CN105028496B - A kind of preparation method of high-efficiency environment friendly biological weed killer - Google Patents
A kind of preparation method of high-efficiency environment friendly biological weed killer Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of high-efficiency environment friendly biological weed killer, comprise the following steps：Kudzu after drying is crushed to obtain kudzu powder, kudzu, water are uniformly mixed to obtain mixed material, mixed material pH value is adjusted, then adds complex enzyme formulation, stir evenly, concentration mixed material is concentrated to give after standing；Continue to add ethanol water, after supersound process, filter, washing, is concentrated to give kudzu solution；Kudzu solution is poured into resin separating column, after standing, the ethanol water for sequentially adding distilled water and two kinds of various concentrations obtains liquid material A, liquid material B, liquid material C；By above-mentioned three kinds of liquid materials after mixing, concentrate, be dried to obtain kudzu active material；Kudzu active material, rapeseed oil are ultrasonically treated after mixing to obtain kudzu active material solution；Kudzu active material solution is added in wall material solution after homogeneous, spray drying, cooling obtains high-efficiency environment friendly biological weed killer.
Description
Technical field
The present invention relates to herbicide preparing technical field, more particularly to a kind of preparation side of high-efficiency environment friendly biological weed killer
Method.
Background technology
Weeds easily cause crop failure in farmland excessive multiplication, so that economic loss is brought to peasant household, because
This, peasant takes the mode for spraying chemical herbicide to kill weeds mostly.However, long-time service herbicide has also triggered many ask
Topic, as resistance weed breeding, soil pollution, water pollution and herbicide remain the harm to the mankind in crop.With
The raising of people's environmental consciousness, seeking a kind of biological weed killer of high-efficiency environment friendly becomes relevant enterprise research direction.
Kudzu, also known as Pueraria lobota bar, elegant jessamine, Convolvulaceae, silver back of the body Calamus liana, kudzu can grow even up to a hundred up to tens of rice
Rice, its leaf alternate, length is up to 40-50cm.Kudzu has edible and medical value concurrently, and the root of kudzu is due to containing abundant amino
The nutrients such as acid, isoflavones, Puerarin, and with lowering blood pressure and blood fat, relieve inflammation or internal heat toxin expelling and other effects and deep liked by common people
Love.However, kudzu breeding is very fast, in forest zone often due to overpreading so as to wrapping up, cover trees and cause trees can not be just
It is frequently grown even dead.Containing largely the active material based on alkali, these active materials can sprout careless class seed in kudzu
Hair has strong inhibitory action.
The content of the invention
Based on technical problem existing for background technology, the present invention proposes a kind of preparation side of high-efficiency environment friendly biological weed killer
Method, herbicidal performance of the present invention is excellent and the duration is long, environmentally safe.
A kind of preparation method of high-efficiency environment friendly biological weed killer proposed by the present invention, comprises the following steps：
S1, be crushed to 5-10 mesh by kudzu after drying and obtain kudzu powder, by weight by 100-120 parts of kudzu, 180-
200 parts of water are uniformly mixed to obtain mixed material, mixed material pH value are adjusted to 4.8-6.2, then to the mixing after adjusting pH value
Complex enzyme formulation is added in material, is stirred evenly, concentration mixed material is concentrated to give after standing 1-2h；Into concentrated liquid material
200-250 part mass fractions of addition be 90-95wt% ethanol waters, and after supersound process, filtering, washs, be concentrated to give kudzu
Solution；
S2, by parts by volume pour into resin separating column by 80-85 parts of kudzu solution, after standing 4-6h, into resin separating column
120-150 parts of distilled water are added, after once eluting, obtain liquid material A；100- is added into resin separating column after once eluting
The ethanol water that 200 parts of volume fractions are 30-40vol%, after secondary elution, obtains liquid material B；Set after to secondary elution
The ethanol water that 100-200 parts of volume fractions are 60-70vol% is added in fat splitter, after eluting three times, obtains liquids
Expect C；By liquid material A, liquid material B, liquid material C after mixing, concentrate, be dried to obtain kudzu active material；
S3, carry out ultrasonic place after mixing by 60-65 parts of kudzu active materials, 100-110 portions of rapeseed oils by weight
Reason obtains kudzu active material solution, and the frequency of supersound process is 45-50kHz, and the power of supersound process is 450-500W, ultrasound
The time of processing is 3-5min；By 55-58 parts of wall materials, 2-3 parts of glyceride citrates, 1.8-2.2 parts of tartaric acid, 0.9-1.3 parts
Oxidized polyethylene wax, 92-95 part mass fraction are that the ethanol water of 10-13wt% is uniformly mixed, and wall is obtained by filtration after stirring
Material solution；Kudzu active material solution is added in wall material solution after homogeneous, spray drying, cooling obtains high-efficiency environment friendly biology and removes
Careless agent.
Preferably, in S1, in complex enzyme formulation, the weight of circumscribed 1,4 beta-glucanase, beta-glucosidase and zytase
Than for 5-8：1-3：2-4.
Preferably, in S1, the frequency of supersound process is 72-75kHz, and the power of supersound process is 700-800W, at ultrasound
The time of reason is 6-9min.
Preferably, resin separating column is made of ab-8 resins are through Adsorption and desorption in S2.
Preferably, in S3, the temperature of homogeneous is 57-60 DEG C, homogenizing time 15-18min, and the rotating speed of homogeneous is 8000-
11000rpm。
Preferably, in S3, wall material is by weight 3-5 by gelatin, Arabic gum, sodium alginate：2-4:1-1.5 mixing systems
Into.
Preferably, in S2, dry temperature is 75-85 DEG C.
Preferably, in S3, spray drying EAT is 80-100 DEG C, and leaving air temp is 35-45 DEG C.
In implementation process of the present invention, kudzu crushed after being dried to specific mesh number can effectively be discharged into cell inclusion material；
And the complex enzyme formulation of circumscribed 1,4 beta-glucanase, beta-glucosidase and zytase composition can effectively destroy kudzu cell
Wall, so as to be conducive to the release of cell inclusion material；Concentration mixed material mixed with high concentration ethanol aqueous solution after through at ultrasonic
Reason, accelerates the dissolution of kudzu cell rupture and cell inclusion material；And it is dissolved in the kudzu cell inclusion in ethanol water
Ethanol water of the material through distilled water and two kinds of certain concentrations elutes, and can make alkaloids, polysaccharide, polypeptide in kudzu solution
There is the active material for suppressing grass-seed development to be sufficiently separated out for class, steroid etc., so as to be greatly enhanced the present invention's
Herbicidal performance；And S3 by the single particulate of the sonicated formation of kudzu active material and is evenly dispersed in rapeseed oil, avoid
Kudzu active material is connected with each other so that can not microencapsulation；The wall material that gelatin and chitosan are formed with certain proportion, has film forming
The features such as performance is good, embedding rate is high, viscosity is low, can slowly discharge wrapped up kudzu active material in the soil, so that continue,
Effectively kill weeds；Glyceride citrate, can be with tartaric acid with the use of this hair of raising as plasticizer and surfactant
The plasticity of bright micro-capsule, improves the embedding rate of the present invention；And addition of the oxidized polyethylene wax as dispersant, can significantly it carry
High microencapsulation effect of the present invention, reduces and bonds, improves embedding rate；Specific inlet air, leaving air temp is selected to ensure that drop fills
Divide drying, prevent micro-capsule from getting damp again, greatly improve the embedding rate and yield rate of the present invention.
Brief description of the drawings
Fig. 1 is a kind of flow diagram of the preparation method of high-efficiency environment friendly biological weed killer proposed by the present invention.
Embodiment
As shown in Figure 1, the flow that Fig. 1 is a kind of preparation method of high-efficiency environment friendly biological weed killer proposed by the present invention is illustrated
Figure.
With reference to Fig. 1, a kind of preparation method of high-efficiency environment friendly biological weed killer proposed by the present invention, comprises the following steps：
S1, be crushed to 5-10 mesh by kudzu after drying and obtain kudzu powder, by weight by 100-120 parts of kudzu, 180-
200 parts of water are uniformly mixed to obtain mixed material, mixed material pH value are adjusted to 4.8-6.2, then to the mixing after adjusting pH value
Complex enzyme formulation is added in material, is stirred evenly, concentration mixed material is concentrated to give after standing 1-2h；Into concentrated liquid material
200-250 part mass fractions of addition be 90-95wt% ethanol waters, and after supersound process, filtering, washs, be concentrated to give kudzu
Solution；
S2, by parts by volume pour into resin separating column by 80-85 parts of kudzu solution, after standing 4-6h, into resin separating column
120-150 parts of distilled water are added, after once eluting, obtain liquid material A；100- is added into resin separating column after once eluting
The ethanol water that 200 parts of volume fractions are 30-40vol%, after secondary elution, obtains liquid material B；Set after to secondary elution
The ethanol water that 100-200 parts of volume fractions are 60-70vol% is added in fat splitter, after eluting three times, obtains liquids
Expect C；By liquid material A, liquid material B, liquid material C after mixing, concentrate, be dried to obtain kudzu active material；
S3, carry out ultrasonic place after mixing by 60-65 parts of kudzu active materials, 100-110 portions of rapeseed oils by weight
Reason obtains kudzu active material solution, and the frequency of supersound process is 45-50kHz, and the power of supersound process is 450-500W, ultrasound
The time of processing is 3-5min；By 55-58 parts of wall materials, 2-3 parts of glyceride citrates, 1.8-2.2 parts of tartaric acid, 0.9-1.3 parts
Oxidized polyethylene wax, 92-95 part mass fraction are that the ethanol water of 10-13wt% is uniformly mixed, and wall is obtained by filtration after stirring
Material solution；Kudzu active material solution is added in wall material solution after homogeneous, spray drying, cooling obtains high-efficiency environment friendly biology and removes
Careless agent.
In the following, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of high-efficiency environment friendly biological weed killer proposed by the present invention, comprises the following steps：
S1, be crushed to 10 mesh by kudzu after drying and obtain kudzu powder, by weight mixes 100 portions of kudzu, 200 parts of water
Mixed material is uniformly obtained, mixed material pH value is adjusted to 4.8, then adds complex enzyme into the mixed material after adjusting pH value
Preparation, stirs evenly, and concentration mixed material is concentrated to give after standing 2h；200 parts of mass fractions are added into concentrated liquid material
For 95wt% ethanol waters, after supersound process, filter, washing, is concentrated to give kudzu solution；Wherein, in complex enzyme formulation, outside
The weight ratio for cutting 1,4 beta-glucanase, beta-glucosidase and zytase is 5：3：4；
S2, by parts by volume pour into resin separating column by 80 parts of kudzu solution, after standing 6h, is added into resin separating column
120 parts of distilled water, after once eluting, obtain liquid material A；200 parts of volume integrals are added into resin separating column after once eluting
Number is the ethanol water of 30vol%, after secondary elution, obtains liquid material B；Added after to secondary elution in resin separating column
The ethanol water that 200 parts of volume fractions are 60vol%, after eluting three times, obtains liquid material C；By liquid material A, liquid
After mixing, concentration, is dried to obtain kudzu active material by material B, liquid material C；Wherein, resin separating column is by ab-8 trees
Fat is through made of Adsorption and desorption；Dry temperature is 85 DEG C；
S3, be ultrasonically treated to obtain Pueraria lobota after mixing by 60 parts of kudzu active materials, 110 portions of rapeseed oils by weight
Rattan active material solution, the frequency of supersound process is 45kHz, and the power of supersound process is 500W, and the time of supersound process is
3min；It is by 58 parts of wall materials, 2 parts of glyceride citrates, 2.2 parts of tartaric acid, 0.9 part of oxidized polyethylene wax, 95 parts of mass fractions
The ethanol water of 10wt% is uniformly mixed, and wall material solution is obtained by filtration after stirring；Kudzu active material solution is added into wall material
In solution after homogeneous, spray drying, cooling obtains high-efficiency environment friendly biological weed killer；Wherein, the temperature of homogeneous is 60 DEG C, during homogeneous
Between be 15min, the rotating speed of homogeneous is 11000rpm；Wall material is by weight 3 by gelatin, Arabic gum, sodium alginate：4:1 is mixed
Made of conjunction；Spray drying EAT is 100 DEG C, and leaving air temp is 35 DEG C.
Embodiment 2
A kind of preparation method of high-efficiency environment friendly biological weed killer proposed by the present invention, comprises the following steps：
S1, be crushed to 5 mesh by kudzu after drying and obtain kudzu powder, by weight mixes 120 portions of kudzu, 180 parts of water
Mixed material is uniformly obtained, mixed material pH value is adjusted to 6.2, then adds complex enzyme into the mixed material after adjusting pH value
Preparation, stirs evenly, and concentration mixed material is concentrated to give after standing 1h；250 parts of mass fractions are added into concentrated liquid material
For 90wt% ethanol waters, after supersound process, filter, washing, is concentrated to give kudzu solution；Wherein, in complex enzyme formulation, outside
The weight ratio for cutting 1,4 beta-glucanase, beta-glucosidase and zytase is 8：1：2；
S2, by parts by volume pour into resin separating column by 85 parts of kudzu solution, after standing 4h, is added into resin separating column
150 parts of distilled water, after once eluting, obtain liquid material A；100 parts of volume integrals are added into resin separating column after once eluting
Number is the ethanol water of 40vol%, after secondary elution, obtains liquid material B；Added after to secondary elution in resin separating column
The ethanol water that 100 parts of volume fractions are 70vol%, after eluting three times, obtains liquid material C；By liquid material A, liquid
After mixing, concentration, is dried to obtain kudzu active material by material B, liquid material C；Wherein, resin separating column is by ab-8 trees
Fat is through made of Adsorption and desorption；Dry temperature is 75 DEG C；
S3, be ultrasonically treated to obtain Pueraria lobota after mixing by 65 parts of kudzu active materials, 100 portions of rapeseed oils by weight
Rattan active material solution, the frequency of supersound process is 50kHz, and the power of supersound process is 450W, and the time of supersound process is
5min；It is by 55 parts of wall materials, 3 parts of glyceride citrates, 1.8 parts of tartaric acid, 1.3 parts of oxidized polyethylene wax, 92 parts of mass fractions
The ethanol water of 13wt% is uniformly mixed, and wall material solution is obtained by filtration after stirring；Kudzu active material solution is added into wall material
In solution after homogeneous, spray drying, cooling obtains high-efficiency environment friendly biological weed killer；Wherein, the temperature of homogeneous is 57 DEG C, during homogeneous
Between be 18min, the rotating speed of homogeneous is 8000rpm；Wall material is by weight 5 by gelatin, Arabic gum, sodium alginate：2:It is 1.5 mixed
Made of conjunction；Spray drying EAT is 80 DEG C, and leaving air temp is 45 DEG C.
Embodiment 3
A kind of preparation method of high-efficiency environment friendly biological weed killer proposed by the present invention, comprises the following steps：
S1, be crushed to 8 mesh by kudzu after drying and obtain kudzu powder, by weight mixes 105 portions of kudzu, 195 parts of water
Mixed material is uniformly obtained, mixed material pH value is adjusted to 5.4, then adds complex enzyme into the mixed material after adjusting pH value
Preparation, stirs evenly, and concentration mixed material is concentrated to give after standing 1.5h；220 parts of quality point are added into concentrated liquid material
Number is 94wt% ethanol waters, after supersound process, is filtered, washing, is concentrated to give kudzu solution；Wherein, in complex enzyme formulation,
The weight ratio of circumscribed 1,4 beta-glucanase, beta-glucosidase and zytase is 6：2：3；
S2, by parts by volume pour into resin separating column by 83 parts of kudzu solution, after standing 4.5h, is added into resin separating column
140 parts of distilled water, after once eluting, obtain liquid material A；140 parts of volume integrals are added into resin separating column after once eluting
Number is the ethanol water of 38vol%, after secondary elution, obtains liquid material B；Added after to secondary elution in resin separating column
The ethanol water that 140 parts of volume fractions are 66vol%, after eluting three times, obtains liquid material C；By liquid material A, liquid
After mixing, concentration, is dried to obtain kudzu active material by material B, liquid material C；Wherein, resin separating column is by ab-8 trees
Fat is through made of Adsorption and desorption；Dry temperature is 77 DEG C；
S3, be ultrasonically treated to obtain Pueraria lobota after mixing by 64 parts of kudzu active materials, 103 portions of rapeseed oils by weight
Rattan active material solution, the frequency of supersound process is 48kHz, and the power of supersound process is 460W, and the time of supersound process is
4min；By 56 parts of wall materials, 2.5 parts of glyceride citrates, 1.9 parts of tartaric acid, 1.2 parts of oxidized polyethylene wax, 93 parts of mass fractions
It is uniformly mixed for the ethanol water of 12wt%, wall material solution is obtained by filtration after stirring；Kudzu active material solution is added into wall
In material solution after homogeneous, spray drying, cooling obtains high-efficiency environment friendly biological weed killer；Wherein, the temperature of homogeneous is 58 DEG C, homogeneous
Time is 17min, and the rotating speed of homogeneous is 9000rpm；Wall material is by weight 4 by gelatin, Arabic gum, sodium alginate：2.5:
1.3 are mixed；Spray drying EAT is 85 DEG C, and leaving air temp is 43 DEG C.
Embodiment 4
A kind of preparation method of high-efficiency environment friendly biological weed killer proposed by the present invention, comprises the following steps：
S1, be crushed to 6 mesh by kudzu after drying and obtain kudzu powder, by weight mixes 110 portions of kudzu, 190 parts of water
Mixed material is uniformly obtained, mixed material pH value is adjusted to 6.0, then adds complex enzyme into the mixed material after adjusting pH value
Preparation, stirs evenly, and concentration mixed material is concentrated to give after standing 1.2h；230 parts of quality point are added into concentrated liquid material
Number is 92wt% ethanol waters, after supersound process, is filtered, washing, is concentrated to give kudzu solution；Wherein, in complex enzyme formulation,
The weight ratio of circumscribed 1,4 beta-glucanase, beta-glucosidase and zytase is 7：1.4：3.5；
S2, by parts by volume pour into resin separating column by 82 parts of kudzu solution, after standing 5h, is added into resin separating column
130 parts of distilled water, after once eluting, obtain liquid material A；160 parts of volume integrals are added into resin separating column after once eluting
Number is the ethanol water of 35vol%, after secondary elution, obtains liquid material B；Added after to secondary elution in resin separating column
The ethanol water that 160 parts of volume fractions are 64vol%, after eluting three times, obtains liquid material C；By liquid material A, liquid
After mixing, concentration, is dried to obtain kudzu active material by material B, liquid material C；Wherein, resin separating column is by ab-8 trees
Fat is through made of Adsorption and desorption；Dry temperature is 82 DEG C；
S3, be ultrasonically treated to obtain Pueraria lobota after mixing by 61 parts of kudzu active materials, 107 portions of rapeseed oils by weight
Rattan active material solution, the frequency of supersound process is 46kHz, and the power of supersound process is 480W, and the time of supersound process is
3.5min；By 57 parts of wall materials, 2.2 parts of glyceride citrates, 2.1 parts of tartaric acid, 1 part of oxidized polyethylene wax, 94 parts of mass fractions
It is uniformly mixed for the ethanol water of 11wt%, wall material solution is obtained by filtration after stirring；Kudzu active material solution is added into wall
In material solution after homogeneous, spray drying, cooling obtains high-efficiency environment friendly biological weed killer；Wherein, the temperature of homogeneous is 59 DEG C, homogeneous
Time is 16min, and the rotating speed of homogeneous is 10000rpm；Wall material is by weight 3.5 by gelatin, Arabic gum, sodium alginate：3:
1.2 are mixed；Spray drying EAT is 90 DEG C, and leaving air temp is 38 DEG C.
Make a service test to 1-4 of the embodiment of the present invention, using commercially available biological weed killer as a control group, selection corn,
Soybean field is as experimental field, and under the identical amount of spraying, spraying time and field pipe measure, its result is as shown in the table：
Field weeds amount refers to the weeds strain number and the weeds strain number in unused herbicide plot using herbicide field
Ratio, as seen from the above table, it is efficient, lasting that the present invention has the characteristics that compared to control group.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of preparation method of high-efficiency environment friendly biological weed killer, it is characterised in that comprise the following steps：
S1, be crushed to 5-10 mesh by kudzu after drying and obtain kudzu powder, by weight by 100-120 portions of kudzu, 180-200 parts
Water is uniformly mixed to obtain mixed material, mixed material pH value is adjusted to 4.8-6.2, then into the mixed material after adjusting pH value
Complex enzyme formulation is added, is stirred evenly, concentration mixed material is concentrated to give after standing 1-2h；Added into concentrated liquid material
200-250 parts of mass fractions are 90-95wt% ethanol waters, after supersound process, are filtered, washing, is concentrated to give kudzu solution；
S2, by parts by volume pour into resin separating column by 80-85 parts of kudzu solution, after standing 4-6h, is added into resin separating column
120-150 parts of distilled water, after once eluting, obtain liquid material A；100-200 is added into resin separating column after once eluting
The ethanol water that part volume fraction is 30-40vol%, after secondary elution, obtains liquid material B；Resin after to secondary elution
The ethanol water that 100-200 parts of volume fractions are 60-70vol% is added in splitter, after eluting three times, obtains liquid material
C；By liquid material A, liquid material B, liquid material C after mixing, concentrate, be dried to obtain kudzu active material；
S3, carry out being ultrasonically treated after mixing by 60-65 parts of kudzu active materials, 100-110 portions of rapeseed oils by weight
To kudzu active material solution, the frequency of supersound process is 45-50kHz, and the power of supersound process is 450-500W, is ultrasonically treated
Time be 3-5min；By 55-58 parts of wall materials, 2-3 parts of glyceride citrates, 1.8-2.2 parts of tartaric acid, 0.9-1.3 parts of oxidations
Tissuemat E, 92-95 part mass fraction are that the ethanol water of 10-13wt% is uniformly mixed, and it is molten that wall material is obtained by filtration after stirring
Liquid；Kudzu active material solution is added in wall material solution after homogeneous, spray drying, cooling obtains high-efficiency environment friendly biological weed control
Agent；
Wherein, resin separating column is made of ab-8 resins are through Adsorption and desorption in S2.
2. the preparation method of high-efficiency environment friendly biological weed killer according to claim 1, it is characterised in that in S1, complex enzyme system
In agent, the weight ratio of circumscribed 1,4 beta-glucanase, beta-glucosidase and zytase is 5-8：1-3：2-4.
3. the preparation method of high-efficiency environment friendly biological weed killer according to claim 1 or claim 2, it is characterised in that in S1, at ultrasound
The frequency of reason is 72-75kHz, and the power of supersound process is 700-800W, and the time of supersound process is 6-9min.
4. the preparation method of high-efficiency environment friendly biological weed killer according to claim 1 or claim 2, it is characterised in that in S3, homogeneous
Temperature is 57-60 DEG C, homogenizing time 15-18min, and the rotating speed of homogeneous is 8000-11000rpm.
5. the preparation method of high-efficiency environment friendly biological weed killer according to claim 1 or claim 2, it is characterised in that in S3, wall material is
By gelatin, Arabic gum, sodium alginate by weight 3-5：2-4:What 1-1.5 was mixed.
6. the preparation method of high-efficiency environment friendly biological weed killer according to claim 1 or claim 2, it is characterised in that in S2, dry
Temperature is 75-85 DEG C.
7. the preparation method of high-efficiency environment friendly biological weed killer according to claim 1 or claim 2, it is characterised in that in S3, spraying is dry
Dry inlet air temperature is 80-100 DEG C, and leaving air temp is 35-45 DEG C.
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| CN106922664A (en) * | 2017-04-14 | 2017-07-07 | 广西大学 | Compound herbicide for gardens and preparation method thereof |
| CN110367016A (en) * | 2019-07-31 | 2019-10-25 | 六安市兆丰商贸有限责任公司 | A kind of deinsectization herbicidal methods of white peach plantation |
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