CN105028496A - Preparation method of efficient and environment-friendly bioherbicide - Google Patents
Preparation method of efficient and environment-friendly bioherbicide Download PDFInfo
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Abstract
The invention discloses a preparation method of an efficient and environment-friendly bioherbicide. The preparation method comprises the following steps: smashing dried kudzu to obtain kudzu powder, uniformly mixing kudzu with water to obtain a mixed material; adjusting the pH value of the mixed material, adding a complex enzyme preparation, uniformly stirring, and after carrying out standing, concentrating to obtain a concentrated mixed material; continuously adding ethanol water, after carrying out ultrasonic treatment, filtering, washing, and concentrating to obtain a kudzu solution; pouring the kudzu solution into a resin separation column, after carrying out standing, sequentially adding distilled water and two kinds of ethanol water with different concentration, so as to obtain a liquid material A, a liquid material B and a liquid material C; after uniformly mixing the three liquid materials, concentrating, and drying to obtain a kudzu active material; after uniformly mixing the kudzu active material with colza oil, carrying out ultrasonic treatment to obtain a kudzu active material solution; after adding the kudzu active material solution into a wall material solution for homogenization, carrying out spray drying, and cooling to obtain the efficient and environment-friendly bioherbicide.
Description
Technical field
The present invention relates to weed killer herbicide preparing technical field, particularly relate to a kind of preparation method of high-efficiency environment friendly biological weed killer.
Background technology
The excessive multiplication of weeds in farmland very easily causes crop failure, thus brings loss economically to peasant household, and therefore, peasant takes the mode spraying chemical herbicide to kill weeds mostly.But Long-Time Service weed killer herbicide has also caused problems, as the residual harm to the mankind in crop of resistance weed breeding, soil pollution, water pollutions and weed killer herbicide.Along with the raising of people's environmental consciousness, the biological weed killer seeking a kind 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 and reach tens of rice rice even up to a hundred, and its leaf alternate, length can reach 40-50cm.Kudzu has edible and medical value concurrently, and the root of kudzu due to containing the abundant nutritive element such as amino acid, isoflavones, Puerarin, and has the effects such as hypotensive, reducing blood lipid, the toxin expelling that relieves inflammation or internal heat and dark liking by common people.But, kudzu breeding very fast, in forest zone often due to overpreading thus parcel, cover trees cause trees cannot normal growth even dead.Containing a large amount of active material based on alkali in kudzu, these active materials can have strong inhibitory action to the sprouting of careless class seed.
Summary of the invention
Based on the technical problem that background technology exists, the present invention proposes a kind of preparation method of high-efficiency environment friendly biological weed killer, herbicidal performance of the present invention be excellent and the duration is long, environmentally safe.
The preparation method of a kind of high-efficiency environment friendly biological weed killer that the present invention proposes, comprises the following steps:
S1, kudzu after drying is crushed to 5-10 order obtains kudzu powder, by weight 100-120 part kudzu, 180-200 part water are mixed and obtains mixed material, regulate mixed material pH value to 4.8-6.2, then in the mixed material after adjust ph, complex enzyme formulation is added, stir, concentrate after leaving standstill 1-2h and obtain enriched mixture material; In concentrated liquid material, add 200-250 part mass fraction is 90-95wt% ethanol water, after ultrasonic process, filters, washing, concentrates and obtain kudzu solution;
S2, by volume part pour 80-85 part kudzu solution into resin separating column, after leaving standstill 4-6h, add 120-150 part distilled water, after a wash-out, obtain liquid material A in resin separating column; After a wash-out, add 100-200 part volume fraction in resin separating column is the ethanol water of 30-40vol%, after secondary wash-out, obtains liquid material B; After secondary wash-out, add 100-200 part volume fraction in resin separating column is the ethanol water of 60-70vol%, after three wash-outs, obtains liquid material C; After liquid material A, liquid material B, liquid material C being mixed, concentrated, drying obtains kudzu active material;
S3, by weight 60-65 part kudzu active material, 100-110 part rapeseed oil are carried out ultrasonic process after mixing and obtain kudzu active material solution, the frequency of ultrasonic process is 45-50kHz, the power of ultrasonic process is 450-500W, and the time of ultrasonic process is 3-5min; Be that the ethanol water of 10-13wt% mixes by 55-58 part wall material, 2-3 part citric acid glyceride, 1.8-2.2 part tartaric acid, 0.9-1.3 part OPE, 92-95 part mass fraction, filter after stirring and obtain wall material solution; Added by kudzu active material solution in wall material solution after homogeneous, spraying dry, cooling obtains high-efficiency environment friendly biological weed killer.
Preferably, in S1, in complex enzyme formulation, the weight ratio of circumscribed 1,4 beta-glucanase, beta-glucosidase and zytase is 5-8:1-3:2-4.
Preferably, in S1, the frequency of ultrasonic process is 72-75kHz, and the power of ultrasonic process is 700-800W, and the time of ultrasonic process is 6-9min.
Preferably, in S2, resin separating column is made up through Adsorption and desorption of ab-8 resin.
Preferably, in S3, the temperature of homogeneous is 57-60 DEG C, and homogenizing time is 15-18min, and the rotating speed of homogeneous is 8000-11000rpm.
Preferably, in S3, wall material is mixed by weight 3-5:2-4:1-1.5 by gelatin, gum Arabic, sodium alginate.
Preferably, in S2, dry temperature is 75-85 DEG C.
Preferably, in S3, spraying dry EAT is 80-100 DEG C, and leaving air temp is 35-45 DEG C.
In the invention process process, kudzu crushed after being dried to specific order number effectively can be included material by release cells; And the complex enzyme formulation of circumscribed 1,4 beta-glucanase, beta-glucosidase and zytase composition can destroy kudzu cell wall effectively, thus be conducive to the release of cell inclusion material; Through ultrasonic process after enriched mixture material and high concentration ethanol aqueous solution, accelerate the stripping of kudzu cell rupture and cell inclusion material; And be dissolved in kudzu cell inclusion material in the ethanol water ethanol water wash-out through distilled water and two kinds of certain concentration, alkaloids in kudzu solution, polysaccharose, polypeptide class, steroid etc. can be made to have the active material suppressing grass-seed to grow fully separate, thus greatly improve herbicidal performance of the present invention; And kudzu active material is formed single particulate through ultrasonic process and is evenly dispersed in rapeseed oil by S3, kudzu active material is avoided to be interconnected thus cannot microencapsulation; The wall material that gelatin and shitosan are formed with certain proportion, has the features such as filming performance is good, embedding rate is high, viscosity is low, can slow releasing wraps up in soil kudzu active material, thus continues, effectively kills weeds; Citric acid glyceride, as plasticizer and surfactant, with tartaric acid with the use of the plasticity improving micro-capsule of the present invention, can improve embedding rate of the present invention; And OPE is as the interpolation of dispersant, significantly can improve microencapsulation effect of the present invention, reduce bonding, improve embedding rate; Drop is fully dry to select specific air intake, leaving air temp to ensure, prevents micro-capsule from getting damp again, and greatly improves embedding rate of the present invention and yield rate.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the preparation method of a kind of high-efficiency environment friendly biological weed killer that the present invention proposes.
Embodiment
As shown in Figure 1, Fig. 1 is the schematic flow sheet of the preparation method of a kind of high-efficiency environment friendly biological weed killer that the present invention proposes.
With reference to Fig. 1, the preparation method of a kind of high-efficiency environment friendly biological weed killer that the present invention proposes, comprises the following steps:
S1, kudzu after drying is crushed to 5-10 order obtains kudzu powder, by weight 100-120 part kudzu, 180-200 part water are mixed and obtains mixed material, regulate mixed material pH value to 4.8-6.2, then in the mixed material after adjust ph, complex enzyme formulation is added, stir, concentrate after leaving standstill 1-2h and obtain enriched mixture material; In concentrated liquid material, add 200-250 part mass fraction is 90-95wt% ethanol water, after ultrasonic process, filters, washing, concentrates and obtain kudzu solution;
S2, by volume part pour 80-85 part kudzu solution into resin separating column, after leaving standstill 4-6h, add 120-150 part distilled water, after a wash-out, obtain liquid material A in resin separating column; After a wash-out, add 100-200 part volume fraction in resin separating column is the ethanol water of 30-40vol%, after secondary wash-out, obtains liquid material B; After secondary wash-out, add 100-200 part volume fraction in resin separating column is the ethanol water of 60-70vol%, after three wash-outs, obtains liquid material C; After liquid material A, liquid material B, liquid material C being mixed, concentrated, drying obtains kudzu active material;
S3, by weight 60-65 part kudzu active material, 100-110 part rapeseed oil are carried out ultrasonic process after mixing and obtain kudzu active material solution, the frequency of ultrasonic process is 45-50kHz, the power of ultrasonic process is 450-500W, and the time of ultrasonic process is 3-5min; Be that the ethanol water of 10-13wt% mixes by 55-58 part wall material, 2-3 part citric acid glyceride, 1.8-2.2 part tartaric acid, 0.9-1.3 part OPE, 92-95 part mass fraction, filter after stirring and obtain wall material solution; Added by kudzu active material solution in wall material solution after homogeneous, spraying dry, cooling obtains high-efficiency environment friendly biological weed killer.
Below, by specific embodiment, technical scheme of the present invention is described in detail.
Embodiment 1
The preparation method of a kind of high-efficiency environment friendly biological weed killer that the present invention proposes, comprises the following steps:
S1, kudzu after drying is crushed to 10 orders obtains kudzu powder, by weight 100 portions of kudzu, 200 parts of water are mixed and obtain mixed material, regulate mixed material pH value to 4.8, then in the mixed material after adjust ph, complex enzyme formulation is added, stir, concentrate after leaving standstill 2h and obtain enriched mixture material; In concentrated liquid material, add 200 parts of mass fractions is 95wt% ethanol water, after ultrasonic process, filters, washing, concentrates and obtain kudzu solution; Wherein, in complex enzyme formulation, the weight ratio of circumscribed 1,4 beta-glucanase, beta-glucosidase and zytase is 5:3:4;
S2, by volume part pour 80 parts of kudzu solution into resin separating column, after leaving standstill 6h, add 120 parts of distilled water, after a wash-out, obtain liquid material A in resin separating column; After a wash-out, add 200 parts of volume fractions in resin separating column is the ethanol water of 30vol%, after secondary wash-out, obtains liquid material B; After secondary wash-out, add 200 parts of volume fractions in resin separating column is the ethanol water of 60vol%, after three wash-outs, obtains liquid material C; After liquid material A, liquid material B, liquid material C being mixed, concentrated, drying obtains kudzu active material; Wherein, resin separating column is made up through Adsorption and desorption of ab-8 resin; Dry temperature is 85 DEG C;
S3, by weight 60 parts of kudzu active materials, 110 portions of rapeseed oils are carried out ultrasonic process after mixing and obtain kudzu active material solution, the frequency of ultrasonic process is 45kHz, and the power of ultrasonic process is 500W, and the time of ultrasonic process is 3min; Be that the ethanol water of 10wt% mixes by 58 parts of wall materials, 2 parts of citric acid glycerides, 2.2 parts of tartaric acid, 0.9 part of OPE, 95 parts of mass fractions, filter after stirring and obtain wall material solution; Added by kudzu active material solution in wall material solution after homogeneous, spraying dry, cooling obtains high-efficiency environment friendly biological weed killer; Wherein, the temperature of homogeneous is 60 DEG C, and homogenizing time is 15min, and the rotating speed of homogeneous is 11000rpm; Wall material is mixed by weight 3:4:1 by gelatin, gum Arabic, sodium alginate; Spraying dry EAT is 100 DEG C, and leaving air temp is 35 DEG C.
Embodiment 2
The preparation method of a kind of high-efficiency environment friendly biological weed killer that the present invention proposes, comprises the following steps:
S1, kudzu after drying is crushed to 5 orders obtains kudzu powder, by weight 120 portions of kudzu, 180 parts of water are mixed and obtain mixed material, regulate mixed material pH value to 6.2, then in the mixed material after adjust ph, complex enzyme formulation is added, stir, concentrate after leaving standstill 1h and obtain enriched mixture material; In concentrated liquid material, add 250 parts of mass fractions is 90wt% ethanol water, after ultrasonic process, filters, washing, concentrates and obtain kudzu solution; Wherein, in complex enzyme formulation, the weight ratio of circumscribed 1,4 beta-glucanase, beta-glucosidase and zytase is 8:1:2;
S2, by volume part pour 85 parts of kudzu solution into resin separating column, after leaving standstill 4h, add 150 parts of distilled water, after a wash-out, obtain liquid material A in resin separating column; After a wash-out, add 100 parts of volume fractions in resin separating column is the ethanol water of 40vol%, after secondary wash-out, obtains liquid material B; After secondary wash-out, add 100 parts of volume fractions in resin separating column is the ethanol water of 70vol%, after three wash-outs, obtains liquid material C; After liquid material A, liquid material B, liquid material C being mixed, concentrated, drying obtains kudzu active material; Wherein, resin separating column is made up through Adsorption and desorption of ab-8 resin; Dry temperature is 75 DEG C;
S3, by weight 65 parts of kudzu active materials, 100 portions of rapeseed oils are carried out ultrasonic process after mixing and obtain kudzu active material solution, the frequency of ultrasonic process is 50kHz, and the power of ultrasonic process is 450W, and the time of ultrasonic process is 5min; Be that the ethanol water of 13wt% mixes by 55 parts of wall materials, 3 parts of citric acid glycerides, 1.8 parts of tartaric acid, 1.3 parts of OPEs, 92 parts of mass fractions, filter after stirring and obtain wall material solution; Added by kudzu active material solution in wall material solution after homogeneous, spraying dry, cooling obtains high-efficiency environment friendly biological weed killer; Wherein, the temperature of homogeneous is 57 DEG C, and homogenizing time is 18min, and the rotating speed of homogeneous is 8000rpm; Wall material is mixed by weight 5:2:1.5 by gelatin, gum Arabic, sodium alginate; Spraying dry EAT is 80 DEG C, and leaving air temp is 45 DEG C.
Embodiment 3
The preparation method of a kind of high-efficiency environment friendly biological weed killer that the present invention proposes, comprises the following steps:
S1, kudzu after drying is crushed to 8 orders obtains kudzu powder, by weight 105 portions of kudzu, 195 parts of water are mixed and obtain mixed material, regulate mixed material pH value to 5.4, then in the mixed material after adjust ph, complex enzyme formulation is added, stir, concentrate after leaving standstill 1.5h and obtain enriched mixture material; In concentrated liquid material, add 220 parts of mass fractions is 94wt% ethanol water, after ultrasonic process, filters, washing, concentrates and obtain 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 volume part pour 83 parts of kudzu solution into resin separating column, after leaving standstill 4.5h, add 140 parts of distilled water, after a wash-out, obtain liquid material A in resin separating column; After a wash-out, add 140 parts of volume fractions in resin separating column is the ethanol water of 38vol%, after secondary wash-out, obtains liquid material B; After secondary wash-out, add 140 parts of volume fractions in resin separating column is the ethanol water of 66vol%, after three wash-outs, obtains liquid material C; After liquid material A, liquid material B, liquid material C being mixed, concentrated, drying obtains kudzu active material; Wherein, resin separating column is made up through Adsorption and desorption of ab-8 resin; Dry temperature is 77 DEG C;
S3, by weight 64 parts of kudzu active materials, 103 portions of rapeseed oils are carried out ultrasonic process after mixing and obtain kudzu active material solution, the frequency of ultrasonic process is 48kHz, and the power of ultrasonic process is 460W, and the time of ultrasonic process is 4min; Be that the ethanol water of 12wt% mixes by 56 parts of wall materials, 2.5 parts of citric acid glycerides, 1.9 parts of tartaric acid, 1.2 parts of OPEs, 93 parts of mass fractions, filter after stirring and obtain wall material solution; Added by kudzu active material solution in wall material solution after homogeneous, spraying dry, cooling obtains high-efficiency environment friendly biological weed killer; Wherein, the temperature of homogeneous is 58 DEG C, and homogenizing time is 17min, and the rotating speed of homogeneous is 9000rpm; Wall material is mixed by weight 4:2.5:1.3 by gelatin, gum Arabic, sodium alginate; Spraying dry EAT is 85 DEG C, and leaving air temp is 43 DEG C.
Embodiment 4
The preparation method of a kind of high-efficiency environment friendly biological weed killer that the present invention proposes, comprises the following steps:
S1, kudzu after drying is crushed to 6 orders obtains kudzu powder, by weight 110 portions of kudzu, 190 parts of water are mixed and obtain mixed material, regulate mixed material pH value to 6.0, then in the mixed material after adjust ph, complex enzyme formulation is added, stir, concentrate after leaving standstill 1.2h and obtain enriched mixture material; In concentrated liquid material, add 230 parts of mass fractions is 92wt% ethanol water, after ultrasonic process, filters, washing, concentrates and obtain 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 volume part pour 82 parts of kudzu solution into resin separating column, after leaving standstill 5h, add 130 parts of distilled water, after a wash-out, obtain liquid material A in resin separating column; After a wash-out, add 160 parts of volume fractions in resin separating column is the ethanol water of 35vol%, after secondary wash-out, obtains liquid material B; After secondary wash-out, add 160 parts of volume fractions in resin separating column is the ethanol water of 64vol%, after three wash-outs, obtains liquid material C; After liquid material A, liquid material B, liquid material C being mixed, concentrated, drying obtains kudzu active material; Wherein, resin separating column is made up through Adsorption and desorption of ab-8 resin; Dry temperature is 82 DEG C;
S3, by weight 61 parts of kudzu active materials, 107 portions of rapeseed oils are carried out ultrasonic process after mixing and obtain kudzu active material solution, the frequency of ultrasonic process is 46kHz, and the power of ultrasonic process is 480W, and the time of ultrasonic process is 3.5min; Be that the ethanol water of 11wt% mixes by 57 parts of wall materials, 2.2 parts of citric acid glycerides, 2.1 parts of tartaric acid, 1 part of OPE, 94 parts of mass fractions, filter after stirring and obtain wall material solution; Added by kudzu active material solution in wall material solution after homogeneous, spraying dry, cooling obtains high-efficiency environment friendly biological weed killer; Wherein, the temperature of homogeneous is 59 DEG C, and homogenizing time is 16min, and the rotating speed of homogeneous is 10000rpm; Wall material is mixed by weight 3.5:3:1.2 by gelatin, gum Arabic, sodium alginate; Spraying dry EAT is 90 DEG C, and leaving air temp is 38 DEG C.
Embodiment of the present invention 1-4 is made a service test, adopts commercially available biological weed killer as a control group, select corn, soybean field as experimental field, the identical amount of spraying, spray time and field pipe measure under, its result is as shown in the table:
Field weeds amount refers to the ratio of the weeds strain number using the weeds strain number of weed killer herbicide field and do not use weed killer herbicide plot, and as seen from the above table, the present invention has efficient, lasting feature compared to control group.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (8)
1. a preparation method for high-efficiency environment friendly biological weed killer, is characterized in that, comprises the following steps:
S1, kudzu after drying is crushed to 5-10 order obtains kudzu powder, by weight 100-120 part kudzu, 180-200 part water are mixed and obtains mixed material, regulate mixed material pH value to 4.8-6.2, then in the mixed material after adjust ph, complex enzyme formulation is added, stir, concentrate after leaving standstill 1-2h and obtain enriched mixture material; In concentrated liquid material, add 200-250 part mass fraction is 90-95wt% ethanol water, after ultrasonic process, filters, washing, concentrates and obtain kudzu solution;
S2, by volume part pour 80-85 part kudzu solution into resin separating column, after leaving standstill 4-6h, add 120-150 part distilled water, after a wash-out, obtain liquid material A in resin separating column; After a wash-out, add 100-200 part volume fraction in resin separating column is the ethanol water of 30-40vol%, after secondary wash-out, obtains liquid material B; After secondary wash-out, add 100-200 part volume fraction in resin separating column is the ethanol water of 60-70vol%, after three wash-outs, obtains liquid material C; After liquid material A, liquid material B, liquid material C being mixed, concentrated, drying obtains kudzu active material;
S3, by weight 60-65 part kudzu active material, 100-110 part rapeseed oil are carried out ultrasonic process after mixing and obtain kudzu active material solution, the frequency of ultrasonic process is 45-50kHz, the power of ultrasonic process is 450-500W, and the time of ultrasonic process is 3-5min; Be that the ethanol water of 10-13wt% mixes by 55-58 part wall material, 2-3 part citric acid glyceride, 1.8-2.2 part tartaric acid, 0.9-1.3 part OPE, 92-95 part mass fraction, filter after stirring and obtain wall material solution; Added by kudzu active material solution in wall material solution after homogeneous, spraying dry, cooling obtains high-efficiency environment friendly biological weed killer.
2. the preparation method of high-efficiency environment friendly biological weed killer according to claim 1, it is characterized in that, in S1, in complex enzyme formulation, 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 2, it is characterized in that, in S1, the frequency of ultrasonic process is 72-75kHz, and the power of ultrasonic process is 700-800W, and the time of ultrasonic process is 6-9min.
4. the preparation method of high-efficiency environment friendly biological weed killer according to any one of claim 1-3, it is characterized in that, in S2, resin separating column is made up through Adsorption and desorption of ab-8 resin.
5. the preparation method of high-efficiency environment friendly biological weed killer according to any one of claim 1-4, it is characterized in that, in S3, the temperature of homogeneous is 57-60 DEG C, and homogenizing time is 15-18min, and the rotating speed of homogeneous is 8000-11000rpm.
6. the preparation method of high-efficiency environment friendly biological weed killer according to any one of claim 1-5, is characterized in that, in S3, wall material is mixed by weight 3-5:2-4:1-1.5 by gelatin, gum Arabic, sodium alginate.
7. the preparation method of high-efficiency environment friendly biological weed killer according to any one of claim 1-6, is characterized in that, in S2, dry temperature is 75-85 DEG C.
8. the preparation method of high-efficiency environment friendly biological weed killer according to any one of claim 1-7, it is characterized in that, in S3, spraying dry EAT is 80-100 DEG C, and leaving air temp is 35-45 DEG C.
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