JPH049308A - Germicide composition for agriculture and horticulture - Google Patents
Germicide composition for agriculture and horticultureInfo
- Publication number
- JPH049308A JPH049308A JP11242590A JP11242590A JPH049308A JP H049308 A JPH049308 A JP H049308A JP 11242590 A JP11242590 A JP 11242590A JP 11242590 A JP11242590 A JP 11242590A JP H049308 A JPH049308 A JP H049308A
- Authority
- JP
- Japan
- Prior art keywords
- copper
- zeolite
- substance
- ion
- calcium
- 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.)
- Pending
Links
- 239000000203 mixture Substances 0.000 title abstract description 32
- 230000002070 germicidal effect Effects 0.000 title abstract 5
- 238000003898 horticulture Methods 0.000 title description 3
- 239000010457 zeolite Substances 0.000 claims abstract description 28
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 26
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000012013 faujasite Substances 0.000 claims abstract description 11
- 239000004480 active ingredient Substances 0.000 claims abstract description 10
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 3
- 239000000417 fungicide Substances 0.000 claims description 8
- 230000000855 fungicidal effect Effects 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 125000004436 sodium atom Chemical group 0.000 claims description 2
- 229910009116 xCuO Inorganic materials 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 52
- 238000005342 ion exchange Methods 0.000 abstract description 37
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 abstract description 30
- 201000010099 disease Diseases 0.000 abstract description 27
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 abstract description 17
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 abstract description 17
- 229910001424 calcium ion Inorganic materials 0.000 abstract description 17
- 229910001431 copper ion Inorganic materials 0.000 abstract description 17
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 15
- 229910052802 copper Inorganic materials 0.000 abstract description 15
- 239000010949 copper Substances 0.000 abstract description 15
- 230000000694 effects Effects 0.000 abstract description 7
- 229910001415 sodium ion Inorganic materials 0.000 abstract description 6
- 231100000674 Phytotoxicity Toxicity 0.000 abstract description 2
- 239000005739 Bordeaux mixture Substances 0.000 abstract 1
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 43
- 239000013078 crystal Substances 0.000 description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- 239000000243 solution Substances 0.000 description 20
- 239000007864 aqueous solution Substances 0.000 description 16
- 239000012153 distilled water Substances 0.000 description 14
- 238000009472 formulation Methods 0.000 description 14
- 239000011575 calcium Substances 0.000 description 12
- 229910052791 calcium Inorganic materials 0.000 description 12
- 240000008067 Cucumis sativus Species 0.000 description 11
- 241000196324 Embryophyta Species 0.000 description 11
- -1 organic acid salts Chemical class 0.000 description 11
- 239000000843 powder Substances 0.000 description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 9
- 235000010799 Cucumis sativus var sativus Nutrition 0.000 description 8
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 8
- 238000000921 elemental analysis Methods 0.000 description 8
- 235000007688 Lycopersicon esculentum Nutrition 0.000 description 7
- 240000007594 Oryza sativa Species 0.000 description 7
- 240000003768 Solanum lycopersicum Species 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 7
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- 235000011121 sodium hydroxide Nutrition 0.000 description 7
- 239000000725 suspension Substances 0.000 description 7
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- 235000006140 Raphanus sativus var sativus Nutrition 0.000 description 6
- 229910000365 copper sulfate Inorganic materials 0.000 description 6
- 239000003814 drug Substances 0.000 description 6
- 229940079593 drug Drugs 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 235000009566 rice Nutrition 0.000 description 6
- 238000005507 spraying Methods 0.000 description 6
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 5
- 244000061176 Nicotiana tabacum Species 0.000 description 5
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 5
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- 229920003023 plastic Polymers 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate group Chemical group S(=O)(=O)([O-])[O-] QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 241000233679 Peronosporaceae Species 0.000 description 4
- 241000589516 Pseudomonas Species 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000004115 Sodium Silicate Substances 0.000 description 4
- 239000001110 calcium chloride Substances 0.000 description 4
- 229910001628 calcium chloride Inorganic materials 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 238000011081 inoculation Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000003449 preventive effect Effects 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 4
- 229910052911 sodium silicate Inorganic materials 0.000 description 4
- 235000013311 vegetables Nutrition 0.000 description 4
- 239000004563 wettable powder Substances 0.000 description 4
- 239000005995 Aluminium silicate Substances 0.000 description 3
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- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- 235000012211 aluminium silicate Nutrition 0.000 description 3
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 230000001580 bacterial effect Effects 0.000 description 3
- 150000001669 calcium Chemical class 0.000 description 3
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 3
- 239000001639 calcium acetate Substances 0.000 description 3
- 235000011092 calcium acetate Nutrition 0.000 description 3
- 229960005147 calcium acetate Drugs 0.000 description 3
- 159000000007 calcium salts Chemical class 0.000 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 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 150000001879 copper Chemical class 0.000 description 3
- 230000000887 hydrating effect Effects 0.000 description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 3
- 230000003902 lesion Effects 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- 229910001388 sodium aluminate Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 241000223600 Alternaria Species 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 2
- 208000035143 Bacterial infection Diseases 0.000 description 2
- 241000207199 Citrus Species 0.000 description 2
- 241001480643 Colletotrichum sp. Species 0.000 description 2
- 244000068988 Glycine max Species 0.000 description 2
- 235000010469 Glycine max Nutrition 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- 241001674048 Phthiraptera Species 0.000 description 2
- 241000233614 Phytophthora Species 0.000 description 2
- 239000004111 Potassium silicate Substances 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- 244000061456 Solanum tuberosum Species 0.000 description 2
- 235000002595 Solanum tuberosum Nutrition 0.000 description 2
- 244000300264 Spinacia oleracea Species 0.000 description 2
- 235000009337 Spinacia oleracea Nutrition 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 241000589634 Xanthomonas Species 0.000 description 2
- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical compound [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 description 2
- 208000022362 bacterial infectious disease Diseases 0.000 description 2
- 239000000440 bentonite Substances 0.000 description 2
- 229910000278 bentonite Inorganic materials 0.000 description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 2
- 229920005551 calcium lignosulfonate Polymers 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 2
- 235000020971 citrus fruits Nutrition 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 2
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- JYIMWRSJCRRYNK-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4] JYIMWRSJCRRYNK-UHFFFAOYSA-N 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
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- 230000000361 pesticidal effect Effects 0.000 description 2
- 229910001414 potassium ion Inorganic materials 0.000 description 2
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 2
- 229910052913 potassium silicate Inorganic materials 0.000 description 2
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- 235000019333 sodium laurylsulphate Nutrition 0.000 description 2
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- 239000000454 talc Substances 0.000 description 2
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- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 1
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- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 235000021012 strawberries Nutrition 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 150000008054 sulfonate salts Chemical class 0.000 description 1
- 125000004354 sulfur functional group Chemical group 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 238000002255 vaccination Methods 0.000 description 1
- 235000020234 walnut Nutrition 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Landscapes
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
本発明は、銅イオンで一部イオン交換された、カルシウ
ムイオン含有A型ゼオライトを有効成分として含有する
ことを特徴とする農園芸用殺菌剤に関する。[Detailed Description of the Invention] <Industrial Application Field> The present invention provides an agricultural and horticultural fungicide characterized by containing calcium ion-containing type A zeolite, which has been partially ion-exchanged with copper ions, as an active ingredient. Regarding.
〈従来の技術〉
従来、果樹、硫菜等の分野では、ボルドー液等の無a銅
剤が用いられている。また、特公昭61−23164号
公報には、ナトリウムイオンを銅イオンで置換した銅置
換アルミノンリケードが、記載されている。<Prior Art> Conventionally, copper-free agents such as Bordeaux liquid have been used in fields such as fruit trees and sulfur vegetables. Further, Japanese Patent Publication No. 61-23164 describes a copper-substituted aluminonilicade in which sodium ions are replaced with copper ions.
また、特公平1−156905号公報には、ある種の銅
置換ゼオライトが記載されているが、
3 <5iCh/AlzCh≦12であることから、A
型ゼオライトではなく、しかもカルシウムイオンを含有
じていないことから本発明のゼオライトとは全く異なる
ものである。In addition, Japanese Patent Publication No. 1-156905 describes a certain type of copper-substituted zeolite, but since 3 <5iCh/AlzCh≦12, A
The zeolite is not a type zeolite and does not contain calcium ions, so it is completely different from the zeolite of the present invention.
〈解決すべき課題〉
従来の銅殺菌剤は効力を発揮する対象病害の範囲が狭か
ったり、作物に薬害をもたらすなどの面から、その適用
範囲に制限があった。<Problems to be Solved> Conventional copper fungicides have limited range of application because they are effective against a narrow range of diseases and cause chemical damage to crops.
さらに、従来の銅置換アルミノンリケードは、銅当りの
効果が不充分であり必ずしも満足できるものとは言い難
く、薬害が少なくかつ低薬量で効果を発揮する高性能な
薬剤の開発が待ち望まれている。In addition, conventional copper-substituted aluminonricades have insufficient effects per copper and cannot be said to be necessarily satisfactory, and the development of high-performance drugs that are less harmful and effective at lower doses is eagerly awaited. ing.
〈課題を解決するための手段〉
このような状況のもとに、薬害が少なくかつ低薬量で効
果を発揮する高性能な薬剤を見い出すべく鋭意検討を重
ねた結果、本発明者らは、−C式〔I〕で示される銅イ
オンで一部イオン交換されたカルシウムイオン含有A型
ゼオライト(以下、本発明物質と称す)が極めて優れた
殺菌活性を有し、しかも問題となる薬害を示さないこと
を見い出し本発明に至った。<Means for Solving the Problems> Under these circumstances, the inventors of the present invention have conducted intensive studies to find a high-performance drug that causes less drug damage and is effective at a low dose. -C Formula [I] The calcium ion-containing type A zeolite partially ion-exchanged with copper ions (hereinafter referred to as the substance of the present invention) has extremely excellent bactericidal activity and does not cause any problematic phytotoxicity. The present invention was based on the discovery that there is no such thing.
すなわち、本発明は、一般式
%式%
〔式中、Mはナトリウム原子またはカリウム原子を表わ
し、x、y、zおよびWは各々下記範囲の数値を表わす
。That is, the present invention is based on the general formula % [where M represents a sodium atom or a potassium atom, and x, y, z and W each represent a numerical value within the following range.
0<x<1.0<3’<1 (旦しx十y≦12≦2
≦2.5.0≦w≦20〕
で示される、フォーンヤケイト群に属する結晶性ゼオラ
イトを有効成分とする農園芸用殺菌剤1を提供する。0<x<1.0<3'<1 (time x y≦12≦2
≦2.5.0≦w≦20] An agricultural and horticultural fungicide 1 is provided, which contains crystalline zeolite belonging to the Founyakeite group as an active ingredient and is represented by the following formula.
本発明物質は、カルシウムイオンを含有することから、
従来のナトリウムイオンを銅イオンで置換した銅置換ゼ
オライトに比べ銅当りの殺菌活性が大幅に向上した。Since the substance of the present invention contains calcium ions,
Compared to conventional copper-substituted zeolite in which sodium ions are replaced with copper ions, the bactericidal activity per copper has been significantly improved.
本発明物質において銅の含有量は任意↓こ決めうるが、
好ましくはw−0に換算して17重量%以下である。The content of copper in the substance of the present invention can be determined arbitrarily, but
Preferably it is 17% by weight or less in terms of w-0.
本発明物質においてカルシウムの含有量′、!イ壬意に
決めうるが、好ましくはw=0に換算して1重量%以上
である。The content of calcium in the substance of the present invention',! Although it can be determined at will, it is preferably 1% by weight or more when converted to w=0.
次に本発明物質の製造法について述べる。Next, a method for producing the substance of the present invention will be described.
本発明物質は、公知の方法、例えばアルミン酸ソーダま
たはアルミン酸カリの水)各法とケイ酸′ノーダまたは
ケイ酸カリの水溶液とを所定の濃度比で、カセイソーダ
水ン各法またはカモイカ1ノ水、容液中で混合し、水熱
合成することにより本発明物質の前駆体である3Aある
いは4A型ゼオライトを製造し、次いでこれらのゼオラ
イトを用し)で、以下の(1)或いは(2)等の反応を
おこなうことにより製造することができる。The substance of the present invention can be produced by a known method, for example, by mixing an aqueous solution of sodium silicate or potassium silicate in a predetermined concentration ratio of each method (for example, sodium aluminate or potassium aluminate water) and an aqueous solution of sodium silicate or potassium silicate. 3A or 4A type zeolite, which is a precursor of the substance of the present invention, is produced by mixing in water and a liquid and hydrothermally synthesized, and then using these zeolites), the following (1) or (2) is carried out. ) can be produced by conducting reactions such as
(1)カルシウム塩を使用して、3A型あるいは4A型
ゼオライトの構成成分であるカリウムイオンあるいはナ
トリウムイオンの全量あるいは一部をカルシウムイオン
に交換して得られるゼオライトと水溶性の銅塩とを水ま
たはアルコール中でイオン交換反応させる。(1) Zeolite obtained by exchanging all or part of the potassium ions or sodium ions, which are the constituent components of type 3A or type 4A zeolite, with calcium ions using a calcium salt and a water-soluble copper salt are mixed in water. Or perform an ion exchange reaction in alcohol.
(2)3A型あるいは4A型ゼオライトにカルシウム塩
および水溶性銅塩を同時に用いて、カリウムイオンある
いはナトリウムイオンをカルシウムイオンおよび銅イオ
ンに同時にイオン交換させる。(2) A calcium salt and a water-soluble copper salt are simultaneously used in 3A type or 4A type zeolite to simultaneously ion-exchange potassium ions or sodium ions into calcium ions and copper ions.
上記のイオン交換反応に用いられるカルシウム塩として
は、塩化カルシウム、臭化カルシウム、硝酸カルシウム
等の12.酸塩、ギ酸カルシウム、酢酸カルシウム等の
有機酸塩が挙げられる。水溶性銅塩としては例えば、塩
化第2i、硫酸第2銅、硝酸第2銅等の鉱酸塩、酢酸第
2銅、ギ酸第2銅等の有機酸塩またはアンモニア銅錯塩
等が挙げられるが、好ましくは、塩化第2銅、硫酸第2
銅、硝酸第2銅等の鉱酸塩等があげられる。Examples of calcium salts used in the above ion exchange reaction include calcium chloride, calcium bromide, calcium nitrate, etc. Examples include organic acid salts such as acid salts, calcium formate, and calcium acetate. Examples of water-soluble copper salts include mineral acid salts such as 2i chloride, cupric sulfate, and cupric nitrate; organic acid salts such as cupric acetate and cupric formate; and ammonia copper complex salts. , preferably cupric chloride, cupric sulfate
Examples include mineral acid salts such as copper and cupric nitrate.
本発明物質は、植物病害に対して優れた効果を発揮する
ことから、農園芸用殺菌剤の有効成分として種々の用途
に用いることができる。Since the substance of the present invention exhibits excellent effects against plant diseases, it can be used for various purposes as an active ingredient in agricultural and horticultural fungicides.
本発明物質が防除し得る植物病害としては以下のような
病害をあげることができる。Plant diseases that can be controlled by the substance of the present invention include the following diseases.
各種野菜の軟腐病(肚肚貼a carotoνora)
、ナス科の青枯病(Pseudomonas so
lanacrearum)、キュウリの斑点細菌病(P
seudomonas Iachrzmans) 。Soft rot of various vegetables (Carotoνora)
, Pseudomonas solanaceae
lanacreum), bacterial spot disease of cucumber (P
seudomonas Iachrzmans).
野菜の男斑菜菌病(Pseudomonas nU那e
」Lmaculicola) 、犀Q病(Xanth
omonas リ訓estris)、根頭がんしゅ病(
釦匹匠丼弘坊y tlmefaciens)、トマト
潰ヨウ病(如り1±軽ym捜m mlch月囲1凹y法
)イネ籾枯細菌病(Pseudomonas g)ma
e) 、タバコ野火病(Pseudomonas ta
baci) 、ミカンかいよう病(Xanthomon
as 7 pv、 ci tri ) 、イネ白葉枯病
(Xanthomonas 躾■朋) 、蔽菜類、ダイ
コン類のべと病(籾皿肚狂ora brassica
e)ホウレン草ノヘト病(A皿並肚どa」肚匣且些)、
タバコのべと病(匡匡凹狂πa tabacina)
、キュウリのベト病(超肥並匹皿皿迂二a cuben
sis) フドウのべと病(肚眩剪匹二 ν1tico
la) 、セリ科植物のべと病(7n1vea)、ツノ
7ゴ、イチゴ、ヤクヨウニンジンの疫病(PhtOht
hOracactorum)、トマトキュウリの灰色疫
病(ハ旦亜旦胚ユC並且虱)、パイナツプルの疫病(7
cinnaIIIomi ) 、ジャガイモ、トマト、
ナスの疫病C池ハ亜帖πa 1nfestans )、
タバコ、ソラマメ、ネギの疫病(ハハ匹坦匡胆n1co
tianae var、 n1cotianae)
、ホウレンソウ立枯病(h旦基m sp、) 、キュ
ウリ苗立枯病(hthiuイ並厘■佃艮旦腹)、コムギ
褐色雪腐病(Pithium 」L) 、タバコ苗立枯
病(h帥旦o+ 伽垣阜anum) 、ダイズのPyt
hium Rot (h旦旦m 亜田皿dermat
um、 ム」畦虹踵朋m、 P、 1rre ular
e、 P。Pseudomonas fungal disease of vegetables
” Lmaculicola), Rhinoceros Q disease (Xanth
omonas estris), tumefaciens disease (
Tomato canker blight (Yori 1 ± light ym search m mlch month circumference 1 indentation y method) Rice rice blight bacterial disease (Pseudomonas g) ma
e) Tobacco wildfire disease (Pseudomonas ta
baci), citrus canker disease (Xanthomon
as 7 pv, ci tri), rice leaf blight (Xanthomonas spp.), downy mildew of vegetables and radish (paddy dish ora brassica)
e) Spinach leaf blight (A dish parallel to a plate),
Tobacco mildew (conformal mildew)
, downy mildew of cucumbers
sis) Downy mildew of Fudou (dizziness)
la), downy mildew of Apiaceae plants (7n1vea), late blight of hornworts, strawberries, and ginseng (PhtOht)
h Oracactorum), gray late blight of tomato cucumber (Hadan Adan Gyoyu C parallel and lice), late blight of pineapple (7
cinnaIIIomi), potatoes, tomatoes,
Eggplant plague C pond ha acho 1nfestans),
Tobacco, fava beans, green onion epidemic (haha)
tianae var, n1cotianae)
, spinach damping-off (hdanki m sp, ), cucumber seedling damping-off (hthiuii 南厘■佾艮danburi), wheat brown snow rot (Pithium 'L), tobacco seedling damping-off (h 帥dano+ 载木阜anum), soybean Pyt
hium Rot (hdandanm ada plate dermat
um, mu” 畦 Rainbow heels tomo m, P, 1rre ular
e, P.
d+ P、 ultiman) 、イネのいもち病(7
亘a 7 、ごま葉枯病(Cochliobolus
7) 、リンゴの黒星病(νenturia釦憇並社
旦) 、腐らん病(Valsamali ) 、斑点落
葉病(Alternaria mali) 、ナシの
黒斑病(計刹rnaria kikuchiana)
、g星病(Venturia nashi並圏)、カ
ンキツの黒点病(但並虹旦e五旦■)カキの炭そ病(阻
男狙狂ガμ岬 虱)、落葉病(強胛脛工罪1.−5竺1
酉コ旦a−唆雪)・フドウの晩腐病(Glomerel
la c■紐ハ田) 、灰色かび病(肢「旦且C罰肛亜
)、葉枯病(と匹肛」tritici ) 、ふ枯病(
Le tos haeria nodorum)ウリ
類の炭そ病(Colletotrichum 7)ツ
ル枯病(取部」匝虹虹圏mel亜旦)、トマトの輪紋病
(Alternaria 5olani) 、タバコ
の赤星病(Alternaria k皿圧並) 、炭
そ病(Colletotrichum tabacum
) 、テンサイの褐斑病(7beticola) 、ジ
ャガイモの夏痩病(Alternariasolani
) 、ラッカセイの褐斑病(廁匹匹匹ユ 肛achid
icola) 、ダイズの褐紋病(と匹oria 雌
型)、黒点病(敗並π劫e−坦旦鱈旦堕セ虎)、炭そ病
(Colletotrichum sp、) 、紫斑病
(7ra kikuchii)などが挙げられる。d+P, ultimate), rice blast disease (7
Wataru a 7, Sesame leaf blight (Cochliobolus
7) Apple scab disease (νenturia kangenamishadan), rot disease (Valsamali), spot leaf fall disease (Alternaria mali), pear black spot disease (keishu rnaria kikuchiana)
, g star disease (Venturia nashi), citrus black spot disease (however, Nijitan e Godan■), oyster anthracnose disease (Kanmanai ga μ Misaki lice), defoliation disease (Stripe thorn 1) .-5 line 1
Glomerel late rot disease (Glomerel)
gray mold (limb), leaf blight (tritici), leaf blight (tritici),
Le tos haeria nodorum) anthracnose of cucurbits (Colletotrichum 7), vine blight (Toribe), tomato ring blight (Alternaria 5olani), tobacco blight (Alternaria k plate pressure) average), anthracnose (Colletotrichum tabacum)
), brown spot disease of sugar beet (7beticola), summer lean disease of potato (Alternaria solani)
), groundnut brown spot disease
icola), soybean brown spot (Colletotrichum sp.), black spot (Colletotrichum sp.), purpura (7ra kikuchii), etc. can be mentioned.
本発明物質は、畑地、水田、果樹園、茶園、牧草地、芝
生地等に農園芸用殺菌剤として用いることができ、また
他の植物病害防除剤と混合して用いることにより、殺菌
効力の増強をも期待できる。The substance of the present invention can be used as an agricultural and horticultural fungicide in fields, paddy fields, orchards, tea gardens, pastures, lawns, etc., and can be used in combination with other plant disease control agents to increase the bactericidal effect. We can also expect an increase.
さらに、殺虫側、殺ダニ剤、殺線虫剤、除草剤、植物生
長調節剤、肥料と混合して用いることもできる。Furthermore, it can be used in combination with insecticides, acaricides, nematicides, herbicides, plant growth regulators, and fertilizers.
本発明物質を殺菌剤の有効成分として用いる場合は、他
の何らの成分も加えずそのままで用いてもよいが、通常
は、固体担体、液体担体、界面活性剤その他の製剤用補
強剤と混合して、粒剤、水和剤、懸濁剤、粉剤等に製剤
して用いる。本発明物質の製剤中の含有量は0.1〜9
9.9%、好ましくは1〜99%である。When the substance of the present invention is used as an active ingredient of a disinfectant, it may be used as it is without adding any other ingredients, but it is usually mixed with a solid carrier, liquid carrier, surfactant, or other formulation reinforcing agent. Then, it is formulated into granules, wettable powders, suspensions, powders, etc. and used. The content of the substance of the present invention in the preparation is 0.1 to 9
9.9%, preferably 1-99%.
上述の固体担体としては、カオリンクレー、アッタバル
ジャイトクレー、ベントナイト、酸性白土、パイロフィ
ライト、タルク、珪藻土、方解石、トウモロコシ穂軸粉
、クルミ殻粉、尿素、硫酸アンモニウム、合成含水酸化
珪素等の微粉末あるいは粒状物が挙げられ、液体担体と
しては、水等があげられる。The solid carriers mentioned above include fine particles such as kaolin clay, attabulgite clay, bentonite, acid clay, pyrophyllite, talc, diatomaceous earth, calcite, corn cob flour, walnut shell flour, urea, ammonium sulfate, and synthetic hydrous silicon oxide. Examples of the carrier include powder or granules, and examples of the liquid carrier include water.
乳化、分散、?W展等のために用いられる界面活性剤と
しては、アルキル硫酸エステル塩、アルキル(アリール
)スルホン酸塩、ジアルキルスルホコハク酸塩、ポリオ
キシエチレンアルキルアリールエーテルリン酸エステル
塩、ナフタレンスルホン酸ホルマリン縮合物等の陰イオ
ン界面活性剤、ポリオキンエチレンアルキルエーテル、
ポリオキシエチレンポリオキンプロピレンブロノクコボ
リマー、ソルビタン脂肪酸エステル、ポリオキシエチレ
ンソルビクン脂肪酸エステル等の非イオン界面活性剤が
あげられる。製剤用補強剤としては、リグニンスルホン
酸塩、アルギン酸塩、ポリビニルアルコール、アラビア
ガム、CMC(カルボキンメチルセルロース)、PAP
(酸性リン酸イソプロピル)等があげられる。Emulsification, dispersion,? Surfactants used for W exhibition, etc. include alkyl sulfate salts, alkyl (aryl) sulfonate salts, dialkyl sulfosuccinate salts, polyoxyethylene alkylaryl ether phosphate salts, naphthalene sulfonic acid formalin condensates, etc. anionic surfactant, polyoxine ethylene alkyl ether,
Examples include nonionic surfactants such as polyoxyethylene polyquine propylene bronoquinone polymer, sorbitan fatty acid ester, and polyoxyethylene sorbicun fatty acid ester. Strengthening agents for formulations include lignin sulfonate, alginate, polyvinyl alcohol, gum arabic, CMC (carboxylic methyl cellulose), and PAP.
(acidic isopropyl phosphate), etc.
また、本発明の農園芸用殺菌剤の施用方法としては、例
えば茎葉散布、土壌処理、種子消毒等があげられるが、
通常当業者が利用するどのような施用方法にても用いる
ことができる。In addition, examples of methods for applying the agricultural and horticultural fungicide of the present invention include foliage spraying, soil treatment, seed disinfection, etc.
Any application method commonly used by those skilled in the art can be used.
本発明物質を農園芸用殺菌剤の有効成分として用いる場
合、その有効成分の施用量は、対象作物、対象病害、病
害の発生程度、製剤形態、施用方法、施用時期、気象条
件、銅の含有量等によって異なるが、通常1アールあた
り0.3〜600g、好ましくは0.3〜300gであ
り、水和剤、懸濁剤等を水で希釈して施用する場合、そ
の施用濃度は、0.015〜1.5%、好ましくは0.
03〜0.6%テアリ粉剤、粒剤等はなんら希釈するこ
となくそのまま施用する。When the substance of the present invention is used as an active ingredient of a fungicide for agriculture and horticulture, the application amount of the active ingredient depends on the target crop, target disease, degree of disease occurrence, formulation form, application method, application timing, weather conditions, copper content, etc. Although it varies depending on the amount, it is usually 0.3 to 600 g per are, preferably 0.3 to 300 g. When applying a wetting agent, suspending agent, etc. diluted with water, the application concentration is 0. .015-1.5%, preferably 0.015% to 1.5%, preferably 0.015% to 1.5%, preferably 0.
03-0.6% Teari powder, granules, etc. are applied as is without any dilution.
〈実施例〉
以下、本発明をさらに詳細に説明するが、本発明はこれ
らに限定されるものではない。<Examples> The present invention will be described in more detail below, but the present invention is not limited thereto.
まず、製剤例を示す。なお、部は重量部を表わす。First, a formulation example will be shown. Note that parts represent parts by weight.
製剤例1
本発明物質50部、リグニンスルホン酸カルシウム3部
、ラウリル硫酸ナトリウム2部および合成含水酸化珪素
45部をよく粉砕混合することにより水和剤が得られる
。Formulation Example 1 A wettable powder is obtained by thoroughly pulverizing and mixing 50 parts of the substance of the present invention, 3 parts of calcium lignosulfonate, 2 parts of sodium lauryl sulfate, and 45 parts of synthetic hydrous silicon oxide.
製剤例2
本発明物’1t95部、リグニンスルホン酸カルシウム
3部、ラウリル硫酸ナトリウム2部をよく粉砕混合する
ことにより水和剤が得られる。Formulation Example 2 A wettable powder is obtained by thoroughly pulverizing and mixing 95 parts of the present invention '1t, 3 parts of calcium lignosulfonate, and 2 parts of sodium lauryl sulfate.
製剤例3
本発明物質50部、ポリオキシエチレンソルビタンモノ
オレエート3部、CMC3部及び水44部を混合し、有
効成分の粒度が5ミクロン以下になるまで湿式粉砕する
ことにより懸濁剤が得られる。Formulation Example 3 A suspension is obtained by mixing 50 parts of the substance of the present invention, 3 parts of polyoxyethylene sorbitan monooleate, 3 parts of CMC, and 44 parts of water and wet-pulverizing the mixture until the particle size of the active ingredient becomes 5 microns or less. It will be done.
製剤例4
本発明物質5部、カオリンクレー85部およびタルク1
0部をよく粉砕混合することにより粉剤が得られる。Formulation Example 4 5 parts of the substance of the present invention, 85 parts of kaolin clay, and 1 part of talc
A powder is obtained by thoroughly grinding and mixing 0 parts.
製剤例5
本発明物!20部、合成含水酸化珪素1部、リグニンス
ルホン酸カルシウム2部、ベントナイト30部およびカ
オリンクレー47部をよく粉砕混合し、水を加えてよく
練り合わせた後、造粒乾燥することにより粒剤が得られ
る。Formulation Example 5 Inventive product! 20 parts of synthetic hydrous silicon oxide, 1 part of calcium lignin sulfonate, 30 parts of bentonite and 47 parts of kaolin clay were thoroughly ground and mixed, water was added and the mixture was thoroughly kneaded, followed by granulation and drying to obtain granules. It will be done.
次に、本発明物質が農園芸用殺衆剤として有用であるこ
とを試験例で示す。Next, test examples will show that the substance of the present invention is useful as a pesticide for agriculture and horticulture.
尚、該試験において、供試物質は、以下に示す操作によ
り調製した。In addition, in this test, the test substance was prepared by the operation shown below.
本発明物質(1)
Nato 26.3重量%、^It’343.2重量
%と1Iffi。Substance of the present invention (1) Nato 26.3% by weight, ^It'343.2% by weight and 1Iffi.
30.5重量%とを含むアルミン酸ナトリウム106.
2gとNa2O77,5重量%含む水酸化ナトリウム8
9゜67gとを蒸留水582.6gに溶解した。この溶
液をNano 9.2重量%、Sing 29.0重
量%を含むケイ酸ナトリウムの水溶液186.21gに
撹拌しながら加えた。ここで得られた物質は、
4、]Na2O・^hos ・2.05iOz 9
2.782Oで示される。30.5% by weight of sodium aluminate 106.
Sodium hydroxide 8 containing 2g and 77.5% by weight of Na2O
9.67g was dissolved in 582.6g of distilled water. This solution was added to 186.21 g of an aqueous solution of sodium silicate containing 9.2% by weight of Nano and 29.0% by weight of Sing while stirring. The substance obtained here is 4,]Na2O・^hos・2.05iOz 9
It is shown as 2.782O.
次に反応器を密閉し、室温で3時間、さらに、60℃で
3時間撹拌した。次いで析出した粉末状の結晶を減圧下
に濾集した後、該結晶をその洗液のPHが約8〜9にな
るまで蒸留水で洗浄し、120゛Cで16時間乾燥させ
た。Next, the reactor was sealed and stirred at room temperature for 3 hours and then at 60°C for 3 hours. The precipitated powder crystals were then collected by filtration under reduced pressure, washed with distilled water until the pH of the washing solution reached about 8-9, and dried at 120°C for 16 hours.
次にこの結晶10HにIN酢酸カルシウム水溶液100
dを加えた後、室温で4時間攪拌してカルシウムイオン
交換反応を行った。イオン交換反応終了後、反応液を濾
過し、得られた結晶を蒸留水でpHが7付近になるまで
洗浄後、120’Cで16時間乾燥させた。Next, to this crystal 10H, IN calcium acetate aqueous solution 100%
After adding d, the mixture was stirred at room temperature for 4 hours to perform a calcium ion exchange reaction. After the ion exchange reaction was completed, the reaction solution was filtered, and the obtained crystals were washed with distilled water until the pH reached around 7, and then dried at 120'C for 16 hours.
次にこのカルシウムイオン交換後の結晶より5gを取り
、0.04M硫酸銅水溶液118紙を加えた後、系内の
pHを10%苛性ソーダを用いて6,9に調整し、室温
で4時間攪拌して銅イオン交換反応を行った。イオン交
換反応終了後、反応液を濾過し、得られた結晶を遺留水
で硫酸根が検出されなくなるまで洗浄後、120°Cで
16時間乾燥させた。Next, take 5 g of the calcium ion-exchanged crystals, add 0.04M copper sulfate aqueous solution 118 paper, adjust the pH of the system to 6.9 using 10% caustic soda, and stir at room temperature for 4 hours. A copper ion exchange reaction was performed. After the ion exchange reaction was completed, the reaction solution was filtered, and the resulting crystals were washed with residual water until no sulfate groups were detected, and then dried at 120°C for 16 hours.
このようにして得られた粉末状の物質はX&!i!回折
法によりフォージャサイト群に属する結晶性ゼオライト
であることを確認した。また元素分析によりS i /
A l原子比は115、銅の含有量は4.3重量%、
カルシウムの含有量は、2,9重量%であり、該物質は
0.27CuO・0.29CaO・0.44Na2O・
Al2Oi ・2.30Si(h・ 5.21H20
で示される。The powdered substance thus obtained is X&! i! It was confirmed by diffraction method that it is a crystalline zeolite belonging to the faujasite group. Furthermore, elemental analysis shows that S i /
Al atomic ratio is 115, copper content is 4.3% by weight,
The content of calcium is 2.9% by weight, the substance is 0.27CuO.0.29CaO.0.44Na2O.
Al2Oi ・2.30Si(h・5.21H20
It is indicated by.
本発明物質(2)
Nano 26.3重量%、Al2O243,2重量
%とH2O30.5重量%とを含むアルミン酸ナトリウ
ム100.0gとNazo 77.5重量%含む水酸
化ナトリウム85.5gとを蒸留水580.Ogに溶解
した。この溶液をN11209.2重量%、Sing
29.0重量%を含むケイ酸ナトリウムの水溶液185
.0gに攪拌しながら加えた。Substance of the present invention (2) 100.0 g of sodium aluminate containing 26.3% by weight of Nano, 43.2% by weight of Al2O2 and 0.5% by weight of H2O and 85.5g of sodium hydroxide containing 77.5% by weight of Nazo were distilled. Water 580. Dissolved in Og. This solution was mixed with N11209.2% by weight, Sing
Aqueous solution of sodium silicate containing 29.0% by weight 185
.. 0 g with stirring.
ここで得られた物質は、
4.17Na2OHAl2Oi ・2.11SiOz
・97.5H20で示される。The substance obtained here is 4.17Na2OHAl2Oi ・2.11SiOz
- Shown as 97.5H20.
次に反応器を密閉し、室温で3時間、さらに、60″C
で3時間攪拌した。次いで析出した粉末状の結晶を減圧
下に濾集した後、該結晶をその洗液のpHが約8〜9に
なるまで蒸留水で洗浄し、120″Cで16時間乾燥さ
せた。The reactor was then sealed and kept at room temperature for 3 hours at 60″C.
The mixture was stirred for 3 hours. Then, the precipitated powder crystals were collected by filtration under reduced pressure, washed with distilled water until the pH of the washing solution became about 8-9, and dried at 120''C for 16 hours.
次にこの結晶10gにIN酢酸カルシウム水溶液100
mを加えた後、室温で4時間攪拌してカルシウムイオン
交換反応を行った。イオン交換反応終了後、反応液を濾
過し、得られた結晶を蒸留水でpHが7付近になるまで
洗浄後、120℃で16時間乾燥させた。Next, add 100 g of IN calcium acetate aqueous solution to 10 g of this crystal.
After adding m, the mixture was stirred at room temperature for 4 hours to perform a calcium ion exchange reaction. After the ion exchange reaction was completed, the reaction solution was filtered, and the obtained crystals were washed with distilled water until the pH reached around 7, and then dried at 120° C. for 16 hours.
次にこのカルシウムイオン交換後の結晶より5gを取り
、0.04M硫酸銅水溶液118dを加えた後、系内の
pHを10%苛性ソーダを用いて6.9に調整し、室温
で4時間攪拌して銅イオン交換反応を行った。イオン交
換反応終了後、反応液を濾過し、得られた結晶を蒸留水
で硫酸根が検出されなくなるまで洗浄後、120°Cで
16時間乾燥させた。Next, 5 g of this calcium ion-exchanged crystal was taken, 118 d of 0.04 M copper sulfate aqueous solution was added, and the pH of the system was adjusted to 6.9 using 10% caustic soda, and the mixture was stirred at room temperature for 4 hours. A copper ion exchange reaction was performed. After the ion exchange reaction was completed, the reaction solution was filtered, and the resulting crystals were washed with distilled water until no sulfate groups were detected, and then dried at 120°C for 16 hours.
このようにして得られた粉末状の物質はX線回折法によ
りフォージャサイト群に属する結晶性ゼオライトである
ことを確認した。また元素分析によりSi/Al原子比
は1.21、銅の含有量は12.1重量%、カルシウム
の含有量は3.1重量%であり、該物質は、
0.68Cu0 ・0.28Ca0・0.04Na2O
・Al2Os ・2.42SiO□・ 2.10H2
0で示される。The powdery substance thus obtained was confirmed by X-ray diffraction to be a crystalline zeolite belonging to the faujasite group. Further, elemental analysis revealed that the Si/Al atomic ratio was 1.21, the copper content was 12.1% by weight, and the calcium content was 3.1% by weight, and the substance was 0.68Cu0 ・0.28Ca0 ・0.04Na2O
・Al2Os ・2.42SiO□・ 2.10H2
Indicated by 0.
本発明物1t(3)
本発明物質(1)と同様の調製法でカルシウムイオン交
換前の結晶を得た。次にこの様にして得られた結晶5g
に0.073M塩化カルシウム水溶液59〆と0.29
4M硫酸銅水溶液59ateを同時に加えた後室温で4
時間撹拌してイオン交換反応を行った。イオン交換反応
終了後、反応液を濾過し、得られた結晶を蒸留水で塩素
イオン及び硫#根が検出されなくなるまで洗浄後、12
0°Cで16時間乾燥させた。このようにして得られた
粉末状の物質はX線回折法によりフォージャサイト群に
属する結晶性ゼオライトであることを確認した。また元
素分析によりSi/Al原子比は1.15、銅の含有量
は14゜4重量%、カルシウムの含有量は1.9重量%
であり、該物質は、
0.82Cu0 ・0.17Ca(l 0.01N
a2O・AI2Oz ・2.30SiO,・ 2.5
0Hzoで示される。Present invention product 1t(3) Crystals before calcium ion exchange were obtained by the same preparation method as the present invention material (1). Next, 5g of crystals obtained in this way
0.073M calcium chloride aqueous solution 59〆 and 0.29
After simultaneously adding 4M copper sulfate aqueous solution 59ate,
The mixture was stirred for hours to perform an ion exchange reaction. After the ion exchange reaction was completed, the reaction solution was filtered, and the obtained crystals were washed with distilled water until no chlorine ions and sulfur groups were detected.
Dry at 0°C for 16 hours. The powdery substance thus obtained was confirmed by X-ray diffraction to be a crystalline zeolite belonging to the faujasite group. Also, elemental analysis shows that the Si/Al atomic ratio is 1.15, the copper content is 14.4% by weight, and the calcium content is 1.9% by weight.
and the substance is 0.82Cu0 ・0.17Ca(l 0.01N
a2O・AI2Oz・2.30SiO,・2.5
It is indicated by 0Hz.
本発明物質(4)
本発明物質(1)と同様の調製法でカルシウムイオン交
換反応終了後、銅イオン交換前の結晶を得た。次にこの
様にして得られた結晶5gに0.90M塩化カルシウム
水溶液59dと0.08M硫酸銅水溶液59細を同時に
加えた後、室温で4時間攪拌してイオン交換反応を行っ
た。イオン交換反応終了後、反応液を濾過し、得られた
結晶を蒸留水で塩素イオン及び硫酸根が検出されなくな
るまで洗浄後、120″Cで16時間乾燥させた。Substance of the Present Invention (4) Crystals were obtained after completion of the calcium ion exchange reaction and before copper ion exchange using the same preparation method as for the substance of the present invention (1). Next, 59 d of a 0.90 M aqueous calcium chloride solution and 59 d of a 0.08 M aqueous copper sulfate solution were simultaneously added to 5 g of the crystals thus obtained, and the mixture was stirred at room temperature for 4 hours to carry out an ion exchange reaction. After the ion exchange reaction was completed, the reaction solution was filtered, and the resulting crystals were washed with distilled water until no chloride ions or sulfate groups were detected, and then dried at 120''C for 16 hours.
このようにして得られた粉末状の物質はX線回折法によ
りフォージャサイト群に属する結晶性ゼオライトである
ことを確認した。また元素分析によりS i /A 1
原子比は1.15、銅の含有量は4.3重量%、カルシ
ウムの含有量は8.4重量%であり、該物質は、
0.24CuO・0.75Ca(l 0.0INa2
O・Al2O3・2.30SiOz・3.04)12O
で示される。The powdery substance thus obtained was confirmed by X-ray diffraction to be a crystalline zeolite belonging to the faujasite group. In addition, elemental analysis shows that S i /A 1
The atomic ratio is 1.15, the content of copper is 4.3% by weight, the content of calcium is 8.4% by weight, and the substance is 0.24CuO・0.75Ca(l 0.0INa2
O・Al2O3・2.30SiOz・3.04)12O
It is indicated by.
本発明物質(5)
本発明物質(1)と同様の調製法でカルシうエイオン交
換前の結晶を得た。次にこの様にして得られた結晶10
gに0.076M塩化カルシウム水溶液236+dを加
えた後、室温で4時間攪拌してカルシウムイオン交換反
応を行った。イオン交換反応終了後、反応液を濾過し、
得られた結晶を蒸留水で塩素イオンが検出されなくなる
まで洗浄後、120°Cで16時間乾燥させた。Substance of the Present Invention (5) Crystals before calcium ion exchange were obtained by the same preparation method as the substance of the present invention (1). Next, crystal 10 obtained in this way
After adding 0.076M calcium chloride aqueous solution 236+d to g, the mixture was stirred at room temperature for 4 hours to perform a calcium ion exchange reaction. After the ion exchange reaction is completed, the reaction solution is filtered,
The obtained crystals were washed with distilled water until no chloride ions were detected, and then dried at 120°C for 16 hours.
次にこのカルシウムイオン交換後の結晶より5gを取り
、0.20Mg酸嗣水溶液60IIiを加えた後系内の
pHを10%苛性ソーダを用いて6.9に調整し、室温
で4時間撹拌して銅イオン交換反応を行った。イオン交
換反応終了後、反応液を濾過し、得られた結晶を寥留水
で硫酸根が検出されなくなるまで洗浄後、120°Cで
16時間乾燥させた。Next, 5 g of this calcium ion-exchanged crystal was taken, and after adding 0.20 Mg acid sulfur aqueous solution 60 IIi, the pH of the system was adjusted to 6.9 using 10% caustic soda, and the mixture was stirred at room temperature for 4 hours. A copper ion exchange reaction was performed. After the ion exchange reaction was completed, the reaction solution was filtered, and the obtained crystals were washed with distilled water until no sulfate groups were detected, and then dried at 120°C for 16 hours.
このようにして得られた粉末状の物質はX線回折法によ
りフォージャサイト群に属する結晶性ゼオライトである
ことを確認した。また元素分析によりSi/^1原子比
は1.15、銅の含有量は16.1重量%、カルシウム
の含有量は2.3重量%であり、該物質は、
0.80CuO・0.18Ca(l 0.02Na2
OA12O* ・2.3SiOz ・ 0.02H
,Oで示される。The powdery substance thus obtained was confirmed by X-ray diffraction to be a crystalline zeolite belonging to the faujasite group. Also, elemental analysis showed that the Si/^1 atomic ratio was 1.15, the copper content was 16.1% by weight, the calcium content was 2.3% by weight, and the substance was 0.80CuO・0.18Ca. (l 0.02Na2
OA12O* ・2.3SiOz ・0.02H
, O.
本発明物質(6)
本発明物質(1)と同様の調製法でカルシウムイオン交
換前の結晶を得た。次にこの様にして得られた結晶10
gに0.191M塩化カルシウム水溶液236mを加え
た後、室温で4時間攪拌してカルシウムイオン交換反応
を行った。イオン交換反応終了後、反応液を濾過し、得
られた結晶を蒸留水で塩素イオンが検出されなくなるま
で洗浄後、120°Cで16時間乾燥させた。Substance of the Present Invention (6) Crystals before calcium ion exchange were obtained by the same preparation method as the Substance of the Present Invention (1). Next, crystal 10 obtained in this way
After adding 236 ml of a 0.191M calcium chloride aqueous solution to the mixture, the mixture was stirred at room temperature for 4 hours to perform a calcium ion exchange reaction. After the ion exchange reaction was completed, the reaction solution was filtered, and the obtained crystals were washed with distilled water until no chloride ions were detected, and then dried at 120°C for 16 hours.
次にこのカルシウムイオン交換後の結晶より5gを取り
、0.20M硫酸銅水溶液60紙を加えた後系内のPH
を10%苛性ソーダを用いて6.9に調整し、室温で4
時間撹拌して銅イオン交換反応を行った。イオン交換反
応終了後、反応液を濾過し、得られた結晶を蒸留水で硫
酸根が検出されなくなるまで洗浄後、120°Cで16
時間乾燥させた。Next, take 5g of this calcium ion-exchanged crystal, add 60 pieces of 0.20M copper sulfate aqueous solution, and then adjust the pH of the system.
was adjusted to 6.9 using 10% caustic soda, and then heated to 4 at room temperature.
The mixture was stirred for hours to perform a copper ion exchange reaction. After the ion exchange reaction was completed, the reaction solution was filtered, the obtained crystals were washed with distilled water until no sulfate groups were detected, and then incubated at 120°C for 16 days.
Let dry for an hour.
このようにして得られた粉末状の物質はX線回折法によ
りフォージャサイト群に属する結晶性ゼオライトである
ことを確認した。また元素分析によりS i / A
l原子比は1.15、銅の含有量は17.0重量%、カ
ルシウムの含有量は1.4重量%であり、該物質は、
0.85CuO・ 0.11Ca(10,04Na2O
・Al2O* ・2.30SiO,・ o、osH2
0で示される。The powdery substance thus obtained was confirmed by X-ray diffraction to be a crystalline zeolite belonging to the faujasite group. In addition, elemental analysis revealed that Si/A
The l atomic ratio is 1.15, the content of copper is 17.0% by weight, the content of calcium is 1.4% by weight, and the substance is 0.85CuO・0.11Ca(10,04Na2O
・Al2O* ・2.30SiO,・o,osH2
Indicated by 0.
本発明物質(7)
本発明物質(1)と同様の調製法でカルシウムイオン交
換反応後、銅イオン交換前の結晶を得た。Substance of the Present Invention (7) Crystals were obtained after calcium ion exchange reaction and before copper ion exchange using the same preparation method as the substance of the present invention (1).
次にこの様にして得られた結晶5gに0.0033M硫
酸銅水溶液670jfを加えた後、室温で10分間撹拌
して銅イオン交換反応を行った。反応液を濾別後、回収
した結晶に再び上記の銅イオン交換反応を繰り返し行っ
た6合計5回の銅イオン交換反応終了後、反応液を濾過
し、得られた結晶を蒸留水で硫酸根が検出されなくなる
まで洗浄後、120°Cで16時間乾燥させた。Next, 670 jf of a 0.0033 M copper sulfate aqueous solution was added to 5 g of the crystals thus obtained, and the mixture was stirred at room temperature for 10 minutes to perform a copper ion exchange reaction. After the reaction solution was filtered, the above-mentioned copper ion exchange reaction was repeated again on the recovered crystals. After a total of 5 copper ion exchange reactions, the reaction solution was filtered, and the obtained crystals were treated with distilled water to remove sulfuric acid. After washing until no longer detected, it was dried at 120°C for 16 hours.
このようにして得られた粉末状の物質はX線回折法によ
り結晶化度が50%のフォージャサイト群に属する結晶
性ゼオライトであることを確認した。また元素分析によ
りSi/At原子比は1.15、銅の含有量は6.3!
量%、カルシウムの含有量は6.1重量%であり、該物
質は、
0.35CuO・0.54CaO・0.11Na20
’A1403 ’2.30SiO□・ 2.75)1
.0で示される。The thus obtained powdery substance was confirmed by X-ray diffraction to be a crystalline zeolite belonging to the faujasite group with a crystallinity of 50%. Also, according to elemental analysis, the Si/At atomic ratio is 1.15 and the copper content is 6.3!
%, the content of calcium is 6.1% by weight, and the substance is 0.35CuO・0.54CaO・0.11Na20
'A1403'2.30SiO□・2.75)1
.. Indicated by 0.
比較物1t(a)
本発明物質(1)と同様の調製法でカルシうムイオン交
換前の結晶を得た。次にこの結晶5gに0、16M硝酸
銅水溶液60−を加えた後、系内のpHを10%苛性ソ
ーダを用いて6.9に調整し、室温で4時間攪拌してイ
オン交換反応を行った。イオン交換反応終了後、反応液
を濾過し、得られた結晶を蒸留水で銅イオンおよび硝酸
根が検出されなくなるまで洗浄後、120°Cで16時
間乾燥させた。Comparative substance 1t(a) Crystals before calcium ion exchange were obtained by the same preparation method as the substance (1) of the present invention. Next, 60 - of a 0.16 M copper nitrate aqueous solution was added to 5 g of this crystal, and the pH of the system was adjusted to 6.9 using 10% caustic soda, and the mixture was stirred at room temperature for 4 hours to perform an ion exchange reaction. . After the ion exchange reaction was completed, the reaction solution was filtered, and the resulting crystals were washed with distilled water until copper ions and nitrate groups were no longer detected, and then dried at 120°C for 16 hours.
このようにして得られた粉末状の物質はX線回折法によ
りフォージャサイト群に属する結晶性ゼオライトである
ことを確認した。また元素分析によりS i / A
l原子比はJ、15、銅の含有量は10重量%であり、
該物質は、
0.63Cu0 ・ 0.37Na20 ・Al2
O3’ 2.30SiOz ・4.91H1Oで示
される。The powdery substance thus obtained was confirmed by X-ray diffraction to be a crystalline zeolite belonging to the faujasite group. In addition, elemental analysis revealed that Si/A
The l atomic ratio is J, 15, the copper content is 10% by weight,
The substance is 0.63Cu0 ・0.37Na20 ・Al2
O3' 2.30SiOz 4.91H1O.
下記試験例において防除効力は、調査時の供試植物の発
病状態すなわち葉、茎等の菌叢、病斑の程度を肉眼観察
し、菌叢、病斑が全く認められなければr5J、10%
程度認められれば「4」、30%程度認められれば「3
」、50%程度認められれば「2」、70%程度認めら
れれば「1」、それ以上で化合物を供試していない場合
の発病状態と差が認められなければ「O」として、6段
階に評価し、それぞれ5. 4. 3. 2. 1.
Oで示す。In the following test example, the control efficacy is determined by visually observing the diseased state of the test plant at the time of investigation, that is, the degree of bacterial flora and lesions on leaves, stems, etc., and if no bacterial flora or lesions are observed, r5J, 10%.
If it is recognized to a certain extent, it will be ``4'', and if it is recognized to be around 30%, it will be ``3''.
", if it is observed in about 50%, it is "2", if it is observed in about 70%, it is "1", and if there is no difference from the disease onset state when no compound is tested, it is "O", and it is graded into 6 stages. Evaluate each 5. 4. 3. 2. 1.
Indicated by O.
試験例1
キュウリベと病防除効果(予防効果)
プラスチックボットに砂壌土を詰め、キュウリを播種し
、温室内で20日間育成した。第2本葉が展開したキュ
ウリの幼苗に、製剤例1に準して水和剤にした供試薬剤
を水で希釈して所定濃度にし、それを葉面に充分付着す
るように茎葉散布した。散布後、キュウリベと病菌の胞
子懸濁液を噴霧、接種した。接種後、20°C1多湿下
で1日覆いた後、さらに照明下で5日間生育し、防除効
力を調査した。その結果を第1表に示す。Test Example 1 Cucumber and disease control effect (preventive effect) A plastic bottle was filled with sandy loam, and cucumbers were sown and grown in a greenhouse for 20 days. A test drug prepared as a hydrating powder according to Formulation Example 1 was diluted with water to a specified concentration on cucumber seedlings that had developed their second true leaves, and was sprayed on the foliage so that it adhered sufficiently to the leaf surface. . After spraying, a spore suspension of cucumber and disease bacteria was sprayed and inoculated. After inoculation, the plants were covered for 1 day at 20°C and humid, and then grown for 5 days under light to investigate the pesticidal efficacy. The results are shown in Table 1.
試験例2
トマト疫病防除試験(予防効果)
プラスチックボットに砂壌土を詰め、トマト(ポンチロ
ーザ)を播種し、温室内で20日間育成した。第2〜3
本葉が展開したトマトの幼苗に、製剤例1に準じて水和
剤にした供試薬剤を水で希釈して所定濃度にし、それを
葉面に充分付着するように茎葉散布した。散布後、トマ
ト疫病菌の胞子懸濁液を噴霧、接種した。接種後、20
°C1多湿下で1日覆いた後、さらに照明下で5日間生
育し、防除効力を調査した。その結果を第2表に示す。Test Example 2 Tomato Phytophthora control test (preventive effect) A plastic bottle was filled with sandy loam, tomatoes (ponchirosa) were sown, and grown in a greenhouse for 20 days. 2nd to 3rd
A test chemical prepared as a hydrating powder according to Formulation Example 1 was diluted with water to a predetermined concentration and sprayed on the foliage of tomato seedlings with developed true leaves so as to sufficiently adhere to the leaf surface. After spraying, a spore suspension of Phytophthora tomato was sprayed and inoculated. After vaccination, 20
After covering for 1 day under high humidity at 1°C, the plants were grown under lighting for 5 days to investigate the pesticidal efficacy. The results are shown in Table 2.
試験例3
ダイコン黒すす病防除試験(予防効果)プラスチックボ
ットに砂壌土を詰め、ダイコン(60日ダイコン)を播
種し、温室内で6日間育成した。子葉が展開したダイコ
ンの幼苗に、製剤例1に準して水和剤にした供試薬剤を
水で希釈して所定濃度にし、それを葉面に充分付着する
ように茎葉散布した。散布後、ダイコンくるすす病菌の
胞子懸濁液を噴霧、接種した。接種後、18°C1多湿
下で1B1いた後、さらに照明下で3日間生育し、防除
効力を調査した。その結果を第3表に示す。Test Example 3 Japanese radish soot disease control test (preventive effect) A plastic bot was filled with sandy loam, and radish (60-day radish) was sown and grown in a greenhouse for 6 days. A test drug prepared as a hydrating powder according to Formulation Example 1 was diluted with water to a predetermined concentration, and the solution was sprayed onto radish seedlings with developed cotyledons so as to sufficiently adhere to the leaf surface. After the spraying, a spore suspension of the radish rust fungus was sprayed and inoculated. After inoculation, the plants were grown under 1B1 at 18° C. under high humidity, and then grown under lighting for 3 days to investigate the control efficacy. The results are shown in Table 3.
第
表
試験例4
キュウリ斑点細菌病防除試験(残存効果試験)プラスチ
ックボットに砂壌土を詰め、キュウリ(相接半白)を播
種し、温室内で35日間育成した。その後、製剤例1に
準じて水和剤にした供試薬剤を水で希釈して所定濃度に
し、それを葉面に充分付着するように茎葉散布した。散
布後、7日間温室内(昼間20°C1夜間17°C)で
栽培した後、キュウリ斑点細菌病菌の胞子懸濁液を噴霧
接種した。接種後、多湿下で約24時装置いた後、さら
に上記の温室条件下で10日間生育した。その後、接種
葉ごとに病斑の進展に従い防除効果を算出した。その結
果を第4表に示す。Table 1 Test Example 4 Cucumber Spot Bacterial Disease Control Test (Residual Effect Test) A plastic bot was filled with sandy loam, and cucumbers (joint half white) were sown and grown in a greenhouse for 35 days. Thereafter, the test drug prepared as a wettable powder according to Formulation Example 1 was diluted with water to a predetermined concentration, and the solution was sprayed on the leaves so as to sufficiently adhere to the leaf surface. After spraying, the plants were cultivated in a greenhouse for 7 days (20° C. during the day and 17° C. at night) and then inoculated with a spore suspension of cucumber spot bacterium. After inoculation, the plants were kept in a humid environment for about 24 hours and then grown for another 10 days under the above greenhouse conditions. Thereafter, the control effect was calculated according to the development of lesions on each inoculated leaf. The results are shown in Table 4.
第
表
試験例5
イネ籾枯病防除試験(予防効果)
プラスチックボットに砂壌土を詰め、イネ(近畿33号
)を播種し、温室内で70日間育成した。Test Example 5 in Table 5 Rice blight control test (preventive effect) A plastic bot was filled with sandy loam, and rice (Kinki No. 33) was sown and grown in a greenhouse for 70 days.
イネ苗に、製剤例2に準して水和剤にした供試薬剤を水
で希釈して所定濃度にし、それを穂に充分付着するよう
に散布した。散布後、植物を風乾しイネ籾枯病の胞子懸
濁液を噴霧、接種した。接種後、23°C1暗黒、多湿
下で1日間室いた後、27°C温室条件下で9日間発病
させて防除効力を調査した。その結果を第5表に示す。A test chemical prepared as a wettable powder according to Formulation Example 2 was diluted with water to a predetermined concentration, and was sprayed onto rice seedlings so that it would sufficiently adhere to the ears. After spraying, the plants were air-dried and then sprayed with a spore suspension of rice blight and inoculated. After inoculation, the plants were kept in a dark and humid room at 23°C for 1 day, and then allowed to develop for 9 days under greenhouse conditions at 27°C to investigate the control efficacy. The results are shown in Table 5.
第 5 表
るとの大きな利点を有する。また、ある種のゼオライト
(例えば特公平1−156905号公報に記載のゼオラ
イト)に比べ、安価であり、経済的に有利である。Table 5 has great advantages. Furthermore, it is cheaper and economically advantageous than certain zeolites (for example, the zeolite described in Japanese Patent Publication No. 1-156905).
〈発明の効果〉<Effect of the invention>
Claims (1)
晶性ゼオライトを有効成分として含有することを特徴と
する農園芸用殺菌剤。 xCuO・yCaO・(1−x−y)M_2O・Al_
2O_3・_zSiO_2・wH_2O〔式中、Mはナ
トリウム原子またはカリウム原子を表わし、x、y、z
およびwは各々下記範囲の数値を表わす。 0<x<1、0<y<1但しx+y≦1 2≦z≦2.5、0≦w≦20〕[Scope of Claims] An agricultural and horticultural fungicide characterized by containing crystalline zeolite belonging to the faujasite group, represented by the following general formula, as an active ingredient. xCuO・yCaO・(1-x-y)M_2O・Al_
2O_3・_zSiO_2・wH_2O [In the formula, M represents a sodium atom or a potassium atom, x, y, z
and w each represent a numerical value within the following range. 0<x<1, 0<y<1 but x+y≦1 2≦z≦2.5, 0≦w≦20]
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP11242590A JPH049308A (en) | 1990-04-27 | 1990-04-27 | Germicide composition for agriculture and horticulture |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP11242590A JPH049308A (en) | 1990-04-27 | 1990-04-27 | Germicide composition for agriculture and horticulture |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH049308A true JPH049308A (en) | 1992-01-14 |
Family
ID=14586321
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP11242590A Pending JPH049308A (en) | 1990-04-27 | 1990-04-27 | Germicide composition for agriculture and horticulture |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH049308A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
RU2724665C1 (en) * | 2019-05-20 | 2020-06-25 | Федеральное государственное бюджетное научное учреждение "Всероссийский научно-исследовательский институт защиты растений" | Natural insecticide and method for potato pests control based thereon |
-
1990
- 1990-04-27 JP JP11242590A patent/JPH049308A/en active Pending
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
RU2724665C1 (en) * | 2019-05-20 | 2020-06-25 | Федеральное государственное бюджетное научное учреждение "Всероссийский научно-исследовательский институт защиты растений" | Natural insecticide and method for potato pests control based thereon |
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