CN1241358A - Copper resinate bactericidal acaricide and preparation method thereof - Google Patents
Copper resinate bactericidal acaricide and preparation method thereof Download PDFInfo
- Publication number
- CN1241358A CN1241358A CN 99114686 CN99114686A CN1241358A CN 1241358 A CN1241358 A CN 1241358A CN 99114686 CN99114686 CN 99114686 CN 99114686 A CN99114686 A CN 99114686A CN 1241358 A CN1241358 A CN 1241358A
- Authority
- CN
- China
- Prior art keywords
- copper
- acaricide
- rosin
- germicidal
- preparation
- Prior art date
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 44
- 239000010949 copper Substances 0.000 title claims abstract description 44
- 230000000895 acaricidal effect Effects 0.000 title claims abstract description 26
- 239000000642 acaricide Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 230000000844 anti-bacterial effect Effects 0.000 title abstract description 9
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims abstract description 25
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims abstract description 23
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- 150000001879 copper Chemical class 0.000 claims abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 9
- 239000010779 crude oil Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000004945 emulsification Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000002699 waste material Substances 0.000 claims abstract description 3
- 230000002070 germicidal effect Effects 0.000 claims description 19
- 239000003995 emulsifying agent Substances 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 4
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 4
- 239000012752 auxiliary agent Substances 0.000 claims description 3
- 239000002283 diesel fuel Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 claims description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 2
- 239000001293 FEMA 3089 Substances 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- -1 industrial naptha Substances 0.000 claims description 2
- 239000010721 machine oil Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000002023 wood Substances 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims 3
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 240000007594 Oryza sativa Species 0.000 abstract description 3
- 235000007164 Oryza sativa Nutrition 0.000 abstract description 3
- 230000001580 bacterial effect Effects 0.000 abstract description 3
- 235000009566 rice Nutrition 0.000 abstract description 3
- 235000013311 vegetables Nutrition 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 2
- 241000238876 Acari Species 0.000 abstract 1
- 231100000674 Phytotoxicity Toxicity 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 12
- 239000003899 bactericide agent Substances 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 5
- 231100000572 poisoning Toxicity 0.000 description 5
- 230000000607 poisoning effect Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 241000233639 Pythium Species 0.000 description 2
- SVOAENZIOKPANY-CVBJKYQLSA-L copper;(z)-octadec-9-enoate Chemical compound [Cu+2].CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O SVOAENZIOKPANY-CVBJKYQLSA-L 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 239000003640 drug residue Substances 0.000 description 2
- 230000003129 miticidal effect Effects 0.000 description 2
- 244000144730 Amygdalus persica Species 0.000 description 1
- 239000005739 Bordeaux mixture Substances 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000207199 Citrus Species 0.000 description 1
- 239000005752 Copper oxychloride Substances 0.000 description 1
- 244000241257 Cucumis melo Species 0.000 description 1
- 235000015510 Cucumis melo subsp melo Nutrition 0.000 description 1
- 235000011511 Diospyros Nutrition 0.000 description 1
- 244000236655 Diospyros kaki Species 0.000 description 1
- 206010023126 Jaundice Diseases 0.000 description 1
- 235000006040 Prunus persica var persica Nutrition 0.000 description 1
- 241000220324 Pyrus Species 0.000 description 1
- 241001282571 Salmonella enterica subsp. enterica serovar Tennessee Species 0.000 description 1
- FJJCIZWZNKZHII-UHFFFAOYSA-N [4,6-bis(cyanoamino)-1,3,5-triazin-2-yl]cyanamide Chemical compound N#CNC1=NC(NC#N)=NC(NC#N)=N1 FJJCIZWZNKZHII-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000003139 biocide Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- HKMOPYJWSFRURD-UHFFFAOYSA-N chloro hypochlorite;copper Chemical compound [Cu].ClOCl HKMOPYJWSFRURD-UHFFFAOYSA-N 0.000 description 1
- 235000020971 citrus fruits Nutrition 0.000 description 1
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- AEJIMXVJZFYIHN-UHFFFAOYSA-N copper;dihydrate Chemical compound O.O.[Cu] AEJIMXVJZFYIHN-UHFFFAOYSA-N 0.000 description 1
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 1
- 229940112669 cuprous oxide Drugs 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 235000021017 pears Nutrition 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000017260 vegetative to reproductive phase transition of meristem Effects 0.000 description 1
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a copper resinate bactericidal acaricide and a preparation method thereof. It uses special rosin, KOH (or NaOH), soluble copper salt and organic solvent as raw materials, and makes them react under the condition of heating, and adopts centrifugal machine and oil-water separator to separate crude oil, and makes them pass through the processes of emulsification so as to obtain the copper resinate bactericidal acaricide. The production method has the advantages of low production cost, high product yield, less three wastes, extremely high adhesion of the prepared product and no phytotoxicity when used in an effective range. The product of the invention has excellent performance and special effects on bacterial leaf streak of rice, vegetable soft rot, soft rot and the like. And not only does not induce the damage of mites, but also has higher acaricidal effect.
Description
The invention belongs to organic compound biocide technical field, relate in particular to copper resinate germicidal acaricide and preparation method thereof.
In agricultural production, the copper series bactericidal agent is owing to there is the advantage that does not develop immunity to drugs with fungicidal spectrum is wide, drug effect is high, flourishing long time always for many years, proportion maximum in bactericide, kind also constantly increases, be use bordeaux mixture in 1882 the earliest, then use multiple inorganic copper agent, as Kocide SD, copper oxychloride, cuprous oxide etc.But inorganic copper agent is used in the conduct of copper sensitivity such as peach, Lee, pears, persimmon, melon etc. as last easy generation poisoning, and brings out easily that the mite class is rampant to be taken place.And the poisoning of organic copper preparation is less relatively, and the degree of bringing out the harm of mite class is also less.As the Copoloid of development U.S. Tennessee company sixties (Tc-90[Farm Chemicals, 127, NO.6,62 (1964)]) on these two kinds of performances just better.But it exists following problem again: 1, product instability, its composition are the mixture of multiple copper abietinate and copper oleate, and the easy oxidation deterioration of copper abietinate, product are buied property for a long time and given birth to precipitation.2, copper oleate mixes in wherein making product adhesion decline; Though 3, its poisoning is more much lower than inorganic copper, still has poisoning, this makes this product fail to promote and comes.Publication number is that the organic copper agent used as bactericide and acaricide of CN1176740A has then overcome above-mentioned shortcoming more effectively.But this product still has following deficiency on the preparation method, 1, raw materials used single, and preparation cost is higher; 2, separating method is original, and yield is lower, and substantial oil is sneaked in the waste water and dregs.3, reaction at normal temperatures and pressures, the reaction time is long, and not thorough; 4, the product emulsifying effectiveness is relatively poor.
The object of the present invention is to provide raw material extensively to reach and produce the product yield height, production cost is low, the preparation method of the preparation copper resinate germicidal acaricide that the three wastes are few.
Another object of the present invention is to be to provide bactericidal property superior, and multiple diseases such as bacterial leaf streak of rice, vegetables pythium rot, soft rot are had special efficacy, and product adhesion is high, and drug residue is low, and the copper resinate germicidal acaricide of miticidal effect is arranged.
Copper resinate germicidal acaricide of the present invention is made up of following weight proportion:
Copper resinate 10-30%
Organic solvent 60-83%
Emulsifier 5-10%
Auxiliary agent 0-2%
The preparation method of copper resinate germicidal acaricide of the present invention is as follows: with extraordinary rosin, KOH or NaoH is raw material, under heating condition, make the two reaction, the insulation certain hour is a raw material with aforementioned product and soluble copper salt, organic solvent again, the three is mixed stirring, under heating condition, react copper resinate crude oil and waste water and dregs, adopt centrifuge and oil water separator to isolate copper resinate crude oil, the copper resinate crude oil dropping emulsifier and the solvent that separate the back gained are carried out emulsification, get copper resinate germicidal acaricide at last.
The preparation method of copper resinate germicidal acaricide of the present invention, its raw material is made up of following weight proportion:
Extraordinary rosin 18-32%
KOH or NaiH 1.8-10%
Soluble copper salt 1.1-2.0%
Organic solvent 60-70%
Emulsifier is an amount of
Wherein preferred version is: extraordinary rosin 23%
Organic solvent 70% KOH (or NaoH) 5%
Soluble copper salt 1.1%
Emulsifier 6%
Extraordinary rosin refers to wood rosin, hydrogenated rosin, vinsol, polymerized rosin, maleated rosin, disproportionated rosin.
Soluble copper salt is mainly copper sulphate, copper nitrate, copper chloride.
Organic solvent is: diesel oil, machine oil, industrial naptha, turpentine oil, toluene, dimethylbenzene, styrene, cyclohexanone, MEK, glycerine.
The preparation method of copper resinate germicidal acaricide of the present invention is owing to be to react under heating condition, so the reaction time reduces, product yield improves, and simultaneously raw materials used is extraordinary rosin, and production cost is reduced greatly.Adopt centrifuge to separate and separate with oil water separator, make and separate thoroughly, three refuses reduce.The copper resinate germicidal acaricide superior performance that adopts preparation method of the present invention to make, bacterial leaf streak of rice, vegetables pythium rot, soft rot, citrus carbon jaundice disease, canker etc. there is remarkable result, product adhesion is high, result of use is constant half an hour behind the rain before the rain, drug residue is lower than the existing copper series bactericidal agent, in prescribed limit, use no any poisoning, also can use at flowering phase of crop; As other copper bactericide the harm of mite class not taking place, has higher miticidal effect on the contrary.
Below in conjunction with specific embodiment the present invention is described in detail:
To produce hydrogenated resin acid copper agent used as bactericide and acaricide 370g is example:
Get hydrogenated rosin 150g, 33%KOH aqueous solution 90g adds conical flask with hydrogenated rosin and is heated to fusion, open agitation and dropping KOH solution, be heated to 106 ℃, be incubated 1 hour, with previous reaction product and 40% copper-bath 237g, diesel oil 230g mixes, and adds in the conical flask, is heated with stirring to 80 ℃, be incubated after two hours, make the copper resinate mixture, adopt centrifuge to separate in this mixture, liquid phase changes the profit height separator over to, separate copper resinate crude oil 340g, the copper resinate crude oil that makes is added emulsifier " 8203 " 30g, promptly get hydrogenated resin acid copper agent used as bactericide and acaricide 370g, product yield 90% through emulsification.
Claims (8)
1, copper resinate germicidal acaricide, it is as follows that it forms proportioning: (by weight)
Copper resinate 10-30%, organic solvent 60-83%,
Emulsifier 5-10%, auxiliary agent 0-2%
2, copper resinate germicidal acaricide preparation method, be to be raw material with extraordinary rosin, KOH or NaoH, soluble copper salt, organic solvent and emulsifier, earlier extraordinary rosin and KOH or NaoH are reacted under heating condition, then aforementioned reactants is mixed with soluble copper salt and organic solvent, stir, reaction generates copper resinate crude oil and waste material under heating condition, separating obtained copper resinate crude oil dropping emulsifier and solvent are carried out emulsification, promptly make copper resinate germicidal acaricide of the present invention.
3, the preparation method of copper resinate germicidal acaricide according to claim 2 is characterized in that, described raw material weight proportioning is:
Extraordinary rosin 18-32%, soluble copper salt 1.1-2.0%
Organic solvent 60-70%, KOH (or NaoH) 1.8-10%
Emulsifier is an amount of, auxiliary agent 0-2%
4, the preparation method of copper resinate germicidal acaricide according to claim 2 is characterized in that: extraordinary rosin is wood rosin, disproportionated rosin, hydrogenated rosin, vinsol, polymerized rosin, maleated rosin.
5, the preparation method of copper resinate germicidal acaricide according to claim 2, wherein said organic solvent is diesel oil, machine oil, industrial naptha, turpentine oil, toluene, dimethylbenzene, styrene, cyclohexanone, MEK, glycerine.
6, copper resinate germicidal acaricide preparation method according to claim 2, it is characterized in that: the heating-up temperature of described extraordinary rosin and KOH or NaoH reaction is 80 ℃～240 ℃, and aforementioned reactants and soluble copper salt, organic solvent reaction temperature are 40 ℃～120 ℃.
7, the preparation method of copper resinate germicidal acaricide according to claim 2 is characterized in that: copper resinate crude oil separated with oil water separator with separating by centrifuge of waste water and dregs.
8, the preparation method of copper resinate germicidal acaricide according to claim 2 is characterized in that: described aforementioned reactants and soluble copper salt, organic solvent heating reaction time are 2-4 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99114686 CN1241358A (en) | 1999-02-16 | 1999-02-16 | Copper resinate bactericidal acaricide and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99114686 CN1241358A (en) | 1999-02-16 | 1999-02-16 | Copper resinate bactericidal acaricide and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1241358A true CN1241358A (en) | 2000-01-19 |
Family
ID=5277738
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 99114686 Pending CN1241358A (en) | 1999-02-16 | 1999-02-16 | Copper resinate bactericidal acaricide and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1241358A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935275A (en) * | 2009-06-29 | 2011-01-05 | 孔波 | Preparation method and application of gum rosin acid copper |
| CN103497101A (en) * | 2013-10-11 | 2014-01-08 | 广东植物龙生物技术有限公司 | Preparation method and application of resin acid copper salt synthesized by aqueous phase process |
| CN104478705A (en) * | 2014-11-11 | 2015-04-01 | 柳州市惠农化工有限公司 | Copper abietate raw drug and preparation method and application thereof |
-
1999
- 1999-02-16 CN CN 99114686 patent/CN1241358A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935275A (en) * | 2009-06-29 | 2011-01-05 | 孔波 | Preparation method and application of gum rosin acid copper |
| CN103497101A (en) * | 2013-10-11 | 2014-01-08 | 广东植物龙生物技术有限公司 | Preparation method and application of resin acid copper salt synthesized by aqueous phase process |
| CN104478705A (en) * | 2014-11-11 | 2015-04-01 | 柳州市惠农化工有限公司 | Copper abietate raw drug and preparation method and application thereof |
| CN104478705B (en) * | 2014-11-11 | 2016-04-27 | 柳州市惠农化工有限公司 | The former medicine of a kind of copper rosinate, preparation method and application |
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