacterial agent of a plant growth, be specifically related to a kind of seed growth regulator and antibacterial agent that is used for seedling cultivation of rice, wheat cultivation stage.
Background technology
The growth regulator of plant has obtained using widely in the production of crops, and it mainly is by regulating the physiological activity of plant, strengthening the resistance of plant, to guarantee the quality of crops.As the agricultural chemicals of antimycotic, the viral infection resistings of crops, because fungi and virus, the effect of most of agricultural chemicals is not very effective, and the scope of application is also limited.Based on above situation, carried out the genetically engineered research of disease resisting rice and other crops in China, and obtained considerable achievement, but paddy rice as Chinese's staple food, people's acceptance is in abstracto still had any problem after the transgenosis, and crops have many outstanding landrace, and this neither the complete soluble problem of transgenic crop.Therefore develop environmental protection and respond well agricultural chemicals still has great real value.
We are on the basis of the Physiology and biochemistry characteristics of research paddy rice and wheat, by simulating common fungal cell wall composition, and fungal infection process, but seek inducing paddy rice, wheat chitinase, β-1, the inducing substance of 3 dextranases, by the synergy of several inducers, strengthen the anti-fungal infection ability of paddy rice, wheat.Utilize chemical synthesis process simultaneously, increase the special groups and the positive electricity number of inducing substance,, play direct disease-resistant bacterium effect to strengthen in conjunction with the ability of virus with fungi.
In China, have little molecular chitosan as plant growth regulator, but with sulfated chitosan, sulfonation β-1,3 glucan and small-molecular weight shitosan, the β of certain molecular weight-1,3 glucans are by composite, and synthetic plant growth regulating antibiotic agent is not seen as yet report.
Along with domestic consumer's improving constantly to food safety requirements.Use synthetic materials such as chemical fertilizer, highly toxic pesticide, chemical preservative in the production of food and the process, more and more do not accepted and use gene engineering and product thereof also to be subjected to consumer's query by people.Reduce the use of highly toxic pesticide as the paddy rice of Chinese's staple food, wheat, increase the use of environmental protection class agricultural chemicals, for production safety food with significant.
Summary of the invention
The purpose of this invention is to provide a kind of plant growth regulating antibiotic agent (HTKT).This microbial inoculum inducing paddy rice, wheat effectively produces chitinase, β-1, the activity of 3 dextranases and enzyme can improve hundreds of to thousands of times, can effectively prevent and treat wheat, rice disease, remarkable for the early disease effect of preventing and treating wheat, paddy rice when using as seed dressing.
The technical solution used in the present invention is:
A kind of plant growth regulating antibiotic agent (HTKT), form by following components in part by weight:
Sulfated chitosan 5-25 part;
Sulfonation β-1,3 glucan 5-25 part;
Molecular weight is less than shitosan 25-50 part of 50000;
Molecular weight is less than β-1,3 glucan or crosslinked β-1,3 glucan 25-50 part of 50000;
Superphosphate 5-15 part.
Plant growth regulating antibiotic agent (HTKT) quality standard sees Table 1:
Table 1 plant growth regulating antibiotic agent (HTKT) quality standard unit (%)
The colour mark Granularity Solvability Moisture Total reducing sugar Coarse ash Ca P
≤65 ≤01mm Solvable ≤0.5 ≥70 ≤20.0 3.0-9.0 ≥4
Each component of above-mentioned antibacterial agent can be made by conventional method, also can be prepared by following method provided by the invention:
Sulfated chitosan:
Shitosan: shrimp, the rinsing of crab shell are clean, shine dry grinding and cross 200 mesh sieves, soak 4-6 hour grease removal deproteinization with the sodium hydroxide solution of the heavy 3-5 of raw material 5%-10% doubly under 85-100 ℃ condition, filter, and drying is washed to neutrality; Hydrochloric acid with the heavy 2-4 of raw material 10%-20% doubly soaked 8-12 hour under 45-85 ℃ of condition, decalcification, filter, dry, when being washed to PH and being 5 left and right sides, adding 2-4 doubly 0.5% potassium permanganate soaked 30 minutes, and the sodium hydrogensulfite with 1%-2% decoloured 30 minutes again, filtration, drying is washed to neutrality, the adding raw material weighs the ethanol of 0.01 times of amount 95%, behind the immersion 1h, adds 40% sodium hydroxide that the heavy 1-2 of raw material doubly measures again, heating using microwave 20min, 90-100 ℃ of control reaction temperature is washed to neutrality, and it is indoor to change sulfonating reaction after the drying over to, under the magnetic agitation situation, feed dry sulfur trioxide, according to the amount control reaction time of reactant, the dry nitrogen of feeding is at last removed unnecessary sulfur trioxide and is got product.
Shitosan (molecular weight is less than 50000):
Shrimp, the rinsing of crab shell are clean, shine dry grinding and cross 200 mesh sieves, soak 4-6 hour grease removal deproteinization with the sodium hydroxide solution of the heavy 3-5 of raw material 5%-10% doubly under 60-80 ℃ condition, filter, and drying is washed to neutrality; Hydrochloric acid with the heavy 2-4 of raw material 10%-20% doubly soaked 8-12 hour under normal temperature condition, decalcification, filter, dry, when being washed to PH and being 5 left and right sides, the adding raw material weighs the ethanol of 0.01 times of amount 95%, after soaking 1h, add 40% sodium hydroxide that the heavy 1-2 of raw material doubly measures again, heating using microwave 20min, 90-100 ℃ of control reaction temperature, be washed to neutrality, add doubly extremely dissolving of 1% hydrochloric acid 50-60 ℃ stirring in water bath of raw material 10-20, add the heavy 0.01-0.001 of raw material cellulose hydrolyzation doubly, through time sampling, detect the molecular weight of shitosan with the Ubbelohde viscometer method, when molecular weight is lower than 50000 hydrolyzate through coarse filtration, 0.45 micron filter membrane micro-filtration, remove impurity, with molecular cut off is the hollow cellulose membrane filtration of 50Kd, removes the incomplete shitosan of degraded, and filtrate is concentrated, after the concentrate drying, be finished product.
β-1,3 glucan (molecular weight is less than 50000):
Source 1------sea-tangle processing sewage adds alkali to 1mol Na 2CO 3, to remove supernatant and sediment, get filtrate and add hydrochloric acid accent pH value to the faintly acid electrodialysis desalination through air supporting, through time sampling, with Ubbelohde viscometer method detection molecules amount, hydrolyzate is through coarse filtration when molecular weight is lower than 50000,0.45 the filter membrane micro-filtration of micron, removing impurity, is the hollow cellulose membrane filtration of 50Kd with molecular cut off, removes degraded incomplete β-1,3 glucans, filtrate is concentrated, after the concentrate drying, be finished product.
Source 2-----gets and sends out full bacterium, and the flat mushroom bacterium bag before the fruiting is behind the homogenate, handle 2h in ultrasonic, most of solid matter is removed in centrifugation, and suction filtration is got filtrate, with 0.65 μ m membrane microfiltration, filtrate adds 37 ℃ of protease (complex enzyme) enzymolysis, and 4-6 hour, through time sampling, with Ubbelohde viscometer detection molecules amount, the hydrolyzate molecular cut off is the hollow cellulose membrane filtration of 50Kd when molecular weight is lower than 50000, removes degraded incomplete β-1,3 glucan, filtrate is carried out concentrating under reduced pressure, concentrate under agitation adds ethanol makes concentration reach 80%, leave standstill 24h after, filter, collecting precipitation, with washing with alcohol 3 times, after the low temperature drying, be finished product.
Crosslinked β-1,3 glucan:
In reactor, add 25 parts of β-1,3 glucans, add 5% sodium hydroxide of 40 parts of volume ratios again, fully stir, keeping temperature is 45 ℃, drips 0.4% epoxychloropropane of 12 parts of volume ratios, keep stirring 3 hours, after reaction finishes, regulate pH value to 6.5 with hydrochloric acid, leave standstill, filter, washing, suction filtration, 50 ℃ of dryings make crosslinked β-1,3 glucan.
Sulfonation β-1,3 glucan:
Get the fully dry finished product of above-mentioned molecular weight (less than 50000) β-1,3 glucan, it is indoor to change sulfonating reaction over to, under the magnetic agitation situation, feed dry sulfur trioxide, according to the amount control reaction time of reactant, the dry nitrogen of feeding is at last removed unnecessary sulfur trioxide and is got product.
Each component fully mixed in proportion promptly obtain the said antibacterial agent of the present invention.
When this microbial inoculum uses as the embedding medium of seed, molecular weight can be passed through crosslinking Treatment in advance less than 50000 β-1,3 glucan component, viscosity and stability to increase plant growth regulating antibiotic agent (HTKT) increase the adhesive force with seed.
Plant growth regulating antibiotic agent of the present invention is used for seedling cultivation of rice, the growth of the seed in wheat cultivation stage.Different prescriptions also can be used for the growth regulating during paddy rice, wheat and other crop growth.Fusarium wilt for rice blast, wheat has certain preventive and therapeutic effect.
Embodiment
The invention will be further described below in conjunction with embodiment.Employed in the present invention term unless other explanation is arranged, generally has the implication of those of ordinary skills' common sense
Embodiment 1: the preparation of agent is used on plant growth regulating antibiotic agent (HTKT) blade face
The preparation of each component:
Sulfated chitosan:
Shitosan: shrimp, the rinsing of crab shell are clean, shine dry grinding and cross 200 mesh sieves, soak 4-6 hour grease removal deproteinization with the sodium hydroxide solution of the heavy 3-5 of raw material 5%-10% doubly under 85-100 ℃ condition, filter, and drying is washed to neutrality; Hydrochloric acid with the heavy 2-4 of raw material 10%-20% doubly soaked 8-12 hour under 45-85 ℃ of condition, decalcification, filter, dry, when being washed to PH and being 5 left and right sides, adding 2-4 doubly 0.5% potassium permanganate soaked 30 minutes, and the sodium hydrogensulfite with 1%-2% decoloured 30 minutes again, filtration, drying is washed to neutrality, the adding raw material weighs the ethanol of 0.01 times of amount 95%, behind the immersion 1h, adds 40% sodium hydroxide that the heavy 1-2 of raw material doubly measures again, heating using microwave 20min, 90-100 ℃ of control reaction temperature is washed to neutrality, and it is indoor to change sulfonating reaction after the drying over to, under the magnetic agitation situation, feed dry sulfur trioxide, according to the amount control reaction time of reactant, the dry nitrogen of feeding is at last removed unnecessary sulfur trioxide and is got product.
Shitosan (molecular weight is less than 50000):
Shrimp, the rinsing of crab shell are clean, shine dry grinding and cross 200 mesh sieves, soak 4-6 hour grease removal deproteinization with the sodium hydroxide solution of the heavy 3-5 of raw material 5%-10% doubly under 60-80 ℃ condition, filter, and drying is washed to neutrality; Hydrochloric acid with the heavy 2-4 of raw material 10%-20% doubly soaked 8-12 hour under normal temperature condition, decalcification, filter, dry, when being washed to PH and being 5 left and right sides, the adding raw material weighs the ethanol of 0.01 times of amount 95%, after soaking 1h, add 40% sodium hydroxide that the heavy 1-2 of raw material doubly measures again, heating using microwave 20min, 90-100 ℃ of control reaction temperature, be washed to neutrality, add doubly extremely dissolving of 1% hydrochloric acid 50-60 ℃ stirring in water bath of raw material 10-20, add the heavy 0.01-0.001 of raw material cellulose hydrolyzation doubly, through time sampling, detect the molecular weight of shitosan with the Ubbelohde viscometer method, when molecular weight is lower than 50000 hydrolyzate through coarse filtration, 0.45 micron filter membrane micro-filtration, remove impurity, with molecular cut off is the hollow cellulose membrane filtration of 50Kd, removes the incomplete shitosan of degraded, and filtrate is concentrated, after the concentrate drying, be finished product.
β-1,3 glucan (molecular weight is less than 50000):
Sea-tangle processing sewage adds alkali to 1mol Na 2CO 3, to remove supernatant and sediment, get filtrate and add hydrochloric acid accent pH value to the faintly acid electrodialysis desalination through air supporting, through time sampling, with Ubbelohde viscometer method detection molecules amount, hydrolyzate is through coarse filtration when molecular weight is lower than 50000,0.45 the filter membrane micro-filtration of micron, removing impurity, is the hollow cellulose membrane filtration of 50Kd with molecular cut off, removes degraded incomplete β-1,3 glucans, filtrate is concentrated, after the concentrate drying, be finished product.
Sulfonation β-1,3 glucan:
Get above-mentioned molecular weight less than the fully dry finished product of 50000 β-1,3 glucan, it is indoor to change sulfonating reaction over to, under the magnetic agitation situation, feed dry sulfur trioxide, according to the amount control reaction time of reactant, the dry nitrogen of feeding is at last removed unnecessary sulfur trioxide and is got product.
Sulfated chitosan 15kg;
Sulfonation β-1,3 Dextran 15 kg;
Shitosan (molecular weight is less than 50000) 30kg;
β-1,3 glucan (molecular weight is less than 50000) 30kg;
Superphosphate 10kg;
Get said components mixing, the use agent of plant growth regulating antibiotic agent (HTKT) blade face.
Embodiment 2: substantially the same manner as Example 1, difference is that it consists of:
Sulfated chitosan 5kg;
Sulfonation β-1,3 glucan 5kg;
Shitosan (molecular weight is less than 50000) 50kg;
β-1,3 glucan (molecular weight is less than 50000) 50kg;
Superphosphate 15kg;
Wherein molecular weight is less than 50000 β-1, the preparation of 3 glucans is: get and send out full bacterium, flat mushroom bacterium bag before the fruiting behind the homogenate, is handled 2h in ultrasonic, most of solid matter is removed in centrifugation, suction filtration is got filtrate, and with 0.65 μ m membrane microfiltration, filtrate adds 37 ℃ of protease (complex enzyme) enzymolysis, 4-6 hour, through time sampling, with Ubbelohde viscometer detection molecules amount, the hydrolyzate molecular cut off is the hollow cellulose membrane filtration of 50Kd when molecular weight is lower than 50000, remove degraded incomplete β-1,3 glucans carry out concentrating under reduced pressure to filtrate, and concentrate under agitation adds ethanol makes concentration reach 80%, after leaving standstill 24h, filter, collecting precipitation is used washing with alcohol 3 times, after the low temperature drying, be finished product.
Embodiment 3: the preparation of plant growth regulating antibiotic agent (HTKT) seed soaking agent
Substantially the same manner as Example 1, difference is that it consists of:
Sulfated chitosan 25kg;
Sulfonation β-1,3 glucan 25kg;
Shitosan (molecular weight is less than 50000) 25kg;
Crosslinked β-1,3 glucan 25kg;
Superphosphate 5kg;
The preparation method of wherein crosslinked β-1,3 glucan is: add 25 parts of β-1,3 glucans in reactor, 5% sodium hydroxide that adds 40 parts of volume ratios more fully stirs, and keeping temperature is 45 ℃, drip 0.4% epoxychloropropane of 12 parts of volume ratios, keep stirring 3 hours, after reaction finishes, regulate pH value to 6.5 with hydrochloric acid, leave standstill, filter, washing, suction filtration, 50 ℃ of dryings, make crosslinked β-1,3 glucan.
Embodiment 4: substantially the same manner as Example 3, difference is that its component is:
Sulfated chitosan 10kg;
Sulfonation β-1,3 glucan 10kg;
Shitosan (molecular weight is less than 50000) 40kg;
Crosslinked β-1,3 glucan 50kg;
Superphosphate 8kg.
The invention is not restricted to these disclosed embodiments, the present invention will cover the scope described in the patent book, and the various modification and the equivalence of claim scope.

Claims (3)

1. shitosan complex preparation, form by following components in part by weight:
Sulfated chitosan 5-25 part;
Sulfonation β-1,3 glucan 5-25 part;
Molecular weight is less than shitosan 25-50 part of 50000;
Molecular weight is less than β-1,3 glucan or crosslinked β-1,3 glucan 25-50 part of 50000;
Superphosphate 5-15 part.
2. as the said shitosan complex preparation of claim 1, it is characterized in that, form by following components in part by weight:
15 parts of sulfated chitosans;
Sulfonation β-1,3 Dextran 15 part;
Molecular weight is less than 30 parts of 50000 shitosans;
Molecular weight is less than 30 parts of 50000 β-1,3 glucans;
10 parts of superphosphate.
3. as claim 1 or 2 said shitosan complex preparations, it is characterized in that wherein molecular weight is less than 50000 β-1,3 glucans are made by following method: get and send out full bacterium, flat mushroom bacterium bag before the fruiting behind the homogenate, is handled 2h in ultrasonic, most of solid matter is removed in centrifugation, suction filtration is got filtrate, and with 0.65 μ m membrane microfiltration, filtrate adds 37 ℃ of protease hydrolyzeds, 4-6 hour, through time sampling, with Ubbelohde viscometer detection molecules amount, the hydrolyzate molecular cut off is the hollow cellulose membrane filtration of 50Kd when molecular weight is lower than 50000, remove degraded incomplete β-1,3 glucans carry out concentrating under reduced pressure to filtrate, and concentrate under agitation adds ethanol makes concentration reach 80%, after leaving standstill 24h, filter, collecting precipitation is used washing with alcohol 3 times, after the low temperature drying, be finished product.
CNB2007100248810A 2007-07-05 2007-07-05 Plant growth regulating antibiotic agent Expired - Fee Related CN100566573C (en)

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CN101569310B (en) * 2009-06-15 2012-12-12 四川师范大学 Formulation and application of green fruit/vegetable plant regulator
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