CN101836635A - Antiseptic composition waterborne preparation and method for preparing same - Google Patents
Antiseptic composition waterborne preparation and method for preparing same Download PDFInfo
- Publication number
- CN101836635A CN101836635A CN201010004122A CN201010004122A CN101836635A CN 101836635 A CN101836635 A CN 101836635A CN 201010004122 A CN201010004122 A CN 201010004122A CN 201010004122 A CN201010004122 A CN 201010004122A CN 101836635 A CN101836635 A CN 101836635A
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- CN
- China
- Prior art keywords
- tebuconazole
- oxime bacterium
- bacterium ester
- water
- alcohol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000203 mixture Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 230000002421 anti-septic effect Effects 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 17
- PXMNMQRDXWABCY-UHFFFAOYSA-N 1-(4-chlorophenyl)-4,4-dimethyl-3-(1H-1,2,4-triazol-1-ylmethyl)pentan-3-ol Chemical compound C1=NC=NN1CC(O)(C(C)(C)C)CCC1=CC=C(Cl)C=C1 PXMNMQRDXWABCY-UHFFFAOYSA-N 0.000 claims abstract description 123
- 239000005839 Tebuconazole Substances 0.000 claims abstract description 122
- 239000000839 emulsion Substances 0.000 claims abstract description 79
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 36
- 239000000725 suspension Substances 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 19
- 238000009472 formulation Methods 0.000 claims abstract description 14
- ONCZDRURRATYFI-TVJDWZFNSA-N trifloxystrobin Chemical compound CO\N=C(\C(=O)OC)C1=CC=CC=C1CO\N=C(/C)C1=CC=CC(C(F)(F)F)=C1 ONCZDRURRATYFI-TVJDWZFNSA-N 0.000 claims abstract description 14
- 239000005857 Trifloxystrobin Substances 0.000 claims abstract description 13
- 239000004480 active ingredient Substances 0.000 claims abstract description 10
- 239000006184 cosolvent Substances 0.000 claims abstract description 9
- 150000002148 esters Chemical class 0.000 claims description 123
- 241000894006 Bacteria Species 0.000 claims description 120
- 150000002923 oximes Chemical class 0.000 claims description 119
- -1 enanthol Chemical compound 0.000 claims description 34
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 27
- 239000001293 FEMA 3089 Substances 0.000 claims description 21
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 18
- 239000004094 surface-active agent Substances 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- 230000000740 bleeding effect Effects 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 14
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 14
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 230000002528 anti-freeze Effects 0.000 claims description 12
- 239000013530 defoamer Substances 0.000 claims description 12
- 229920005646 polycarboxylate Polymers 0.000 claims description 12
- 150000003839 salts Chemical class 0.000 claims description 12
- 239000004576 sand Substances 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 11
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- 239000002518 antifoaming agent Substances 0.000 claims description 10
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- 229920001296 polysiloxane Polymers 0.000 claims description 10
- KJIOQYGWTQBHNH-UHFFFAOYSA-N undecanol Chemical compound CCCCCCCCCCCO KJIOQYGWTQBHNH-UHFFFAOYSA-N 0.000 claims description 10
- AXTGDCSMTYGJND-UHFFFAOYSA-N 1-dodecylazepan-2-one Chemical compound CCCCCCCCCCCCN1CCCCCC1=O AXTGDCSMTYGJND-UHFFFAOYSA-N 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 9
- 150000001298 alcohols Chemical class 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 claims description 8
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- ZWRUINPWMLAQRD-UHFFFAOYSA-N nonan-1-ol Chemical compound CCCCCCCCCO ZWRUINPWMLAQRD-UHFFFAOYSA-N 0.000 claims description 8
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- 239000002562 thickening agent Substances 0.000 claims description 8
- WRKCIHRWQZQBOL-UHFFFAOYSA-N octyl dihydrogen phosphate Chemical compound CCCCCCCCOP(O)(O)=O WRKCIHRWQZQBOL-UHFFFAOYSA-N 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 229910019142 PO4 Inorganic materials 0.000 claims description 6
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 6
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- OOCMUZJPDXYRFD-UHFFFAOYSA-L calcium;2-dodecylbenzenesulfonate Chemical compound [Ca+2].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O.CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O OOCMUZJPDXYRFD-UHFFFAOYSA-L 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 5
- 239000010452 phosphate Substances 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 229940057402 undecyl alcohol Drugs 0.000 claims description 5
- DMAXMXPDVWTIRV-UHFFFAOYSA-N 2-(2-phenylethyl)phenol Chemical compound OC1=CC=CC=C1CCC1=CC=CC=C1 DMAXMXPDVWTIRV-UHFFFAOYSA-N 0.000 claims description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 claims description 4
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 4
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- UDHMTPILEWBIQI-UHFFFAOYSA-N butyl naphthalene-1-sulfonate;sodium Chemical compound [Na].C1=CC=C2C(S(=O)(=O)OCCCC)=CC=CC2=C1 UDHMTPILEWBIQI-UHFFFAOYSA-N 0.000 claims description 4
- 229920005551 calcium lignosulfonate Polymers 0.000 claims description 4
- 239000007859 condensation product Substances 0.000 claims description 4
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 4
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 4
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 4
- 150000002576 ketones Chemical class 0.000 claims description 4
- 229920005610 lignin Polymers 0.000 claims description 4
- IXQGCWUGDFDQMF-UHFFFAOYSA-N o-Hydroxyethylbenzene Natural products CCC1=CC=CC=C1O IXQGCWUGDFDQMF-UHFFFAOYSA-N 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 150000003014 phosphoric acid esters Chemical class 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 4
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 4
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 4
- 150000003871 sulfonates Chemical class 0.000 claims description 4
- 150000003460 sulfonic acids Chemical class 0.000 claims description 4
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 4
- 229920001285 xanthan gum Polymers 0.000 claims description 4
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 3
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 3
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 claims description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 3
- PSZYNBSKGUBXEH-UHFFFAOYSA-M naphthalene-1-sulfonate Chemical compound C1=CC=C2C(S(=O)(=O)[O-])=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-M 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
- ZFPGARUNNKGOBB-UHFFFAOYSA-N 1-Ethyl-2-pyrrolidinone Chemical compound CCN1CCCC1=O ZFPGARUNNKGOBB-UHFFFAOYSA-N 0.000 claims description 2
- CDMGNVWZXRKJNS-UHFFFAOYSA-N 2-benzylphenol Chemical compound OC1=CC=CC=C1CC1=CC=CC=C1 CDMGNVWZXRKJNS-UHFFFAOYSA-N 0.000 claims description 2
- 125000000094 2-phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 claims description 2
- 108010010803 Gelatin Proteins 0.000 claims description 2
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- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 235000010489 acacia gum Nutrition 0.000 claims description 2
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses an antiseptic composition waterborne preparation and a method for preparing the same, and in particular relates to trifloxystrobin, a tebuconazole microemulsion, an aqueous emulsion and a suspension emulsion and a method for preparing the same. The antiseptic composition waterborne preparation comprises the following raw materials in percentage by weight: 3 to 20 percent of trifloxystrobin, 6 to 40 percent of tebuconazole, 0.5 to 20 percent of solvent, 0 to 8 percent of cosolvent, and the balance of water. By adopting different solvent combinations and processing technology according to the content of active ingredients, the method can realize the conversion among three formulations; and the waterborne preparation overcomes the defects in the conventional formulation, provides more choices for diversification of the formulations of products and meets market requirements.
Description
Technical field
The present invention relates to a kind of antiseptic composition waterborne preparation, be specifically related to oxime bacterium ester and Tebuconazole composite microemulsion, aqueous emulsion, suspension emulsion and manufacture method thereof, belong to the pesticidal preparations processing technique field.
Background technology
Oxime bacterium ester, chemical name: (2Z)-and 2-methoxyimino-2-[2-[[1-[3-(trifluoromethyl) phenyl] ethyleneimino] the oxygen methyl] phenyl] methyl acetate, English common name Trifloxystrobin, molecular formula: C
20H
19F
3N
2O
4, molecular weight: 408.3, CAS number: 141517-21-7, white solid, 72.9 ℃ of fusing points, boiling point: 312 ℃, be soluble in multiple organic solvent.Oxime bacterium ester is the new fluorine-containing methoxy acrylate bactericide of a class that utilizes natural products Strobilurins successfully to develop as lead compound, characteristics such as having efficient, wide spectrum, protection, treat, root out, infiltration, systemic activity, resistance of rainwater washing against, lasting period are long.Oxime bacterium ester all has good activity to nearly all Mycophytes (Ascomycetes, Basidiomycetes, Oomycete and Fungi Imperfecti) disease such as powdery mildew, rust, glume blight, net blotch, downy mildew, rice blast etc.Except that powdery mildew, leaf spot are had the special efficacy, rust, downy mildew, damping off, apple apple scab all there is good activity, to crop safety.Capable of being fast degraded in soil, water because of it, so environmentally safe.The methoxy acrylate series bactericidal agent mainly is incorporated into the Qo site of cytochrome b part in the pathogen cytochrome b c1 compound, because cytochrome b is by the very high chondriogen group coding of mutation rate, so pathogen is easy to develop immunity to drugs because of the sudden change of this gene.
Tebuconazole, chemical name: (RS)-and 1-(4-chlorphenyl)-4,4-dimethyl-3-(1H-1,2,4-triazol-1-yl methyl) penta-3-alcohol, English common name Tebuconazole, molecular formula: C
16H
22ClN
3O, molecular weight: 307.82, CAS number: 107534-96-3, fusing point 102-105 ℃, white solid is dissolved in multiple organic solvent.Tebuconazole belongs to triazole bactericidal agent, and the tool systemic action can be rapidly partially absorbed and mainly shifts to the top by plant is vegetative.The mechanism of action is ergosterol biosynthesis inhibitor, and somatic cells film function is damaged, thereby reaches the purpose of sterilization.Tebuconazole can be prevented and treated Erysiphe, Puccinia, Rhynchosporium spp, nuclear cavity Pseudomonas and the microbial disease of Septoria such as wheat powdery mildew, loose smut of wheat, wheat banded sclerotial blight, wheat snow mold, take-all, the bunt of wheat, barley leaf blotch, loose smut of barley, barley banded sclerotial blight, maize head smut, head smut of sorghum, soybean rust, sclerotinia rot of colza, sigatoka, tea gall, alternaria leaf spot of apple, pear scab and grape grey mould etc.
Oxime bacterium ester, Tebuconazole are the different bactericide of the mechanism of action, and both use with, not only can enlarge fungicidal spectrum, have complementary advantages, and can delay drug-fast generation, prolong the service life of product.
In the patent documentation report, the composite preparation of oxime bacterium ester and Tebuconazole has wetting powder, water dispersible granules, suspending agent, does not see Water-borne modification formulation reports such as microemulsion, aqueous emulsion, suspension emulsion as yet.Microemulsion, aqueous emulsion, suspension emulsion are important Water-borne modification formulations, and the characteristic of self is arranged separately, compare with conventional dosage forms such as wetting powders to have better quality.
The Water-borne modification formulation is the new trend of formulations of pesticide development, and it is main dispersion medium with water, has not only reduced the toxicity of preparation, minimizing is to the pressure of environment, and make preparation production, transportation, safer, the outstanding advantage of use, make the Water-borne modification formulation be subjected to pursuing widely in the whole world.
Summary of the invention
The purpose of this invention is to provide with oxime bacterium ester and Tebuconazole is the waterborne preparation of active ingredient, comprises microemulsion, aqueous emulsion, suspension emulsion.
It is the manufacture method of the waterborne preparation of active ingredient that another object of the present invention provides with oxime bacterium ester and Tebuconazole.
Basic principle according to microemulsion, aqueous emulsion, suspension emulsion formulation, physicochemical property in conjunction with oxime bacterium ester, Tebuconazole, we are through a large amount of screening test research, invented under different auxiliary agent combinations and fabrication process condition, manufacturing is the different waterborne preparation of active ingredient with oxime bacterium ester, Tebuconazole, adapt to the different content scope, simultaneously, satisfy the demand of market product.
The antiseptic composition waterborne preparation that the present invention relates to, it is characterized in that composition active ingredient contains oxime bacterium ester, Tebuconazole, preparation raw material mass percent is oxime bacterium ester 3%-20%, Tebuconazole 6%-40%, solvent 0.5%-20%, cosolvent 0-8%, bleeding agent 1%-5%, thickener 0-3%, antifreeze 0%-5%, defoamer 0-3%, surfactant 6%-20%, water surplus.
The antiseptic composition waterborne preparation that the present invention relates to, it is characterized by formulation is microemulsion, aqueous emulsion, suspension emulsion.
Oxime bacterium ester that the present invention relates to and Tebuconazole composite microemulsion is characterized by oxime bacterium ester 3%-8%, Tebuconazole 6%-16%, solvent 0.5%-15%, cosolvent 0.5%-8%, bleeding agent 1%-5%, surfactant 8%-20%, water surplus.
Oxime bacterium ester that the present invention relates to and Tebuconazole composition aqueous emulsion is characterized by and contain oxime bacterium ester 3%-12%, Tebuconazole 6%-24%, solvent 0.5%-20%, antifreeze 0.5%-5%, bleeding agent 1%-5%, defoamer 0.1%-3%, surfactant 6%-12%, water surplus.
Oxime bacterium ester that the present invention relates to and Tebuconazole composition suspended emulsion, it is characterized by and contain oxime bacterium ester 3%-17%, Tebuconazole 6%-34%, solvent 0.5%-15%, thickener 0.1%-3%, antifreeze 0.5%-5%, bleeding agent 1%-5%, defoamer 0.1%-3%, surfactant 6%-12%, water surplus.
The solvent that the present invention relates to is characterized by in turpentine oil, the gaultherolin at least a.Turpentine oil includes gum turpentine, steam-distilled turpentine.During use, according to the difference of oxime bacterium ester, Tebuconazole content, two kinds of solvents can be singly with or arbitrary proportion be used in combination.
The cosolvent that the present invention relates to is characterized by in alcohols, the ketone at least a, wherein, alcohols includes ethanol, propyl alcohol, isopropyl alcohol, n-butanol, isobutanol, amylalcohol, isoamyl alcohol, hexanol, enanthol, octanol, nonyl alcohol, decyl alcohol, undecyl alcohol, lauryl alcohol, cyclopentanol, cyclohexanol, phenmethylol; Ketone includes acetone, butanone, acetophenone, propiophenone, N-Methyl pyrrolidone, N-ethyl pyrrolidone.
The antifreeze that the present invention relates to, it is characterized by comprise in glycerine, ethylene glycol, propane diols, the sorbierite at least a.
The bleeding agent that the present invention relates to is characterized by and comprises penetrant t, JFC, water-soluble azone.Penetrant t has another name called the succinate sodium sulfonate, and chemical name is the dioctyl maleate sodium sulfonate; Water-soluble azone, chemical name are 1-positive dodecyl aza cyclohepta-2-ketone.
The surfactant that the present invention relates to can be selected from least a among polyethers, ester class, phosphoric acid ester, Sulfonates, Sulfates, lignin sulfonic acid salt, naphthalenesulfonate, the polycarboxylic acid salt.
Described polyethers comprises alkylphenol polyoxyethylene class (as: NP/OP-4,6,7,9,10,12,15,20,30,40), benzylphenol polyethenoxy ether class (as: No. 300, farming breast, No. 900, farming breast, No. 31, peaceful breast, No. 36, peaceful breast, the newborn BP of farming), phenethyl phenol polyethenoxy ethers (as: No. 601, farming breast, No. 602, farming breast, No. 603, farming breast, No. 604, farming breast), phenethyl fluosite polyethenoxy ether class (as: No. 401, farming breast, No. 402, farming breast, No. 403, farming breast, No. 404, farming breast), the alkyl phenol formaldehyde resin polyoxyethylene ether class (as: comprises No. 701, farming breast, No. 702, farming breast), fatty alcohol polyethenoxy ether class (as: AEO-3,5,7,9,10,15,20, paregal O, O-20, A-20, SA-20, JFC), phenethyl phenol polyethenoxy polyoxypropylene ethers (as: No. 1600, farming breast, No. 1601, farming breast, No. 1602, farming breast), triphen ethyl phenol polyoxyethylene poly-oxygen propylene aether class (as: No. 33, farming breast, No. 34, farming breast), sorbitan fatty acid ester polyethenoxy ether class (as: polysorbas20, polysorbate40, polysorbate60, Tween 80, polysorbate85), castor oil polyoxyethylene ether class (as: EL-20,40,60,80,90,125; BY-110,120,125,130,140,155).
Described ester class comprises sorbitan fatty acid ester class (as: span 20, span 40, sorbester p18, sorbester p17, sorbester p37), polyoxyethylene carboxylate class, general molecular formula RCOO-(CH
2CH
2O)
nH, cithrol class (as: diethylene glycol monostearate, diethylene glycol bis-stearate, PEG400 monostearate, the two stearates of PEG400, the two stearates of Macrogol 6000).
Described phosphoric acid ester includes alkyl phenol polyoxyethylene nonylphenol ether phosphate and salt, aliphatic alcohol polyoxyvinethene phosphate and salt thereof, octyl phosphate and salt thereof, octanol polyoxyethylene ether phosphate and salt thereof.
Described Sulfonates includes neopelex, calcium dodecyl benzene sulfonate, magnesium dodecyl benzene sulfonate.
Described Sulfates includes lauryl sodium sulfate, Stepanol MG.
Described lignin sulfonic acid salt includes sodium lignin sulfonate, calcium lignosulfonate.
Described naphthalenesulfonate class includes sodium metnylene bis-naphthalene sulfonate, sodium butylnaphthalenesulfonate, benzyl naphthalene sulfonic formaldehyde condensation compound, nekal formaldehyde condensation products.
Described polycarboxylic acid salt includes polycarboxylate 2700, polycarboxylate T36, polycarboxylate YUS-WG5.
Described thickener, it is characterized by comprise in gelatin, gum Arabic, xanthans, soluble starch, polyvinyl alcohol, the sodium carboxymethylcellulose at least a.
Described defoamer, it is at least a to it is characterized by polyoxyethylene polyoxypropylene glycerine (as: GPE10, GPE20, GPE30, GPE40, GPE50), silicone defoaming agent, alcohols, and wherein alcohols comprises enanthol, octanol, isooctanol, nonyl alcohol, decyl alcohol, undecyl alcohol, lauryl alcohol etc.
The water that the present invention relates to can be for determining total hardness of water less than 342mg/L (with CaCO
3Meter) water is as running water, deionized water etc.
The oxime bacterium ester that the present invention relates to and the process for producing of Tebuconazole composite microemulsion is characterized by:
At ambient temperature, earlier oxime bacterium ester, Tebuconazole, solvent, cosolvent, bleeding agent, surfactant are added in the reactor by the requirement of raw material mass percent, rotating speed with 100-5000 rev/min, stirred 15-45 minute, form oil phase, add entry again, stirred 10-30 minute, make it to become the liquid of homogeneous, promptly get oxime bacterium ester and Tebuconazole composite microemulsion.
The process for producing of oxime bacterium ester that the present invention relates to and Tebuconazole composition aqueous emulsion is characterized by:
At ambient temperature, earlier oxime bacterium ester, Tebuconazole, solvent are added in the reactor by the requirement of raw material mass percent, under 100-5000 rev/min rotating speed, stir, make it to become the liquid of homogeneous, keep mixing speed, add antifreeze, bleeding agent, defoamer, surfactant, water, stirred 20-60 minute, mix, transfer in the high speed shear reactor, under 1000-20000 rev/min rotating speed, high speed shear 20-90 minute, promptly get oxime bacterium ester and Tebuconazole composition aqueous emulsion.
The oxime bacterium ester that the present invention relates to and the process for producing of Tebuconazole composition suspended emulsion is characterized by:
At ambient temperature, earlier oxime bacterium ester, solvent, surfactant, water are added in the high speed shear reactor, with 1000-20000 rev/min by the requirement of raw material mass percent, high speed shear 30-90 minute, make it to become the liquid of homogeneous, prepare the trifloxystrobin water emulsion, stand-by; In another reactor, add Tebuconazole, antifreeze, bleeding agent, defoamer, surfactant, water, with 100-5000 rev/min, stir, after mixing, add in the sand mill, with 100-5000 rev/min, sand milling 30-180 minute, with the particle size of laser particle diameter distribution instrument mensuration suspension, when average grain diameter during less than 5 μ m, add the trifloxystrobin water emulsion, the thickener that prepare, sand milling 20-40 minute, promptly get oxime bacterium ester and Tebuconazole composition suspended emulsion.
Oxime bacterium ester and the Tebuconazole composite microemulsion that the present invention relates to meet following standard:
PH value: 4.0-8.0.
Stability of emulsion: 342ppm hard water (30 ± 2 ℃), dilute 200 times, place 1h, dilution keeps transparent and homogeneous.
Hold bubble: foam should not surpass 10mL behind the 1min.
Bin stability: in (0 ± 2) ℃, stored 14 days, outward appearance is bright or translucent, and is not stratified, do not have precipitation; In (54 ± 2) ℃, to store 14 days, outward appearance is bright, and is not stratified, do not have precipitation; Active ingredient resolution ratio≤5%; Stability of emulsion is still qualified.
Soup average grain diameter: 0.01～0.1 μ m.
Oxime bacterium ester that the present invention relates to and Tebuconazole composition aqueous emulsion meet following standard:
PH value: 4.0-8.0.
Stability of emulsion: 342ppm hard water (30 ± 2 ℃), when diluting 200 times, placed 1 hour, on do not have oil slick, do not have oil slick and a precipitation down.
Hold bubble: foam should not surpass 10mL behind the 1min.
Pourability: topple over back residue≤3%.
Bin stability: in (0 ± 2) ℃, stored 14 days, not stratified, there is not precipitation; In (54 ± 2) ℃, stored 14 days, not stratified, there is not precipitation; Active ingredient resolution ratio≤5%; Stability of emulsion is still qualified.
Soup average grain diameter: 0.1～40 μ m.
Oxime bacterium ester and the Tebuconazole composition suspended emulsion that the present invention relates to meet following standard:
PH value: 4.0-8.0.
Dispersion stabilization: 342ppm hard water (30 ± 2 ℃), dilute 200 times, observe:
Initial dispersion stabilization: disperse fully, the dilution homogeneous does not have precipitation and oil slick;
Dilution stability behind the 30min: emulsifiable paste≤1mL, precipitation≤1mL, oil slick: do not have;
24h is dispersion stabilization again: disperse fully, the dilution homogeneous does not have precipitation and oil slick;
24.5h after dispersed again: emulsifiable paste≤1.5mL, precipitation≤1.5mL, oil slick≤0.5mL.
Hold bubble: foam should not surpass 10mL behind the 1min.
Pourability: topple over back residue≤3%.
Wet screening test: have 98% sample at least by on the 45 μ m testing sieves.
Bin stability: in (0 ± 2) ℃, stored 14 days, not stratified, there is not precipitation; In (54 ± 2) ℃, stored 14 days, not stratified, there is not precipitation; Active ingredient resolution ratio≤5%; The test of dispersion stabilization, wet screening is still qualified.
Soup average grain diameter: 0.1～40 μ m.
The oxime bacterium ester that the present invention relates to is compared with prior dosage form with Tebuconazole composite microemulsion, aqueous emulsion, suspension emulsion has outstanding characteristics and significantly progressive:
1, adopt water as main medium, raw material is cheap and easy to get, simultaneously, makes production, packing, transportation, the use of product safer.
2, compare with wetting powder, water dispersible granules, the processing technology of the oxime bacterium ester that the present invention relates to and three kinds of formulations of Tebuconazole composition is simple, the production efficiency height has avoided processing or packing (use) process problem, the problem includes: problems such as dust pollution, high energy consumption, poor efficiency.
3, it is thinner that the oxime bacterium ester that the present invention relates to and Tebuconazole composition waterborne preparation and existing formulation are compared the soup particle diameter, helps the absorption of medicament, and drug effect is better.
4, oxime bacterium ester that the present invention relates to and Tebuconazole composition waterborne preparation, microemulsion, aqueous emulsion, suspension emulsion have been comprised, can adopt different auxiliary agents and production technology can prepare different formulation products according to the difference of active constituent content, can better meet the need of market.
Embodiment
In order to make the object of the invention and technical scheme clearer, give detailed explanation by the following specific embodiments, but be not limited to these concrete examples.
Oxime bacterium ester and Tebuconazole composite microemulsion embodiment
Embodiment 1 9% oxime bacterium ester tebuconazole microemulsion
Each raw material mass percent is as follows: (95%) 32 kilogram of the former medicine of oxime bacterium ester, (95%) 64 kilogram of the former medicine of Tebuconazole, turpentine oil double centner, 50 kilograms of ethanol, 15 kilograms of penetrant ts, 35 kilograms of No. 601, farming breasts, 30 kilograms of Tween 80s, 40 kilograms of calcium dodecyl benzene sulfonates, 634 kilograms in water; During production, oxime bacterium ester, Tebuconazole, turpentine oil, ethanol, penetrant t, No. 601, farming breast, Tween 80, calcium dodecyl benzene sulfonate are added in the reactor, with 1000 rev/mins, stirred 20 minutes, fully dissolving forms oil phase, slowly add entry, stirred 15 minutes, and became the liquid of transparent and homogeneous, promptly get 9% oxime bacterium ester tebuconazole microemulsion.
Embodiment 2 18% oxime bacterium ester tebuconazole microemulsions
Each raw material mass percent is as follows: (95%) 64 kilogram of the former medicine of oxime bacterium ester, (95%) 127 kilogram of the former medicine of Tebuconazole, 80 kilograms in turpentine oil, 40 kilograms of gaultherolins, 50 kilograms of isopropyl alcohols, 30 kilograms of N-Methyl pyrrolidone, 15 kilograms of water-soluble azones, 30 kilograms of No. 701, farming breasts, 80 50 kilograms of OP-15,40 kilograms of calcium dodecyl benzene sulfonates, neopelex 20,454 kilograms in water; During production, oxime bacterium ester, Tebuconazole, turpentine oil, gaultherolin, isopropyl alcohol, N-Methyl pyrrolidone, water-soluble azone, No. 701, farming breast, OP-15, calcium dodecyl benzene sulfonate, neopelex are added in the reactor, with 2000 rev/mins, stirred 20 minutes, fully dissolving forms oil phase, slowly add entry, stirred 15 minutes, and became the liquid of transparent and homogeneous, promptly get 18% oxime bacterium ester tebuconazole microemulsion.
Embodiment 3 24% oxime bacterium ester tebuconazole microemulsions
Each raw material mass percent is as follows: (95%) 85 kilogram of the former medicine of oxime bacterium ester, (95%) 169 kilogram of the former medicine of Tebuconazole, 110 kilograms in turpentine oil, 40 kilograms of gaultherolins, 50 kilograms in acetone, 30 kilograms of undecyl alcohols, 15 kilograms of water-soluble azones, JFC 10,40 kilograms of EL-60,20 kilograms of No. 403, farming breasts, 50 kilograms of No. 34, farming breasts, 40 kilograms of calcium dodecyl benzene sulfonates, lauryl sodium sulfate 30,454 kilograms in water.During production, oxime bacterium ester, Tebuconazole, turpentine oil, gaultherolin, acetone, undecyl alcohol, water-soluble azone, JFC, EL-60, No. 403, farming breast, No. 34, farming breast, calcium dodecyl benzene sulfonate, neopelex are added in the reactor, with 2000 rev/mins, stirred 25 minutes, fully dissolving forms oil phase, slowly add entry, stirred 25 minutes, and became the liquid of transparent and homogeneous, promptly get 24% oxime bacterium ester tebuconazole microemulsion.
Oxime bacterium ester tebuconazole aqueous emulsion embodiment
Embodiment 4 9% oxime bacterium ester tebuconazole aqueous emulsions
Each raw material mass percent is as follows: (95%) 32 kilogram of the former medicine of oxime bacterium ester, (95%) 64 kilogram of the former medicine of Tebuconazole, the turpentine oil double centner, 30 kilograms of glycerine, 15 kilograms of penetrant ts, 10 kilograms of GPE50,20 kilograms of No. 601, farming breasts, 30 kilograms of octanol polyoxyethylene ether phosphates, 15 kilograms of sodium metnylene bis-naphthalene sulfonates, 684 kilograms in water; During production, oxime bacterium ester, Tebuconazole, turpentine oil are added in the reactor, with 1000 rev/mins, stirring and dissolving is a homogeneous liquid, adds glycerine, penetrant t, GPE50, No. 601, farming breast, octanol polyoxyethylene ether phosphate, sodium metnylene bis-naphthalene sulfonate, water, stirred 30 minutes, fully mixing is transferred in the high speed shear reactor, with 10000 rev/mins, sheared 20 minutes, and promptly got 9% oxime bacterium ester tebuconazole aqueous emulsion.
Embodiment 5 24% oxime bacterium ester tebuconazole aqueous emulsions
Each raw material mass percent is as follows: (95%) 85 kilogram of the former medicine of oxime bacterium ester, (95%) 169 kilogram of the former medicine of Tebuconazole, 120 kilograms in turpentine oil, 20 kilograms of gaultherolins, 20 kilograms of propane diols, 20 kilograms of ethylene glycol, 20 kilograms of water-soluble azones, the JFC10 kilogram, 20 kilograms of octanols, 40 kilograms of the two stearates of Macrogol 6000,30 kilograms in fatty alcohol-polyoxyethylene ether phosphoric acid fat, 30 kilograms of calcium lignosulfonates, 416 kilograms in water; During production, oxime bacterium ester, Tebuconazole, turpentine oil, gaultherolin are added in the reactor, with 1200 rev/mins, stirring and dissolving is a homogeneous liquid, adds propane diols, ethylene glycol, water-soluble azone, JFC, octanol, the two stearates of Macrogol 6000, fatty alcohol-polyoxyethylene ether phosphoric acid fat, calcium lignosulfonate, water, stirred 35 minutes, fully mixing is transferred in the high speed shear reactor, with 12000 rev/mins, sheared 25 minutes, and promptly got 24% oxime bacterium ester tebuconazole aqueous emulsion.
Embodiment 6 36% oxime bacterium ester tebuconazole aqueous emulsions
Each raw material mass percent is as follows: (95%) 126.5 kilogram of the former medicine of oxime bacterium ester, (95%) 252.7 kilogram of the former medicine of Tebuconazole, 150 kilograms in turpentine oil, 40 kilograms of gaultherolins, 40 kilograms of ethylene glycol, 20 kilograms of water-soluble azones, 10 kilograms of silicone defoaming agents, 40 kilograms in alkyl phenol polyoxyethylene nonylphenol ether phosphoric acid fat, 30 kilograms of No. 1602, farming breasts, 40 kilograms of polycarboxylate T36,250.8 kilograms in water; During production, oxime bacterium ester, Tebuconazole, turpentine oil, gaultherolin are added in the reactor, with 1500 rev/mins, stirring and dissolving is a homogeneous liquid, adds ethylene glycol, water-soluble azone, silicone defoaming agent, alkyl phenol polyoxyethylene nonylphenol ether phosphoric acid fat, No. 1602, farming breast, polycarboxylate T36, water, stirred 40 minutes, fully mixing is transferred in the high speed shear reactor, with 15000 rev/mins, sheared 30 minutes, and promptly got 36% oxime bacterium ester tebuconazole aqueous emulsion.
Oxime bacterium ester Tebuconazole suspension emulsion embodiment
Embodiment 7 9% oxime bacterium ester Tebuconazole suspension emulsions
Each raw material mass percent is as follows: (95%) 32 kilogram of the former medicine of oxime bacterium ester, (95%) 64 kilogram of the former medicine of Tebuconazole, 30 kilograms in turpentine oil, 30 kilograms of glycerine, 20 kilograms of penetrant ts, 5 kilograms of GPE50,5 kilograms of silicone defoaming agents, 25 kilograms of xanthans, 20 kilograms of No. 1600, farming breasts, 2,700 20 kilograms of polycarboxylates, 20 kilograms of sodium lignin sulfonates, 729 kilograms in water; During production, oxime bacterium ester, turpentine oil, No. 1600, farming breast, water are added in the high speed shear reactor, with 10000 rev/mins, high speed shear 30 minutes makes it to become the liquid of homogeneous, prepares the trifloxystrobin water emulsion, and is stand-by.In another reactor, add Tebuconazole, glycerine, penetrant t, GPE50, silicone defoaming agent, polycarboxylate 2700, sodium lignin sulfonate, water, with 3000 rev/mins, sand milling 60 minutes, measure the particle size of suspension, when average grain diameter during less than 5 μ m, trifloxystrobin water emulsion, xanthans sand milling that adding prepares 30 minutes promptly get 9% oxime bacterium ester Tebuconazole suspension emulsion.
Embodiment 8 24% oxime bacterium ester Tebuconazole suspension emulsions
Each raw material mass percent is as follows: (95%) 85 kilogram of the former medicine of oxime bacterium ester, (95%) 169 kilogram of the former medicine of Tebuconazole, 50 kilograms in turpentine oil, 20 kilograms of gaultherolins, 30 kilograms of sorbierites, 25 kilograms of water-soluble azones, 10 kilograms of silicone defoaming agents, 15 kilograms of sodium carboxymethylcelluloses, 20 kilograms of octyl phosphates, 15 kilograms of the two stearates of PEG400,2,700 40 kilograms of polycarboxylates, 10 kilograms in sodium butylnaphthalenesulfonate water, 511 kilograms in water; During production, oxime bacterium ester, turpentine oil, gaultherolin, octyl phosphate, the two stearates of PEG400, water are added in the high speed shear reactor, with 12000 rev/mins, high speed shear 35 minutes, make it to become the liquid of homogeneous, prepare the trifloxystrobin water emulsion, stand-by.In another reactor, add Tebuconazole, sorbierite, water-soluble azone, silicone defoaming agent, polycarboxylate 2700, sodium lignin sulfonate, sodium butylnaphthalenesulfonate, water, with 3000 rev/mins, sand milling 120 minutes, measure the particle size of suspension, when average grain diameter during less than 5 μ m, trifloxystrobin water emulsion, sodium carboxymethylcellulose sand milling that adding prepares 30 minutes promptly get 24% oxime bacterium ester Tebuconazole suspension emulsion.
Embodiment 9 51% oxime bacterium ester Tebuconazole suspension emulsions
Each raw material mass percent is as follows: (95%) 179 kilogram of the former medicine of oxime bacterium ester, (95%) 357.9 kilogram of the former medicine of Tebuconazole, 85 kilograms in turpentine oil, 30 kilograms of gaultherolins, 10 kilograms of sorbierites, 10 kilograms of ethylene glycol, 10 kilograms of penetrant ts, 10 kilograms of water-soluble azones, 5 kilograms of silicone defoaming agents, 5 kilograms of isooctanol, 0.5 kilogram of polyvinyl alcohol, 20 kilograms of sorbester p37s, 20 kilograms in fatty alcohol-polyoxyethylene ether phosphoric acid fat, 30 kilograms of nekal formaldehyde condensation products, 20 kilograms in sodium lignin sulfonate water, 207.6 kilograms in water; During production, oxime bacterium ester, turpentine oil, gaultherolin, sorbester p37, fatty alcohol-polyoxyethylene ether phosphoric acid fat, water are added in the high speed shear reactor, with 15000 rev/mins, high speed shear 40 minutes, make it to become the liquid of homogeneous, prepare the trifloxystrobin water emulsion, stand-by.In another reactor, add Tebuconazole, sorbierite, ethylene glycol, penetrant t, water-soluble azone, silicone defoaming agent, isooctanol, nekal formaldehyde condensation products, sodium lignin sulfonate, water, with 3000 rev/mins, sand milling 150 minutes, measure the particle size of suspension, when average grain diameter during less than 5 μ m, trifloxystrobin water emulsion, polyvinyl alcohol sand milling that adding prepares 35 minutes promptly get 51% oxime bacterium ester Tebuconazole suspension emulsion.
Oxime bacterium ester and Tebuconazole composition waterborne preparation stability test.
With reference to the World Food Programme (FAO) method, measure oxime bacterium ester tebuconazole microemulsion, aqueous emulsion, suspension emulsion storage-stable.Medicament is sealed in the ampoule bottle, places (54 ± 2) ℃ incubator respectively, in (0 ± 2) ℃ ,-18 ℃ the refrigerator, preserve 14 days continuously after, the stability of each index of test oxime bacterium ester Tebuconazole waterborne preparation.
Table one different content oxime bacterium ester tebuconazole microemulsion storage-stable result of the test (14 days)
From table one data as can be seen, the every index of oxime bacterium ester tebuconazole microemulsion of different content meets standard-required.
Table two different content oxime bacterium ester tebuconazole microemulsion storage-stable test appearance change (14 days)
| Temperature | 9% oxime bacterium ester tebuconazole microemulsion (embodiment 1) | 18% oxime bacterium ester tebuconazole microemulsion (embodiment 2) | 24% oxime bacterium ester tebuconazole microemulsion (embodiment 3) |
| ??(54±2)℃ | Homogeneous, transparent clear | Homogeneous, transparent clear | Homogeneous, transparent clear |
| ??(0±2)℃ | Homogeneous, transparent clear | Homogeneous, transparent clear | Homogeneous, transparent clear |
| ??-18℃ | Homogeneous, transparent clear | Homogeneous, transparent clear | Translucent, room temperature can be recovered homogeneous, transparent clear voluntarily |
As can be seen from Table II, through storage test, oxime bacterium ester tebuconazole microemulsion preparation outward appearance is good, and the preparation outward appearance also can be recovered normally to meet standard-required voluntarily under the extreme low temperature condition.
Table three different content oxime bacterium ester tebuconazole aqueous emulsion storage-stable result of the test (14 days)
From table three data as can be seen, the every index of oxime bacterium ester tebuconazole microemulsion of different content meets standard-required.
Table four different content oxime bacterium ester tebuconazole aqueous emulsion storage-stable test appearance change (14 days)
| Temperature | 9% oxime bacterium ester tebuconazole aqueous emulsion (embodiment 4) | 24% oxime bacterium ester tebuconazole aqueous emulsion (embodiment 5) | 36% oxime bacterium ester tebuconazole aqueous emulsion (embodiment 6) |
| ??(54±2℃ | Not stratified, there is not precipitation | Not stratified, there is not precipitation | Not stratified, there is not precipitation |
| ??(0±2)℃ | Not stratified, there is not precipitation | Not stratified, there is not precipitation | Not stratified, there is not precipitation |
| ??-18℃ | Not stratified, there is not precipitation | Not stratified, there is not precipitation | Not stratified, there is not precipitation |
As can be seen from Table IV, through storage test, oxime bacterium ester tebuconazole aqueous emulsion preparation outward appearance is good, meets standard-required.
Table five different content oxime bacterium ester Tebuconazole suspension emulsion storage-stable result of the test (14 days)
From table five data as can be seen, the every index of oxime bacterium ester Tebuconazole suspension emulsion of different content meets standard-required.
Table six different content oxime bacterium ester Tebuconazole suspension emulsion storage-stable test appearance change (14 days)
| Temperature | 9% oxime bacterium ester Tebuconazole suspension emulsion (embodiment 7) | 24% oxime bacterium ester Tebuconazole suspension emulsion (embodiment 8) | 51% oxime bacterium ester Tebuconazole suspension emulsion (embodiment 9) |
| ??(54±2)℃ | Not stratified, there is not precipitation | Not stratified, there is not precipitation | Not stratified, there is not precipitation |
| ??(0±2)℃ | Not stratified, there is not precipitation | Not stratified, there is not precipitation | Not stratified, there is not precipitation |
| ??-18℃ | Not stratified, there is not precipitation | Not stratified, there is not precipitation | Not stratified, there is not precipitation |
As can be seen from Table VI, through storage test, oxime bacterium ester Tebuconazole suspension emulsion preparation outward appearance is good, meets standard-required.
Test of pesticide effectiveness embodiment
Indoor, adopt pot-culture method to measure of the therapeutic action of 24% oxime bacterium ester tebuconazole microemulsion different dosage forms such as (embodiment 3) to powdery mildew of cucumber, result of the test is as follows:
Different dosage forms such as table seven employing pot-culture method mensuration oxime bacterium ester tebuconazole microemulsion are prevented and treated the indoor therapeutic action result of powdery mildew of cucumber bacterium
From table seven data as can be seen, under equal active ingredient, oxime bacterium ester tebuconazole microemulsion, aqueous emulsion, suspension emulsion are better than oxime bacterium ester Tebuconazole wetting powder, suspending agent, water dispersible granules to the result of treatment of powdery mildew of cucumber.
Claims (15)
1. antiseptic composition waterborne preparation, it is characterized in that composition active ingredient contains oxime bacterium ester, Tebuconazole, preparation raw material mass percent is oxime bacterium ester 3%-20%, Tebuconazole 6%-40%, solvent 0.5%-20%, cosolvent 0-8%, bleeding agent 1%-5%, thickener 0-3%, antifreeze 0%-5%, defoamer 0-3%, surfactant 6%-20%, water surplus.
2. antiseptic composition waterborne preparation according to claim 1, it is characterized by formulation is microemulsion, aqueous emulsion, suspension emulsion.
3. antiseptic composition waterborne preparation according to claim 1 and 2, it is characterized by oxime bacterium ester and Tebuconazole composite microemulsion, contain oxime bacterium ester 3%-8%, Tebuconazole 6%-16%, solvent 0.5%-15%, cosolvent 0.5%-8%, bleeding agent 1%-5%, surfactant 8%-20%, water surplus.
4. antiseptic composition waterborne preparation according to claim 1 and 2, it is characterized by oxime bacterium ester and Tebuconazole composition aqueous emulsion, contain oxime bacterium ester 3%-12%, Tebuconazole 6%-24%, solvent 0.5%-20%, antifreeze 0.5%-5%, bleeding agent 1%-5%, defoamer 0.1%-3%, surfactant 6%-12%, water surplus.
5. antiseptic composition waterborne preparation according to claim 1 and 2, it is characterized by oxime bacterium ester and Tebuconazole composition suspended emulsion, contain oxime bacterium ester 3%-17%, Tebuconazole 6%-34%, solvent 0.5%-15%, thickener 0.1%-3%, antifreeze 0.5%-5%, bleeding agent 1%-5%, defoamer 0.1%-3%, surfactant 6%-12%, water surplus.
6. according to claim 1,3,4,5 each described antiseptic composition waterborne preparations, it is characterized by described solvent and comprise in turpentine oil, the gaultherolin at least a.
7. according to claim 1 or 3 described antiseptic composition waterborne preparations, it is characterized by described cosolvent comprises in alcohols, the ketone at least a, wherein, alcohols comprises ethanol, propyl alcohol, isopropyl alcohol, n-butanol, isobutanol, amylalcohol, isoamyl alcohol, hexanol, enanthol, octanol, nonyl alcohol, decyl alcohol, undecyl alcohol, lauryl alcohol, cyclopentanol, cyclohexanol, phenmethylol; Ketone comprises acetone, butanone, acetophenone, propiophenone, N-Methyl pyrrolidone, N-ethyl pyrrolidone.
8. according to claim 1,4,5 each described antiseptic composition waterborne preparations, it is characterized by described antifreeze and contain in glycerine, ethylene glycol, propane diols, the sorbierite at least a.
9. according to claim 1,3,4,5 each described bleeding agents, it is characterized by comprise in penetrant t, JFC, the water-soluble azone at least a.
10. antiseptic composition waterborne preparation according to claim 1 or 5 is characterized by described thickener and comprises in gelatin, gum Arabic, xanthans, soluble starch, polyvinyl alcohol, the sodium carboxymethylcellulose at least a.
11. according to claim 1,4,5 each described antiseptic composition waterborne preparations, it is characterized by described defoamer, to comprise polyoxyethylene polyoxypropylene glycerols, silicone defoaming agent, alcohols at least a, and wherein alcohols comprises enanthol, octanol, isooctanol, nonyl alcohol, decyl alcohol, undecyl alcohol, lauryl alcohol.
12. according to claim 1,3,4,5 each described antiseptic composition waterborne preparations, it is characterized by described surfactant and be selected from polyethers, the ester class, phosphoric acid ester, Sulfonates, Sulfates, the lignin sulfonic acid salt, naphthalenesulfonate, the polycarboxylic acid salt is at least a, wherein, polyethers comprises alkylphenol polyoxyethylene, the benzylphenol APEO, the phenethyl phenol polyethenoxy ether, phenethyl fluosite APEO, alkyl phenol formaldehyde resin polyoxyethylene ether, fatty alcohol-polyoxyethylene ether, phenethyl phenol polyethenoxy polyethenoxy ether, triphen ethyl phenol polyoxyethylene poly-oxygen propylene aether, the sorbitan fatty acid ester APEO, castor oil polyoxyethylene ether; The ester class comprises sorbitan fatty acid ester, polyoxyethylene carboxylate, cithrol; Phosphoric acid ester comprises alkyl phenol polyoxyethylene nonylphenol ether phosphoric acid fat and salt, fatty alcohol-polyoxyethylene ether phosphoric acid fat and salt, octyl phosphate and salt thereof, octanol polyoxyethylene ether phosphate and salt thereof; Sulfonates includes neopelex, calcium dodecyl benzene sulfonate, magnesium dodecyl benzene sulfonate etc.; Sulfates includes lauryl sodium sulfate, Stepanol MG; The lignin sulfonic acid salt includes sodium lignin sulfonate, calcium lignosulfonate; Naphthalenesulfonate includes sodium metnylene bis-naphthalene sulfonate, sodium butylnaphthalenesulfonate, alkylnaphthalene sulfonate formaldehyde condensation products; The polycarboxylic acid salt includes polycarboxylate 2700, polycarboxylate T36, polycarboxylate YUS-WG5.
13. the process for producing of claim 1 or 3 described oxime bacterium esters and Tebuconazole composite microemulsion is characterized by:
At ambient temperature, earlier oxime bacterium ester, Tebuconazole, solvent, cosolvent, bleeding agent, surfactant are added in the reactor by the requirement of raw material mass percent, with 100-5000 rev/min, stirred 15-45 minute, form oil phase, add entry again, stirred 10-30 minute, make it to become the liquid of homogeneous, promptly get oxime bacterium ester and Tebuconazole composite microemulsion.
14. the process for producing of claim 1 or 4 described oxime bacterium esters and Tebuconazole composition aqueous emulsion is characterized by:
At ambient temperature, earlier oxime bacterium ester, Tebuconazole, solvent are added in the reactor by the requirement of raw material mass percent,, stir with 100-5000 rev/min, make it to become the liquid of homogeneous, add antifreeze, bleeding agent, defoamer, surfactant, water, stirred 20-60 minute, mix, transfer in the high speed shear reactor, with 1000-20000 rev/min, high speed shear 20-90 minute, promptly get oxime bacterium ester and Tebuconazole composition aqueous emulsion.
15. the process for producing of claim 1 or 5 described oxime bacterium esters and Tebuconazole composition suspended emulsion is characterized by:
At ambient temperature, earlier oxime bacterium ester, solvent, surfactant, water are added in the high speed shear reactor, with 1000-20000 rev/min by the requirement of raw material mass percent, high speed shear 30-90 minute, make it to become the liquid of homogeneous, prepare the trifloxystrobin water emulsion, stand-by.In another reactor, add Tebuconazole, antifreeze, bleeding agent, defoamer, surfactant, water, with 100-5000 rev/min, stir, after mixing, add in the sand mill, with 100-5000 rev/min, sand milling 30-180 minute, with the particle size of laser particle diameter distribution instrument mensuration suspension, when average grain diameter during less than 5 μ m, add the trifloxystrobin water emulsion, the thickener that prepare, sand milling 20-40 minute, promptly get oxime bacterium ester and Tebuconazole composition suspended emulsion.
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| CN108160227A (en) * | 2017-12-27 | 2018-06-15 | 苏州佳辉化工有限公司 | A kind of method of industrial bactericide lotion production |
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