CN106496347A - A kind of copper complex formazan preparation method of Sargassum polysaccharides - Google Patents

A kind of copper complex formazan preparation method of Sargassum polysaccharides Download PDF

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Publication number
CN106496347A
CN106496347A CN201611056613.2A CN201611056613A CN106496347A CN 106496347 A CN106496347 A CN 106496347A CN 201611056613 A CN201611056613 A CN 201611056613A CN 106496347 A CN106496347 A CN 106496347A
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copper
sargassum polysaccharides
sargassum
copper complex
polysaccharides
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CN106496347B (en
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单俊伟
台文静
王海华
郝晓晨
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Qingdao Haida biological Group Co.,Ltd.
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Qingdao Taihe Biological Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/02Biocides, 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
    • A01N43/04Biocides, 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
    • A01N43/14Biocides, 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
    • A01N43/16Biocides, 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
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N59/00Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/16Heavy metals; Compounds thereof
    • A01N59/20Copper
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05FORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
    • C05F11/00Other organic fertilisers
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G3/00Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003General processes for their isolation or fractionation, e.g. purification or extraction from biomass

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pest Control & Pesticides (AREA)
  • Zoology (AREA)
  • Dentistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Environmental Sciences (AREA)
  • Molecular Biology (AREA)
  • Materials Engineering (AREA)
  • Agronomy & Crop Science (AREA)
  • Polymers & Plastics (AREA)
  • Plant Pathology (AREA)
  • Biochemistry (AREA)
  • Wood Science & Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Sustainable Development (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The present invention relates to a kind of copper complex formazan preparation method of Sargassum polysaccharides, belongs to metal complex field.Sargassum is soaked 6 hours in the hot water, extracts polysaccharide, prepares Sargassum polysaccharides copper complex with copper ion by common full-boiled process under neutrallty condition, and it can be used as feed additive, functional living being fertilizer or bactericide.When acting on animal, can be used as copper supplement, promote erythrocyte maturation, participate in animal osteogenetic process;When acting on plant, while the bactericidal action with copper, and Sargassum polysaccharides growth promotion, degeneration-resistant, antiviral and the effect in plant surface film property, can sterilizing disease-preventing can promote crop growth again.

Description

A kind of copper complex formazan preparation method of Sargassum polysaccharides
Technical field
The present invention relates to a kind of copper complex formazan preparation method of Sargassum polysaccharides, and in particular to one kind with Sargassum and copper ion is The copper complex formazan preparation method of the Sargassum polysaccharides of raw material, belongs to metal complex field.
Technical background
Copper is the necessary element of animal, is the constituent of poultry body various metals enzyme, directly participate in energy i (in vivo) and Substance metabolism.The homergy for maintaining ferrum is simultaneously participated in, catalytic iron participates in the synthesis of hemoglobin, promotes growth early stage erythrocyte Maturation.Copper also participates in the osteogenetic process of animal, and has substantial connection with mitochondrial collagenic supersession and melanin generation.This Outward, appropriate copper ion concentration can also activate pepsin, improve the digestive function of poultry.But, the mantoquita phase of inorganic forms Stimulation can be produced to body gastrointestinal tract compared with complex copper, absorption efficiency is also lower.
Agriculturally, copper agent is effective antibacterial, has more than 100 years history in application agriculturally.Due to not having There is resistance, still using now, wherein most classical is " Bordeaux mixture ", but the medicine should not be made in high temperature or high humidity weather With, and it is vulnerable to the impact of rainwater, use condition and effect are all restricted, and effect duration is short, and copper ion does not give full play to work With.
Sargassum polysaccharides are by a kind of natural polysaccharide for extracting acquisition in marine algae, can increase in cell after being absorbed by plants Soluble polysaccharide content, increase cellular plasm concentration, viscosity increase, elasticity strengthen, improve cell water suction and water conservation energy Power, keeps the Activity and stabill of the enzymes such as hydrolytic enzyme, protease, esterase, so that the membrane structure of cell exempts from destruction, and can With activities of antioxidant enzymes such as enhancement of SOD enzymes, various free radicals are removed, therefore Sargassum polysaccharides are to the drought resisting of plant, cold-resistant, salt resistance energy Power is all significant.Additionally, Sargassum polysaccharides also have good gel characteristic, one layer of protection can be formed in plant surface Film, so as to reduce moisture transpiration, reduces electrolyte in plant cell and is lost in, completely cut off antibacterial and viral and infect, play good Degeneration-resistant, antiviral effect.
Accordingly, we are prepared for Sargassum polysaccharides copper complex, while the bactericidal action with copper, and Sargassum polysaccharides growth-promoting Long, degeneration-resistant, antiviral and the effect in plant surface film property, can sterilizing disease-preventing can promote crop growth again.
Content of the invention
In order to overcome inorganic mantoquita to stimulate big technical deficiency, the present invention to provide a kind of Sargassum polysaccharides copper to body gastrointestinal tract The preparation method of complex, its obtain Sargassum polysaccharides extracting solution after passing through to extract seaweed meal, add mantoquita to generate Sargassum many Sugared copper complex, can be used for meeting demand of the body to copper, and the copper compared to inorganic forms as feed additive Salt its to body gastrointestinal tract without any stimulation, more preferably, and preparation method is simple for absorption efficiency, with low cost, is suitable for commercial scale Upper production in enormous quantities.
For realizing that object above, the main process of the present invention include the extraction of Sargassum polysaccharides and the complexation of Sargassum polysaccharides and copper Reaction, specific as follows:
1)Sargassum polysaccharides are extracted:Seaweed meal crosses 20 mesh sieves after crushing, and adds the water of 10-30 times of weight, stirs at 60-80 DEG C Extract 6 hours, 3500rpm is centrifuged 10 minutes or 600-1000 mesh filter-cloth filterings, obtains Sargassum polysaccharides extracting solution.
2)The preparation of Sargassum polysaccharides copper:Heating makes Sargassum polysaccharides extracting solution be warming up to 70 DEG C, is slowly added to while stirring The copper-bath of 2mol/L, till precipitation is produced, regulation pH to 6.5-7.5, stirring reaction 1-2 hour at 70 DEG C, By 1000-1500 mesh filter-cloth filtering again by the NF membrane of molecular cut off 2000Da, concentrated solution is spray-dried, obtains reactant liquor Arrive Sargassum polysaccharides copper complex;
In Sargassum polysaccharides copper complex preparation method described above, in concentrated solution, solid content is more than 10%, and concentrated solution is spray-dried, and obtains Arrive sea grass polysaccharide copper complex.
Sargassum polysaccharides copper complex preparation method, it is characterised in that the Sargassum includes red algae, Brown algae, chlorella and cyanophyceae In one or more.Wherein described chlorella is one or two of Entermorpha or Thallus Laminariae (Thallus Eckloniae).
The present invention is also claimed the Sargassum polysaccharides copper complex for preparing according to the method described above.
The present invention be also claimed above-mentioned Sargassum polysaccharides copper complex prepare feed additive, functional living being fertilizer or Application in bactericide.
The present invention compared with prior art, it is a technical advantage that:
1)The Sargassum polysaccharides copper complex that method of the present invention is prepared is used for feed additive, can be used for meeting machine Demand of the body to copper, and compared to inorganic forms mantoquita its to body gastrointestinal tract without any stimulation, absorption efficiency is more preferable.
2)The Sargassum polysaccharides copper complex that method of the present invention is prepared has the growth promotion of Sargassum polysaccharides concurrently, resists Inverse, antiviral and the effect in plant surface film property, can sterilizing disease-preventing can promote crop growth again, apply very wide General.
3)The copper complex formazan preparation method preparation method of Sargassum polysaccharides of the present invention is simple, with low cost, is suitable for commercial scale Upper production in enormous quantities.
Specific embodiment
The present invention is further described below by way of specific embodiment, but the embodiment limit this never in any form Bright, those skilled in the art modify in the technology done by technical solution of the present invention or equivalent substitute all should be included in the present invention specially Within sharp protection domain.
Embodiment 1:Chlorella Entermorpha, crushed 20 mesh sieves using pulverizer after drying and obtained Enteromorpha algae powder, took what 20kg sieved In Enteromorpha algae powder input retort, 200L tap waters are added, stirring is opened, is warming up to 60 DEG C, persistently stirring is extracted 6 hours.Instead Answer liquid through 750 mesh filter cloth plate-and-frame filtration, obtain 180L sea grass polysaccharide extracting solution.Sea grass polysaccharide extracting solution is warming up to 70 DEG C, side Stirring side is slowly added to 2mol/L copper-baths, to blue precipitate is produced, adds copper-bath 6.3L altogether, adds The potassium hydroxide solution 2L of 6mol/L, stirs, and detection pH value is 6.68,70 DEG C and continues stirring reaction 1 hour.Reactant liquor is passed through 1200 mesh filter cloth plate-and-frame filtration, then by the NF membrane of molecular cut off 2000Da, obtain concentrated solution 97L, solid content 11.2%, It is spray-dried, obtains 8.5kg sea grass polysaccharide copper complexs.
Embodiment 2:Step adopts Thallus Laminariae (Thallus Eckloniae) for raw material with embodiment 1, and after drying, pulverizer is crushed, and crosses 20 mesh sieves, takes 20kg The Kelp Powder for sieving is put in retort, adds 500L tap waters, is opened stirring, is warming up to 80 DEG C, and persistently stirring extraction 6 is little When.Reactant liquor obtains 470L laminarin extracting solution through 600 mesh filter cloth plate-and-frame filtration.Laminarin extracting solution liquid is warming up to 70 DEG C, it is slowly added to 2mol/L copper-baths while stirring, to blue precipitate is produced, adds copper-bath altogether 8.4L, adds the potassium hydroxide solution 3.4L of 6mol/L, stirs, and detection pH value is that 7.43,70 DEG C of continuation stirring reactions 1 are little When.Reactant liquor is first through 1000 mesh filter cloth plate-and-frame filtration, then by the NF membrane of molecular cut off 2000Da, obtains concentrated solution 82L, Solid content 10.1%, is spray-dried, obtains 6.9kg laminarin copper complexs.
Embodiment 3:Sargassum polysaccharides copper prevents and treats great Jiang Bacterial Leaf Blights
Using counter point, the great Jiang plot of susceptible bacteria sexually transmitted disease (STD) evil is selected, be Sargassum polysaccharides copper, Bordeaux mixture for trying pesticide(Nothing Machine copper), point 3 process(Polysaccharide copper(Prepare by 1 technique of embodiment), Bordeaux mixture, clear water matched group), often spray within 10-12 days Once, 3 times are continuously sprayed.Spray 14 days laggard row indexs to determine, 2 weeks after spraying for the last time, experimental group great Jiang is all received Obtain, determine dry weight, as a result as shown in table 1.
Prevention effect of the 1 Sargassum polysaccharides copper of table to great Jiang Bacterial Leaf Blights
Go out from the experimental results, polysaccharide copper and Bordeaux mixture are sprayed application on easily susceptible great Jiang, can mitigate Bacterial Leaf Blight disease The generation of shape, and the color of the blade of great Jiang is greener, the dry point of blade tip is significantly reduced.The blade performance for spraying Sargassum polysaccharides copper is deep Green, grow vigorous, great Jiang dry weights increase.And compare and the dry point of blade tip then occur, yellowing leaf is more serious.Find out from this test Sargassum polysaccharides copper has certain fungistatic effect, and promotes plant growth.

Claims (5)

1. the copper complex formazan preparation method of a kind of Sargassum polysaccharides, which comprises the following steps:
1)Sargassum polysaccharides are extracted:20 mesh sieves are crossed after Sargassum dries pulverizing, the water of 10-30 times of weight is added, and are stirred at 60-80 DEG C Extract 6 hours, 3500rpm is centrifuged 10 minutes or 600-1000 mesh filter-cloth filterings, obtains Sargassum polysaccharides extracting solution;
2)The preparation of Sargassum polysaccharides copper:Heating makes Sargassum polysaccharides extracting solution be warming up to 70 DEG C, is slowly added to 2mol/L while stirring Copper-bath, until produce precipitation till, adjust pH to 6.5-7.5, stirring reaction 1-2 hour, reactant liquor at 70 DEG C By 1000-1500 mesh filter-cloth filtering again by the NF membrane of molecular cut off 2000Da, concentrated solution is spray-dried, and obtains Sargassum Polysaccharide copper complex.
2. Sargassum polysaccharides copper complex preparation method as claimed in claim 1, it is characterised in that the Sargassum includes red algae, brown One or more in algae, chlorella and cyanophyceae.
3. Sargassum polysaccharides copper complex preparation method as claimed in claim 1, it is characterised in that described chlorella is Entermorpha or sea Band one or two.
4. the method described in claim 1 prepares Sargassum polysaccharides copper complex.
5. Sargassum polysaccharides copper complex described in claim 4 is preparing feed additive, functional living being fertilizer or plant sterilization Application in agent.
CN201611056613.2A 2016-11-26 2016-11-26 A kind of copper complex formazan preparation method of algal polysaccharides Active CN106496347B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107459582A (en) * 2017-06-06 2017-12-12 威海温喜生物科技有限公司 A kind of preparation method of the polysaccharide selenium copper with bactericidal action
CN109776694A (en) * 2017-11-15 2019-05-21 北京市农林科学院 The preparation method and applications of algal polysaccharide copper, iron, three chelate of zinc
CN111848827A (en) * 2020-06-10 2020-10-30 青岛海大生物集团有限公司 Novel chlorella polysaccharide bactericide and preparation method thereof
CN112206549A (en) * 2019-07-09 2021-01-12 宥盛科技股份有限公司 Extraction method of Eucheuma plants
CN112679267A (en) * 2021-01-23 2021-04-20 青岛海大汇信生物科技有限公司 Algal polysaccharide copper-zinc complex liquid fertilizer for preventing and treating crop virus diseases

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03282367A (en) * 1990-03-30 1991-12-12 Snow Brand Milk Prod Co Ltd Determination of free amino acids
CN1148600A (en) * 1996-03-05 1997-04-30 中国科学院南海海洋研究所 Seaweed polysaccharide trace-element complex and its preparation method and usage
CN101999517A (en) * 2010-10-28 2011-04-06 北京资源亚太饲料科技有限公司 Preparation method and application of low-molecular weight seaweed polysaccharide trace element chelate
WO2014130940A1 (en) * 2013-02-22 2014-08-28 Eastern Maine Healthcare Services Antimicrobial blood pressure cuff cover

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03282367A (en) * 1990-03-30 1991-12-12 Snow Brand Milk Prod Co Ltd Determination of free amino acids
CN1148600A (en) * 1996-03-05 1997-04-30 中国科学院南海海洋研究所 Seaweed polysaccharide trace-element complex and its preparation method and usage
CN101999517A (en) * 2010-10-28 2011-04-06 北京资源亚太饲料科技有限公司 Preparation method and application of low-molecular weight seaweed polysaccharide trace element chelate
WO2014130940A1 (en) * 2013-02-22 2014-08-28 Eastern Maine Healthcare Services Antimicrobial blood pressure cuff cover

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107459582A (en) * 2017-06-06 2017-12-12 威海温喜生物科技有限公司 A kind of preparation method of the polysaccharide selenium copper with bactericidal action
CN109776694A (en) * 2017-11-15 2019-05-21 北京市农林科学院 The preparation method and applications of algal polysaccharide copper, iron, three chelate of zinc
CN109776694B (en) * 2017-11-15 2022-01-21 北京市农林科学院 Preparation method and application of copper, iron and zinc triple chelate of brown algae polysaccharide
CN112206549A (en) * 2019-07-09 2021-01-12 宥盛科技股份有限公司 Extraction method of Eucheuma plants
CN111848827A (en) * 2020-06-10 2020-10-30 青岛海大生物集团有限公司 Novel chlorella polysaccharide bactericide and preparation method thereof
CN112679267A (en) * 2021-01-23 2021-04-20 青岛海大汇信生物科技有限公司 Algal polysaccharide copper-zinc complex liquid fertilizer for preventing and treating crop virus diseases

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