JPH0427171B2 - - Google Patents

Info

Publication number
JPH0427171B2
JPH0427171B2 JP58064298A JP6429883A JPH0427171B2 JP H0427171 B2 JPH0427171 B2 JP H0427171B2 JP 58064298 A JP58064298 A JP 58064298A JP 6429883 A JP6429883 A JP 6429883A JP H0427171 B2 JPH0427171 B2 JP H0427171B2
Authority
JP
Japan
Prior art keywords
solution
active substance
present
crystals
aqueous solution
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.)
Expired - Lifetime
Application number
JP58064298A
Other languages
Japanese (ja)
Other versions
JPS59190226A (en
Inventor
Shoji Yamashita
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
AI BII II JUGEN
Original Assignee
AI BII II JUGEN
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by AI BII II JUGEN filed Critical AI BII II JUGEN
Priority to JP58064298A priority Critical patent/JPS59190226A/en
Publication of JPS59190226A publication Critical patent/JPS59190226A/en
Priority to JP1270700A priority patent/JPH0761875B2/en
Publication of JPH0427171B2 publication Critical patent/JPH0427171B2/ja
Granted legal-status Critical Current

Links

Landscapes

  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Cultivation Of Plants (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
  • Compounds Of Iron (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

【発明の詳細な説明】 本発明は活性作用を有する物質の製造方法に関
するものである。 本発明により得られる上記活性物質は金属防蝕
抑制作用、塩障害除去作用、土壌障害除去作用に
加えて防腐作用等を有するものである。 本発明により得られる活性物質は二価鉄と三価
鉄との中間の性質を示す鉄の塩酸塩であると思わ
れ、塩化第二鉄を多量のカセイソーダ、水酸化カ
リウム、水酸化リチウム、水酸化カルシウム等の
強アルカリの水溶液に投入した場合に得られるも
のである。。以下に本発明の活性物質の製造方法
の具体例を示す。 1.0mgの塩化第二鉄(FeCl3・6H2O)を100ml
の0.5Nカセイソーダ水溶液中に投入し攪拌溶解
した後一夜静置する。生じた不溶性物質を別し
液を塩酸で中和した後減圧濃縮してデシケータ
ー中で乾燥結晶化する。かくして塩化ナトリウム
に担持された本発明の活性物質が得られるが、該
担持物から本発明の活性物質を分離するには更に
50mlのイソプロピルアルコール80%水溶液を加え
て再溶解し、減圧濃縮し溶媒を除去、乾燥させ
る。上記再溶解−濃縮−乾燥操作を数回繰返すこ
とによつて0.25mgの結晶が得られる。 得られた結晶の5重量%水溶液を作成し、その
0.01mlをペーパークロマトグラフ用紙No.51A
(2cm×40cm)の下端から3cm内側の個所にスポ
ツトし、n−ブタノール:酢酸:水=5:1:4
容量比混合物を展開溶媒として20℃、15時間の上
方展開を行う。展開後紙を乾燥させてから1重
量%フエリシアン化カリウム水溶液を発色試薬と
して紙に噴霧発色させると該結晶の展開位置は
1スポツトでRf=0.07であることが確認された。 次いで同様のペーパークロマトグラフテストを
塩化第一鉄および塩化第二鉄の1:1当量混合物
について行つた所、展開の結果は2スポツトとな
りRf=0.095(FeCl2)と、Rf=0.36(FeCl3)であ
ることが確認された。 上記ペーパークロマトグラフテストにより該結
晶は塩化第一鉄と塩化第二鉄の中間の性質を示
し、混合物ではなく単一化合物であることが推定
される。 次いで該結晶の0.1gを蒸溜水に溶かして100ml
とし可検液を作成する。その2.5mlを50ml容メス
フラスコにとり、0.1重量%オルソフエナントロ
リン水溶液2.5ml、および酢酸ナトリウム−酢酸
緩衝液(PH4.5)2.5mlを加え、蒸溜水で標線まで
充たす。30分間室温に静置した後510nmで吸光度
を測定する。塩化第一鉄水溶液について同様の方
法で得た標準曲線から可検液の二価鉄を求めると
0.019g/100mlであつた。 次いで上記操作においてメスフラスコに価検液
を添加した際、予かじめ10重量%ヒドロキシルア
ミン塩酸塩水溶液1.0mlを添加して三価鉄を二価
鉄に還元する。この場合に得られた二価鉄量は
0.038g/100mlであつた。したがつて三価鉄量は
0.038g/100ml−0.019g/100ml=0.019g/100mlと
なり、該結晶中には二価鉄と三価鉄とが当量含ま
れていることが示唆される。 本発明の活性物質は例えば塩化ナトリウム、硫
酸ナトリウム、塩化アンモニウム、硫酸アンモニ
ウム、珪藻土、ベントナイト、シリカ、アルミナ
等の無機化合物、ビタミン、ホルモン、蛋白質、
脂質等の有機化合物に担持されてもよく、その場
合においても活性物質の作用は変化することがな
い。 以下に本発明の使用例を示す。 使用例1 (金属の防蝕) 本使用例は本発明にかかる活性物質の防蝕作用
を示すものである。金属の腐蝕は金属表面で同種
の金属間または異種金属間に腐蝕電流が生ずるこ
とによつて起る。従つて金属を本発明にかかる活
性物質を含む溶液で表面処理をすることによつて
防蝕をはかることができる。 0.2cm×5cm×5cmの鉄片を予かじめ稀塩酸お
よび蒸溜水で洗浄・乾燥させた後、本発明の活性
物質(2.5×10-5/ml)、弗化水素酸(1.2×10-4
g/ml)およびグルコース(10-3g/ml)の混合
溶液200ml中に入れ、80℃で30分間処理した。 処理した鉄片をHCl気流中で腐蝕試験を行つた
ところ、無処理の鉄片は1時間後に既に顕著な腐
蝕をみたが、処理鉄片は6日間の腐蝕試験によつ
ても腐蝕をみなかつた。 使用例2 (塩障害の除去) 本紙用例は本発明の活性物質の塩障害除去作用
を示すものである。電解質溶液とくに海水は含有
する金属イオンのために船舶や海上・沿岸産業に
多大の障害をもたらしている。本発明の活性物質
の適用によつてこれらの障害を除去することがで
きる。 天然海水に10-12g/mlになるように本発明の
活性物質を加え、これに鉄粉、マンガン粉、銅粉
を添加し静置したところ、無処理海水では1日以
内にすべて塩化物を生じたが、処理海水では1年
以上変化が起らなかつた。 使用例3 (連作障害土壌の改質) 本使用例は本発明の活性物質の連作障害土壌の
改質作用を示すものである。同一作物を連作して
いくと作物によつては土壌中に病原菌の繁殖が烈
しく起り殆んど収穫不能に陥ることがある。その
根本原因は土壌中に集積する無機、有機物質のイ
オン反応によるものである。したがつて本発明の
活性物質の導入によつてこれらの障害を除去する
ことができる。 大根栽培地(岐阜県下)で起つたフザリウムの
繁殖を伴つた強度の連作障害土壌にNaClを担体
とした本発明の活性物質を10-12g/mlになるよ
うに水で希釈し、その希釈液を土が潤る程度に与
え、常法通り大根を作付した。その結果、処理土
壌の作物はすべて健全に生育し、対照区の収量
100に対し、240の収量指数が得られた。 使用例4 (防腐、防黴作用) 本使用例は本発明の活性物質の防腐、防黴作用
を示すものである。 本発明の活性物質を塩化マグネシウムを担体と
して合成し、塩化マグネシウム濃度10-6g/mlの
溶液を作り処理液とした。 予かじめアサリおよび餅片を開放系で32℃に3
日間静置し、微生物を繁殖させた。生じた微生物
を上記処理液10mlを入れた試験管中に澱粉および
ペプトン各0.5gと共に入れ、32℃に5日間静置し
た。生じた懸濁液0.1mlを100mlの水に添加し、こ
の液を新鮮なアサリおよび餅に灌水し、密封して
常温に保存した。対照区は何れも腐敗およびカビ
の発生をみたが、処理検体では3週以上微生物の
増殖が起らなかつた。 使用例5 (ウイルス感染阻止効果) 本使用例は本発明の活性物質のウイルス感染阻
止効果を示すものである。 本発明の活性物質によつて維持されている生体
システムに対して外部からこれに変更を加える物
質または要因が侵入した場合、ここに生体機能の
低下が起こりいわゆる病変となつて現われる。ウ
イルス感染障害は外部から該酸が持込まれ生体シ
ステムが破壊されることによつて生ずるものであ
る。従つて本発明の活性物質を効果的に導入する
ことによつて感染障害を除去することができる。 予かじめトマトを宿主植物としてトマト葉に
TMV(タバコモザイクウイルス)を摂取、生体
増殖させた後、試験直前に上記トマト葉より汁液
を採取、該汁液を水で500倍に希釈して試験用
TMV懸濁液とした。 本発明の活性物質の2.9×10-4g/ml水溶液に
安定剤としてMgCl2−6H2Oを1%になるように
添加して活性物質溶液を調整した。 約1ケ月後栽培したタバコ植物葉にカーボラン
ダムを塗布したのち、試験区として該タバコ植物
葉の半部に上記TMV懸濁液を上記活性物質溶液
で2倍に希釈した液を綿に浸して塗布し、対称区
として上記TMV懸濁液を水で2倍に希釈した液
を同一葉の他の半部に同様に塗布した。塗布後葉
が乾いたところで(約30分後)残余のカーボラン
ダムを水洗して、26℃に調節した培養室中で植物
を培養した。 培養3日後に試験区および対称区の葉(夫々N
=3とする)に生じた斑点の数および活性物質溶
液の阻止率を求めた結果は1表に示す通りであつ
た。 【表】
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a process for producing substances with active action. The above-mentioned active substance obtained by the present invention has anticorrosive action, metal corrosion inhibiting action, salt damage removing action, soil damage removing action, and antiseptic action. The active substance obtained by the present invention is considered to be an iron hydrochloride having properties intermediate between divalent iron and trivalent iron, and ferric chloride is mixed with a large amount of caustic soda, potassium hydroxide, lithium hydroxide, and water. It is obtained when added to a strong alkali aqueous solution such as calcium oxide. . Specific examples of the method for producing the active substance of the present invention are shown below. 100ml of 1.0mg ferric chloride (FeCl 3 6H 2 O)
Pour into 0.5N caustic soda aqueous solution and stir to dissolve, then leave to stand overnight. The resulting insoluble substances are separated, the liquid is neutralized with hydrochloric acid, concentrated under reduced pressure, and dried and crystallized in a desiccator. In this way, the active substance of the present invention supported on sodium chloride is obtained, but in order to separate the active substance of the present invention from the support, further steps are required.
Add 50 ml of isopropyl alcohol 80% aqueous solution to redissolve, concentrate under reduced pressure to remove the solvent, and dry. By repeating the above redissolution-concentration-drying operation several times, 0.25 mg of crystals is obtained. A 5% by weight aqueous solution of the obtained crystals was prepared, and the
0.01ml on paper chromatography paper No.51A
(2cm x 40cm) Spot 3cm inside from the bottom edge, n-butanol:acetic acid:water = 5:1:4
Upward development is performed at 20°C for 15 hours using the volume ratio mixture as a developing solvent. After development, the paper was dried and then a 1% by weight potassium ferricyanide aqueous solution was sprayed onto the paper as a coloring reagent to develop color, and it was confirmed that the crystal development position was 1 spot and Rf = 0.07. A similar paper chromatography test was then performed on a 1:1 equivalent mixture of ferrous chloride and ferric chloride, and the developed results were two spots: Rf = 0.095 (FeCl 2 ) and Rf = 0.36 (FeCl 3 ) . ) was confirmed. According to the paper chromatography test described above, the crystals exhibited properties intermediate between those of ferrous chloride and ferric chloride, and are presumed to be a single compound rather than a mixture. Next, dissolve 0.1g of the crystals in distilled water and add 100ml.
Prepare a testable solution. Transfer 2.5 ml of the flask to a 50 ml volumetric flask, add 2.5 ml of 0.1% by weight aqueous orthophenanthroline solution and 2.5 ml of sodium acetate-acetate buffer (PH4.5), and fill to the mark with distilled water. After standing at room temperature for 30 minutes, measure the absorbance at 510 nm. Determining the divalent iron of the testable solution from the standard curve obtained in the same manner for the ferrous chloride aqueous solution,
It was 0.019g/100ml. Next, in the above operation, when adding the valence test solution to the volumetric flask, 1.0 ml of a 10% by weight hydroxylamine hydrochloride aqueous solution is added in advance to reduce trivalent iron to divalent iron. The amount of divalent iron obtained in this case is
It was 0.038g/100ml. Therefore, the amount of trivalent iron is
0.038g/100ml−0.019g/100ml=0.019g/100ml, which suggests that the crystals contain equivalent amounts of divalent iron and trivalent iron. The active substances of the present invention include, for example, inorganic compounds such as sodium chloride, sodium sulfate, ammonium chloride, ammonium sulfate, diatomaceous earth, bentonite, silica, alumina, vitamins, hormones, proteins,
It may also be supported on organic compounds such as lipids, and the action of the active substance will not change even in that case. Examples of use of the present invention are shown below. Use example 1 (corrosion protection of metal) This use example shows the corrosion protection effect of the active substance according to the present invention. Corrosion of metals occurs due to the generation of corrosion current between the same type of metals or between different types of metals on the metal surface. Therefore, corrosion protection can be achieved by surface treating metals with a solution containing the active substance according to the present invention. After washing and drying a 0.2 cm x 5 cm x 5 cm iron piece with dilute hydrochloric acid and distilled water in advance, the active substance of the present invention (2.5 x 10 -5 /ml) and hydrofluoric acid (1.2 x 10 -4
g/ml) and glucose (10 -3 g/ml) and treated at 80°C for 30 minutes. When the treated iron piece was subjected to a corrosion test in an HCl air stream, the untreated iron piece already showed significant corrosion after one hour, but the treated iron piece showed no corrosion even after a 6-day corrosion test. Use Example 2 (Removal of salt damage) This paper example shows the action of the active substance of the present invention in removing salt damage. Electrolyte solutions, especially seawater, pose a great problem to ships and marine/coastal industries due to the metal ions they contain. By applying the active substances according to the invention these obstacles can be eliminated. When the active substance of the present invention was added to natural seawater at a concentration of 10 -12 g/ml, iron powder, manganese powder, and copper powder were added and left to stand, all chloride was removed from untreated seawater within one day. However, no change occurred in the treated seawater for over a year. Use Example 3 (Amending soil with continuous cropping problems) This use example shows the effect of the active substance of the present invention on improving soil with continuous cropping problems. If the same crop is continuously cultivated, depending on the crop, pathogenic bacteria may proliferate in the soil, making it almost impossible to harvest. The root cause is ionic reactions between inorganic and organic substances that accumulate in the soil. These obstacles can therefore be eliminated by the introduction of the active substances according to the invention. The active substance of the present invention containing NaCl as a carrier was diluted with water to a concentration of 10 -12 g/ml in soil with severe continuous cropping damage accompanied by the proliferation of Fusarium that occurred in a radish cultivation area (Gifu Prefecture). The liquid was applied to the soil to moisten it, and daikon radish was planted as usual. As a result, all the crops grown in the treated soil grew healthy and the yield in the control plot was
A yield index of 240 was obtained compared to 100. Use Example 4 (Preservative and anti-mold effect) This use example shows the preservative and anti-mold effect of the active substance of the present invention. The active substance of the present invention was synthesized using magnesium chloride as a carrier, and a solution with a magnesium chloride concentration of 10 -6 g/ml was prepared and used as a treatment solution. Heat the clams and mochi pieces in advance to 32℃ in an open system.
It was left standing for several days to allow microorganisms to grow. The resulting microorganisms were placed in a test tube containing 10 ml of the above treatment solution along with 0.5 g each of starch and peptone, and allowed to stand at 32°C for 5 days. 0.1 ml of the resulting suspension was added to 100 ml of water, and this liquid was irrigated over fresh clams and rice cakes, sealed and stored at room temperature. The control plots all showed rot and mold growth, but no microbial growth occurred for more than 3 weeks in the treated samples. Use Example 5 (Viral infection inhibiting effect) This use example shows the virus infection inhibiting effect of the active substance of the present invention. When a substance or factor that alters the biological system maintained by the active substance of the present invention invades from outside, the biological function deteriorates and appears as a so-called lesion. Viral infection disorders occur when the acid is brought in from the outside and destroys biological systems. Therefore, by effectively introducing the active substances of the present invention, infectious disorders can be eliminated. Tomato leaves are grown as host plants in advance.
After ingesting TMV (Tobacco Mosaic Virus) and growing it biologically, the juice was collected from the above tomato leaves immediately before the test, and the juice was diluted 500 times with water for testing.
It was made into a TMV suspension. An active substance solution was prepared by adding MgCl 2 -6H 2 O as a stabilizer to a 2.9×10 −4 g/ml aqueous solution of the active substance of the present invention to a concentration of 1%. After about 1 month, carborundum was applied to the leaves of the cultivated tobacco plants, and half of the leaves of the tobacco plants were soaked with cotton soaked with a 2-fold dilution of the TMV suspension with the active substance solution as a test plot. Then, as a control area, a solution prepared by diluting the above TMV suspension twice with water was similarly applied to the other half of the same leaf. After the leaves dried after application (approximately 30 minutes later), the remaining carborundum was washed with water, and the plants were cultured in a culture chamber adjusted to 26°C. After 3 days of culture, leaves of test plot and control plot (N
Table 1 shows the results of determining the number of spots that appeared (=3) and the inhibition rate of the active substance solution. 【table】

Claims (1)

【特許請求の範囲】 1 FeCl3を多量の強アルカリの水溶液に投入し
溶解させ所定時間放置する工程1 該溶液を静置し生じた不溶性物質を除去する工
程2 不溶性物質を除去した該溶液を塩酸で中和する
工程3 中和した該溶液を濃縮して結晶を得る工程4 該結晶をアルコール水混合溶媒に再溶解し、再
溶解液を濃縮して結晶を得る工程5 以上の工程1,2,3,4,5からなる活性物
質の製造方法。
[Claims] 1. Step of dissolving FeCl 3 in a large amount of strong alkali aqueous solution and leaving it for a predetermined time. Step 2. Step of leaving the solution still and removing the resulting insoluble substances. 2. Process of removing the insoluble substances from the solution. Step 3 of neutralizing with hydrochloric acid Step 4 of concentrating the neutralized solution to obtain crystals Step 5 of re-dissolving the crystals in an alcohol-water mixed solvent and concentrating the re-dissolved solution Step 5 of the above steps 1, Method for producing active substances consisting of 2, 3, 4, 5.
JP58064298A 1983-04-11 1983-04-11 Bivalent and trivalent iron salt and their preparation Granted JPS59190226A (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP58064298A JPS59190226A (en) 1983-04-11 1983-04-11 Bivalent and trivalent iron salt and their preparation
JP1270700A JPH0761875B2 (en) 1983-04-11 1989-10-17 Method for producing active substance

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP58064298A JPS59190226A (en) 1983-04-11 1983-04-11 Bivalent and trivalent iron salt and their preparation

Related Child Applications (1)

Application Number Title Priority Date Filing Date
JP1270700A Division JPH0761875B2 (en) 1983-04-11 1989-10-17 Method for producing active substance

Publications (2)

Publication Number Publication Date
JPS59190226A JPS59190226A (en) 1984-10-29
JPH0427171B2 true JPH0427171B2 (en) 1992-05-11

Family

ID=13254197

Family Applications (1)

Application Number Title Priority Date Filing Date
JP58064298A Granted JPS59190226A (en) 1983-04-11 1983-04-11 Bivalent and trivalent iron salt and their preparation

Country Status (1)

Country Link
JP (1) JPS59190226A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11744854B2 (en) 2019-11-19 2023-09-05 Yoshimasa Kijima Composition comprising natural extracts and an iron salt

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61247317A (en) * 1985-04-22 1986-11-04 日本植生株式会社 Soil for conditioning soil
JPS6354936A (en) * 1986-08-25 1988-03-09 Masami Oe Activated material
JPH01311007A (en) * 1988-06-08 1989-12-15 I B Ii:Kk Method for treating plant
JPH02113093A (en) * 1988-10-20 1990-04-25 Shizen:Kk Oil treating agent for food
JPH02167879A (en) * 1988-12-20 1990-06-28 Shizen:Kk Divalent-trivalent multiple iron salt formula fertilizer
JPH02208398A (en) * 1989-02-09 1990-08-17 Shizen:Kk Material for treating perfume
EP0541796B1 (en) * 1990-05-22 1994-07-27 I.B.E. Co., Ltd. Ferrous salt composition
JPH0454101A (en) * 1990-06-25 1992-02-21 Tetsuo Takano Preservation of kidney for implantation and preserving device of same kidney
AU1669395A (en) * 1994-02-17 1995-09-04 Merck Patent Gmbh Antiviral or antifungal composition and method
DE4421159C1 (en) * 1994-06-20 1995-08-24 Thomas Bruns Use of ferric oxide for treating immune deficiency
EP0896792A1 (en) * 1997-08-13 1999-02-17 Julphar Pharma GmbH Antiviral agent
TW541286B (en) * 1999-12-26 2003-07-11 Inst State Physics Of Natural Novel aqueous composition and use of the same
JP2002080376A (en) 2000-06-06 2002-03-19 Ibe:Kk Biologically active agent and medicine

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ENCYCLOPEDIA OF CHEMICAL REACTIONS=1951 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11744854B2 (en) 2019-11-19 2023-09-05 Yoshimasa Kijima Composition comprising natural extracts and an iron salt

Also Published As

Publication number Publication date
JPS59190226A (en) 1984-10-29

Similar Documents

Publication Publication Date Title
JPH0427171B2 (en)
SU1380618A3 (en) Method of producing salt of 2-(2-hydroxyethoxy)ethylamine and 3,6-dichloro-2-methoxybenzoic acid
JPH0363593B2 (en)
JP2009249364A (en) Soil-borne disease controlling agent for oryza sativa
Taylor et al. Seed treatment for the control of halo‐blight of beans (Pseudomonas phaseolicola)
SU708978A3 (en) Fungicidic-bactericidic agent
CN110187096B (en) Sucrose-containing biological product stabilizer for ELISA kit and preparation method thereof
US20090118124A1 (en) Novel aqueous composition and use of the same
RU2056084C1 (en) Method of presawing seed preparing
JPH08283104A (en) Agent for stimulating physiological activity of plant
JPH0761875B2 (en) Method for producing active substance
CN117063933B (en) Kasugamycin organic acid salt, pesticide composition containing kasugamycin organic acid salt and application of kasugamycin organic acid salt
JPS6129694B2 (en)
JPH036139B2 (en)
JPS5929041B2 (en) Antibacterial composition
JP2797279B2 (en) Air treatment method
JPH02302326A (en) Production of active substance
JP2976853B2 (en) Potato fungus inhibitor and method of using the same
US3819354A (en) Tobacco sucker control with dialkyl 1,2,5-thiadiazol-3-yl phosphates
SU801813A1 (en) Method of chemical treatment of substratum
Rajagopal et al. Barley leaf unrolling. The proline connection
HU209689B (en) A method of producing a soil conditioner
JPH0431490A (en) Manufacture of soil conditioner
SU168082A1 (en) METHOD OF OBTAINING SEED PROTECTOR
WO2020047716A1 (en) Pyrazinamide compound, preparation method therefor and application thereof, and bactericide