CN106818752A - A kind of preparation method of high content kasugarnycin aqua - Google Patents

A kind of preparation method of high content kasugarnycin aqua Download PDF

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CN106818752A
CN106818752A CN201611215666.4A CN201611215666A CN106818752A CN 106818752 A CN106818752 A CN 106818752A CN 201611215666 A CN201611215666 A CN 201611215666A CN 106818752 A CN106818752 A CN 106818752A
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kasugarnycin
preparation
content
aqua
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CN106818752B (en
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王震
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Shaanxi Lvdun Biopharmaceutical Innovation Center Co.,Ltd.
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
    • A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
    • A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
    • A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00—Processes for the preparation of sugar derivatives
    • C07H1/06—Separation; Purification
    • C07H1/08—Separation; Purification from natural products
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
    • C07H15/20—Carbocyclic rings
    • C07H15/207—Cyclohexane rings not substituted by nitrogen atoms, e.g. kasugamycins

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Zoology (AREA)
  • Biochemistry (AREA)
  • Dentistry (AREA)
  • Wood Science & Technology (AREA)
  • Plant Pathology (AREA)
  • Environmental Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Biotechnology (AREA)
  • Genetics & Genomics (AREA)
  • Molecular Biology (AREA)
  • Toxicology (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The present invention relates to a kind of preparation method of high content kasugarnycin aqua, the method can manufacture high concentration kasugarnycin aqua of the content between 5 8%, and salinity is extremely low in product, and using effect is good and easy to use, can meet and fly the anti-grade use demand high to concentration requirement, storage freight is low.

Description

A kind of preparation method of high content kasugarnycin aqua
Technical field
The invention belongs to pesticide field, and in particular to a kind of preparation method of high content kasugarnycin aqua.
Background technology
Kasugarnycin is a kind of aminoglycoside microbial source biological bactericide agricultural chemicals, and product is typically with the water of kasugarnycin one Hydrochloride hydrate form is present, and is mainly used in fungi and the bacteriums such as preventing and treating rice blast, graw mold of tomato, citrus bacterial canker disease Venereal disease does harm to.Due to prevention effect preferably, kasugarnycin application is more and more extensive.
It is well known that aqua is the best formulation of kasugarnycin, with it is environmentally friendly, efficient, safe the features such as.But existing market The kasugarnycin aqua content of upper registration is generally relatively low, and between 2% ~ 4%, cost of transportation is high, in-convenience in use, can not meet The need for the aspect such as winged anti-being surging forward；Many product impurity contents are high, and especially salt content is high, causes product materialization Proterties and using effect are unstable, or even produce poisoning.Therefore in the long run, these problems and defect can all influence product Promote the use of.
The enterprise of domestic registration and sale kasugarnycin low content aqua is many at present, and major product has two classes, and a class is A certain degree of purification is have passed through, but content is not high, typically in 2-4%；Another kind of is not purified thick aqua, only will Zymotic fluid is concentrated to 2%.This two classes product common problem is exactly impurity content high, and the impurity such as salinity and harmful ion does not have There is control, physicochemical properties are unstable, and using effect is bad, or even poisoning can be produced.
In terms of the development of kasugarnycin, disclosed patent has a lot, and the report in terms of purification mainly has mountain " a kind of extraction process of kasugarnycin aqua " disclosed in Xi Xinyuanhua health chemical inc（201510196286.X）, The method of purification of 0.5%-4% kasugarnycin solution has been sketched in the patent.The main deficiency of the presence of this report has three aspects, One is employing saturated ammonium chloride desorption, in causing a large amount of ammonium salts to remain in stripping liquid, ammonium finally is taken off with nanofiltration, NF membrane is born Lotus is high, it is difficult to thoroughly remove ammonium salt, and last a large amount of ammonium salts are remained in the solution, into product.It is molten with reference to ammonium chloride according to applicant Solution angle value actual measurement, at 20 DEG C, the solubility of industrial ammonium chloride exceedes more than 30g, that is, the ammonium chloride percentage composition of solution 23%, except small part is exchanged on resin, major part is stayed in the product, and the de- ammonium of alone nanofiltration, industrially it is difficult to this Function, this point is also demonstrate that in applicant's long-term practice.Second, because salt residues ammonium chloride content is high, product spring thunder Mycin content is difficult to improve, can only be between 0.5-4%.Third, nanofiltration can only slough monovalent ion, for being brought into zymotic fluid The divalent ion such as calcium, magnesium, can only stay in the product, form impurity, influence product content is further improved.
The content of the invention
In order to overcome problems of the prior art, the present invention to provide a kind of preparation side of high content kasugarnycin aqua Method, the method can manufacture high concentration kasugarnycin aqua of the content between 5-8%, and salinity is extremely low in product, and using effect is good And it is easy to use, can meet and fly the anti-grade use demand high to concentration requirement, storage freight is low.
The present invention is adopted the following technical scheme that：A kind of preparation method of high content kasugarnycin aqua, comprises the following steps：
（1）By the zymotic fluid pH value regulation of kasugarnycin between 2 and 6, the Ga in zymotic fluid is removed2+、 Mg2+；
（2）Using ultrafiltration membrance filter, gained filtrate is exchanged using styrene-divinylbenzene crosslinking copolymerization structure highly acidic cation Resin adsorption active ingredient, sloughs impurity；
（3）Using 0.05mol/L（0.02%）Sodium hydroxide solution to 0.5mol/L (2%) is parsed as parsing agent, is obtained To desorbed solution, 5 ~ 40m/h of elution flow rate；The overwhelming majority Na in elution process+It is switched on resin, reduces salinity and bring into Product；
（4）The pH of the desorbed solution that will be obtained is adjusted to 1.5 ~ 6, is concentrated using nanofiltration, and circulating filtration removes residue Na+Salt；Repeatedly After nanofiltration, control kasugarnycin content and solid content meet requirement, required concentration is diluted to pure water, adds preservative, be made Required kasugarnycin aqua.
In a preferred embodiment of the present invention, the zymotic fluid of described kasugarnycin is to be produced using actinomycete fermentation The zymotic fluid of kasugarnycin.
In a preferred embodiment of the present invention, step（1）Middle to use careless acid for adjusting pH value, pH value is preferably 3.5.
In a preferred embodiment of the present invention, step（2）Described in resin preferably 734 sodium form resins, adsorption flow rate It is 5 ~ 40m/h, preferably 20 m/h.
In a preferred embodiment of the present invention, step（3）Middle use 0.15mol/L (0.6%)) sodium hydroxide solution Parsed as parsing agent, elution flow rate is 18 m/h.
In a preferred embodiment of the present invention, step（4）It is middle to use hydrochloric acid to adjust the pH value of desorbed solution be 3.5, with Unnecessary NaOH in removing desorbed solution.
In a preferred embodiment of the present invention, step（4）Middle use aperture is less than 2nm, retains organic matter molecular mass The NF membrane dehydration of 150-300 is concentrated and removes NaCl, when NF membrane permeate speed is reduced to normal speed 40%, to dense Addition and permeate equal quality and electrical conductivity are less than 10 μ S/cm pure water, continuation concentrating and desalinating, repeatedly until spring thunder is mould in contracting liquid Cellulose content is more than 8.5%, and solid content is less than 0.05% less than 10.6% and NaCl contents.
In a preferred embodiment of the present invention, step（4）Described in pure water be electrical conductivity less than 20 μ S/cm pure water.
In a preferred embodiment of the present invention, described preservative be benzoic acid and its esters, sorbic acid and its esters, One or more in propionic acid and its esters, p-hydroxybenzoate, quaternary ammonium salt；Preferably Sodium Benzoate, cheap suitable With；The consumption of described preservative is 0.1%-0.5%, preferably 0.3%.
In a preferred embodiment of the present invention, adding the kasugarnycin aqua after preservative needs to adjust pH to 1.5- 3.5。
In a preferred embodiment of the present invention, adding the kasugarnycin aqua after preservative needs to use 10mol/L hydrochloric acid Will（Aqua stoste）PH is adjusted to 2.8.
Compared with prior art, the present invention has the following technical effect that：
（1）There is provided a kind of preparation method of the aqua higher than kasugarnycin content in existing product, content can be manufactured and existed High concentration kasugarnycin aqua between 5-8%, thoroughly, product purification efficiency is high, and salt content is low in aqua, especially for removing impurities matter NaCl contents are low, and using effect is good, proterties stabilization the features such as.
（2）It is mould using styrene-divinylbenzene crosslinking copolymerization structure sodium form storng-acid cation exchange resin absorption spring thunder Element, using the NaOH of low concentration as eluant, eluent, it is to avoid introduce high salt concentration, this is also a pass for preparing high content aqua Key.
（3）Concentrating and desalinating repeatedly in nanofiltration concentration process, control NaCl contents are below 0.05%.
（4）By repetition test, more than 8.5%, solid content is below 10.6% and NaCl contents for concentration liquid hold-up During less than 0.05%, concentrate can be configured to the aqua of proterties stabilization, meet aqueous pesticide solution requirement.This is also to prepare high content water Another of agent is crucial.
Specific embodiment
In order that the purpose of the present invention, technical scheme and beneficial effect are clearer, present invention specific examples below Illustrate, but the present invention is limited to absolutely not these examples.
Embodiment 1：
（1）Content is weighed for 1.50% zymotic fluid 2500Kg, pH=3.5 is adjusted with oxalic acid, ultra-filtration filters are filtered out altogether 3800Kg filtered fluids, mixed liquor detection level is 0.94%.
（2）3800Kg filtrates are sloughed into impurity with the speed of 20m/h by 734 sodium form resins.
（3）Eluted with the speed of 18m/h with 0.15mol/LNaOH, obtain content for 3.42% kasugarnycin solution 996Kg, pH=7.4.
（4）PH is adjusted to 3.5 with 0.15mol hydrochloric acid, using 1 nanometer of aperture, molecular cut off is that 150-300 nanofiltrations are dense Contracting, when being concentrated into 502Kg, flow velocity is reduced to the 40% of threshold speed, adds the μ S/cm pure water 494Kg of electrical conductivity 9.1 to continue to concentrate, So repeatedly for three times, after testing, content 8.53%, solid content 10.59%, NaCl contents 0.047% are shut down, and obtain concentrate 385Kg。
Concentrate 150Kg is taken, 0.48Kg Sodium Benzoates are added, adds 8.58Kg electrical conductivity to be less than 9.1 μ S/cm pure water, 10mol/L concentrated hydrochloric acid 0.5Kg are added, 8% kasugarnycin aqua 159.56Kg, liquid pH2.8 is obtained.The 150Kg concentrates are taken, 0.64Kg Sodium Benzoates are added, add 62.00Kg electrical conductivity to be less than 9.1 μ S/cm pure water, add 0.61Kg10mol/L concentrated hydrochloric acids, Obtain 6% kasugarnycin aqua 213.25Kg, liquid pH2.8.Concentrate 85Kg is taken, 0.44Kg Sodium Benzoates are added, added 59.17Kg electrical conductivity is less than 9.1 μ S/cm pure water, adds 0.4Kg10mol/L concentrated hydrochloric acids, obtains 5% kasugarnycin aqua 145.01Kg, liquid pH2.8.
Embodiment 2：
（1）Content is weighed for 1.03% zymotic fluid 2500Kg, pH=3.5 is adjusted with oxalic acid, ultra-filtration filters are filtered out altogether 3805Kg filtered fluids, mixed liquor detection level is 0.65%.
（2）3805Kg filtrates are sloughed into impurity with the speed of 20m/h by 734 sodium form resins.
（3）Eluted with the speed of 18m/h with 0.15mol/LNaOH, obtain content for 3.36% kasugarnycin solution 700Kg, pH=7.4.
（3）PH is adjusted to 3.5 with 0.15mol hydrochloric acid, using 1 nanometer of aperture, molecular cut off is 150-300 NF membranes Concentration, when being concentrated into 502Kg, flow velocity is reduced to the 40% of threshold speed, add electrical conductivity less than 9.8 μ S/cm pure water 494Kg after Continuous concentration, so repeatedly for three times, after testing, content 8.50%, solid content 10.55%, NaCl contents 0.047% are shut down, and are obtained To concentrate 274Kg.
To 1.00Kg Sodium Benzoates are added in the concentrate, add 56.41Kg electrical conductivity to be less than 9.8 μ S/cm pure water, add 1.3Kg10mol/L concentrated hydrochloric acids, obtain 7% kasugarnycin aqua 332.71Kg, liquid pH2.8.
Although by referring to the preferred embodiments of the present invention, invention has been described, this area it is common It will be appreciated by the skilled person that various changes can be made to it in the form and details, without departing from appended right The spirit and scope of the present invention that claim is limited.

Claims (10)

1. a kind of preparation method of high content kasugarnycin aqua, it is characterised in that comprise the following steps：
（1）By the pH value regulation of the zymotic fluid of kasugarnycin between 2 and 6, the Ga in zymotic fluid is removed2+、 Mg2+；
（2）Using ultrafiltration membrance filter, gained filtrate is exchanged using styrene-divinylbenzene crosslinking copolymerization structure highly acidic cation Resin adsorption active ingredient, sloughs impurity；
（3）Using 0.05mol/L（0.02%）Sodium hydroxide solution to 0.5mol/L (2%) is parsed as parsing agent, is obtained To desorbed solution, 5 ~ 40m/h of elution flow rate；
（4）The pH of the desorbed solution that will be obtained is adjusted to 1.5 ~ 6, is concentrated using nanofiltration, and circulating filtration removes residue Na+Salt；Receive repeatedly After filter, control kasugarnycin content and solid content meet requirement, required concentration is diluted to pure water, adds preservative, be made institute Need kasugarnycin aqua.
2. preparation method according to claim 1, it is characterised in that the zymotic fluid of described kasugarnycin is to use unwrapping wire The zymotic fluid of the kasugarnycin of bacterium fermenting and producing.
3. preparation method according to claim 1, it is characterised in that step（1）Middle to use careless acid for adjusting pH value, pH value is excellent Elect 3.5 as.
4. preparation method according to claim 1, it is characterised in that step（2）Described in resin preferably 734 sodium form trees Fat, adsorption flow rate is 5 ~ 40m/h, preferably 20 m/h.
5. preparation method according to claim 1, it is characterised in that step（3）Middle use 0.15mol/L (0.6%)) Sodium hydroxide solution is parsed as parsing agent, and elution flow rate is 18 m/h.
6. preparation method according to claim 1, it is characterised in that step（4）It is middle that desorbed solution is adjusted using hydrochloric acid PH value is 3.5, to remove unnecessary NaOH in desorbed solution.
7. preparation method according to claim 1, it is characterised in that step（4）Middle use aperture is less than 2nm, and retention has The NF membrane dehydration of machine thing molecular weight 150-300 is concentrated and removes NaCl, when NF membrane permeate speed is reduced to normal speed When 40%, 10 μ S/cm pure water are less than to addition in concentrate and permeate equal quality and electrical conductivity, continue concentrating and desalinating, repeatedly Until kasugarnycin content is more than 8.5%, solid content is less than 0.05% less than 10.6% and NaCl contents.
8. preparation method according to claim 1, it is characterised in that step（4）Described in pure water be electrical conductivity be less than 20 μ The pure water of S/cm.
9. preparation method according to claim 1, it is characterised in that described preservative is benzoic acid and its esters, mountain One or more in pears acid and its esters, propionic acid and its esters, p-hydroxybenzoate, quaternary ammonium salt；Preferably benzoic acid Sodium；The consumption of described preservative is 0.1%-0.5%, preferably 0.3%.
10. preparation method according to claim 1, it is characterised in that add the kasugarnycin aqua after preservative to need Adjustment pH to 1.5-3.5, preferably adjusts to 2.8.
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107549164A (en) * 2017-08-28 2018-01-09 江苏绿叶农化有限公司 A kind of preparation method of kasugarnycin aqua
CN107987110A (en) * 2017-12-15 2018-05-04 陕西麦可罗生物科技有限公司 A kind of desalination process of kasugarnycin concentrate
CN109666051A (en) * 2017-10-17 2019-04-23 福州奥尼多生物科技有限公司 A kind of purification process of kasugarnycin
CN110452275A (en) * 2019-09-17 2019-11-15 陕西绿盾环境工程研究院有限公司 A kind of preparation method of high-purity kasugarnycin
CN110743630A (en) * 2019-11-14 2020-02-04 江门市植保有限公司 Ion exchange equipment for preparing kasugamycin aqueous solution and aqueous solution preparation method
CN112205409A (en) * 2020-11-27 2021-01-12 陕西麦可罗生物科技有限公司 Kasugamycin and Xinjunan compound water aqua and preparation method thereof
CN113563397A (en) * 2021-09-01 2021-10-29 山东良福制药有限公司 Method for purifying arbekacin
CN114230622A (en) * 2021-11-12 2022-03-25 陕西麦可罗生物科技有限公司 Method for decoloring kasugamycin concentrated solution
CN117063933A (en) * 2023-10-16 2023-11-17 中国远大集团有限责任公司 Kasugamycin organic acid salt, pesticide composition containing kasugamycin organic acid salt and application of kasugamycin organic acid salt

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107549164A (en) * 2017-08-28 2018-01-09 江苏绿叶农化有限公司 A kind of preparation method of kasugarnycin aqua
CN109666051A (en) * 2017-10-17 2019-04-23 福州奥尼多生物科技有限公司 A kind of purification process of kasugarnycin
CN109666051B (en) * 2017-10-17 2021-10-29 福州奥尼多生物科技有限公司 Purification method of kasugamycin
CN107987110A (en) * 2017-12-15 2018-05-04 陕西麦可罗生物科技有限公司 A kind of desalination process of kasugarnycin concentrate
CN110452275A (en) * 2019-09-17 2019-11-15 陕西绿盾环境工程研究院有限公司 A kind of preparation method of high-purity kasugarnycin
CN110452275B (en) * 2019-09-17 2023-04-07 陕西绿盾环境工程研究院有限公司 Preparation method of high-purity kasugamycin
CN110743630A (en) * 2019-11-14 2020-02-04 江门市植保有限公司 Ion exchange equipment for preparing kasugamycin aqueous solution and aqueous solution preparation method
CN112205409A (en) * 2020-11-27 2021-01-12 陕西麦可罗生物科技有限公司 Kasugamycin and Xinjunan compound water aqua and preparation method thereof
CN113563397A (en) * 2021-09-01 2021-10-29 山东良福制药有限公司 Method for purifying arbekacin
CN114230622A (en) * 2021-11-12 2022-03-25 陕西麦可罗生物科技有限公司 Method for decoloring kasugamycin concentrated solution
CN117063933A (en) * 2023-10-16 2023-11-17 中国远大集团有限责任公司 Kasugamycin organic acid salt, pesticide composition containing kasugamycin organic acid salt and application of kasugamycin organic acid salt
CN117063933B (en) * 2023-10-16 2023-12-26 中国远大集团有限责任公司 Kasugamycin organic acid salt, pesticide composition containing kasugamycin organic acid salt and application of kasugamycin organic acid salt

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