CN106496347B - A kind of copper complex formazan preparation method of algal polysaccharides - Google Patents
A kind of copper complex formazan preparation method of algal polysaccharides Download PDFInfo
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- CN106496347B CN106496347B CN201611056613.2A CN201611056613A CN106496347B CN 106496347 B CN106496347 B CN 106496347B CN 201611056613 A CN201611056613 A CN 201611056613A CN 106496347 B CN106496347 B CN 106496347B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
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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
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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
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
- A01N59/20—Copper
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F11/00—Other organic fertilisers
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES 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
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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Abstract
The present invention relates to a kind of copper complex formazan preparation methods of algal polysaccharides, belong to metal complex field.Seaweed is impregnated 6 hours in the hot water, extracts polysaccharide, prepares algal polysaccharides copper complex by heat together method with copper ion under neutrallty condition, it can be used as feed addictive, functional living being fertilizer or bactericide.It when acting on animal, can be used as copper replenishers, promote erythrocyte maturation, participate in animal osteogenetic process；When acting on plant, while there is bactericidal effect and the algal polysaccharides growth promotion, degeneration-resistant, antiviral and in plant surface film forming effect of copper, sterilizing disease-preventing but also crop growth can be promoted.
Description
Technical field
The present invention relates to a kind of copper complex formazan preparation methods of algal polysaccharides, and in particular to a kind of to be with seaweed and copper ion
The copper complex formazan preparation method of the algal polysaccharides of raw material, belongs to metal complex field.
Technical background
Copper is the necessary element of animal, is the constituent of livestock and poultry body various metals enzyme, directly participation energy i (in vivo) and
Metabolism.The eubolism for maintaining iron is simultaneously participated in, catalytic iron participates in the synthesis of hemoglobin, promotes growth early stage red blood cell
Maturation.Copper also participates in the osteogenetic process of animal, and has substantial connection with the collagenic supersession of mitochondria and melanin production.This
Outside, suitable copper ion concentration can also activate pepsin, improve the digestive function of livestock and poultry.But the mantoquita phase of inorganic forms
Stimulation can be generated to body gastrointestinal tract compared with complex copper, absorption efficiency is also lower.
Agriculturally, copper agent is effective fungicide, has more than 100 years history in application agriculturally.Due to not having
There is resistance, is still using now, wherein most classic is " Bordeaux mixture ", but the medicine should not make in high temperature or high humidity weather
With, and the influence vulnerable to rainwater, use condition and effect are all restricted, validity period is short, and copper ion does not give full play to work
With.
Algal polysaccharides are a kind of natural polysaccharides by extracting acquisition in marine algae, can be increased in cell after being absorbed by plants
Soluble polysaccharide content increases cellular plasm concentration, viscosity increase, elasticity enhancing, improves water suction and the water conservation energy of cell
Power, keeps the Activity and stabill of the enzymes such as hydrolase, protease, esterase, to make the membrane structure of cell from destroying, and can
With activities of antioxidant enzymes such as enhancement of SOD enzymes, various free radicals are removed, therefore algal polysaccharides are to the drought resisting of plant, cold-resistant, salt resistance energy
Power is all significant.In addition, algal polysaccharides also have good gel characteristic, one layer of protection can be formed in plant surface
Film reduces dielectric in plant cell and is lost to reduce moisture transpiration, and isolation bacterium is infected with virus, is played good
Degeneration-resistant, antiviral effect.
Accordingly, we are prepared for algal polysaccharides copper complex, while having the bactericidal effect and algal polysaccharides growth-promoting of copper
Effect long, degeneration-resistant, antiviral and in plant surface film forming sterilizing disease-preventing but also can promote crop growth.
Summary of the invention
In order to overcome inorganic mantoquita to stimulate body gastrointestinal tract big technical deficiency, the present invention provides a kind of algal polysaccharides copper
It is more that mantoquita generation seaweed is added by obtaining algal polysaccharides extracting solution after extracting seaweed meal in the preparation method of complex compound
Sugared copper complex can be used for meeting the needs of body is to copper as feed addictive, and compared to the copper of inorganic forms
Salt its to body gastrointestinal tract without any stimulation, absorption efficiency is more preferable, and preparation method is simple, low in cost, is suitble to commercial scale
Upper mass production.
In order to achieve the above object, main process of the invention includes the extraction of algal polysaccharides and the complexing of algal polysaccharides and copper
Reaction, specific as follows:
1) algal polysaccharides extract: seaweed meal smashes it through 20 meshes, the water of 10-30 times of weight is added, at 60-80 DEG C
Stirring is extracted 6 hours, and 3500rpm is centrifuged 10 minutes or 600-1000 mesh filter-cloth filterings, obtains algal polysaccharides extracting solution.
2) preparation of algal polysaccharides copper: heating makes algal polysaccharides extracting solution be warming up to 70 DEG C, is slowly added to while stirring
The copper-bath of 2mol/L adjusts pH to 6.5-7.5, is stirred to react at 70 DEG C 1-2 hours until generating precipitating,
Reaction solution passes through the nanofiltration membrane of molecular cut off 2000Da by 1000-1500 mesh filter-cloth filtering again, and concentrate spray drying obtains
To algal polysaccharides copper complex；
Solid content is greater than 10% in concentrate in algal polysaccharides copper complex preparation method described above, and concentrate is done by spraying
It is dry, obtain sea grass polysaccharide copper complex.
Algal polysaccharides copper complex preparation method, which is characterized in that the seaweed includes red algae, brown alga, green alga and cyanobacteria
One of or it is a variety of.Wherein the green alga is the one or two of Enteromorpha or kelp.
The algal polysaccharides copper complex being prepared according to the method described above is also claimed in the present invention.
The present invention be also claimed above-mentioned algal polysaccharides copper complex prepare feed addictive, functional living being fertilizer or
Application in bactericide.
Compared with prior art, the present invention it is a technical advantage that:
1) the algal polysaccharides copper complex that method of the present invention is prepared is used for feed addictive, can be used for full
Demand of the sufficient body to copper, and compared to the mantoquita of inorganic forms its to body gastrointestinal tract without any stimulation, absorption efficiency is more preferable.
2) the algal polysaccharides copper complex that method of the present invention is prepared has both the growth promotion of algal polysaccharides, resists
Effect inverse, antiviral and in plant surface film forming sterilizing disease-preventing but also can promote crop growth, and application is very wide
It is general.
3) the copper complex formazan preparation method preparation method of algal polysaccharides of the present invention is simple, low in cost, is suitble to commercial scale
Upper mass production.
Specific embodiment
The present invention is further described below by way of specific embodiment, but the embodiment does not limit this hair in any way
Bright, technology modification or equivalent substitute of the those skilled in the art made by technical solution of the present invention should all be included in of the invention special
Within sharp protection scope.
Embodiment 1: green alga Enteromorpha crushed 20 meshes using pulverizer after drying and obtain Enteromorpha algae powder, and 20kg is taken to be sieved
Enteromorpha algae powder is put into reactor tank, and 200L tap water is added, and is opened stirring, is warming up to 60 DEG C, and lasting stirring is extracted 6 hours.Instead
It answers liquid through 750 mesh filter cloth plate-frame filterings, obtains 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-bath, and until generating blue precipitate, copper-bath 6.3L is added altogether, is added
The potassium hydroxide solution 2L of 6mol/L, stirs evenly, and detection pH value is 6.68,70 DEG C and continues to be stirred to react 1 hour.Reaction solution warp
1200 mesh filter cloth plate-frame filterings, then by the nanofiltration membrane of molecular cut off 2000Da, obtain concentrate 97L, solid content 11.2%,
Spray drying, obtains 8.5kg sea grass polysaccharide copper complex.
Embodiment 2: step uses kelp for raw material with embodiment 1, and pulverizer crushes after drying, crosses 20 meshes, takes 20kg
In the Kelp Powder investment reactor tank of sieving, 500L tap water is added, opens stirring, is warming up to 80 DEG C, it is small that lasting stirring extracts 6
When.Reaction solution obtains 470L laminarin extracting solution through 600 mesh filter cloth plate-frame filterings.Laminarin extracting solution liquid is warming up to
70 DEG C, it is slowly added to 2mol/L copper-bath while stirring, until generating blue precipitate, copper-bath is added altogether
8.4L is added the potassium hydroxide solution 3.4L of 6mol/L, stirs evenly, detection pH value be 7.43,70 DEG C continue to be stirred to react 1 it is small
When.Reaction solution is first through 1000 mesh filter cloth plate-frame filterings, then passes through the nanofiltration membrane of molecular cut off 2000Da, obtains concentrate 82L,
Solid content 10.1%, spray drying, obtains 6.9kg laminarin copper complex.
Embodiment 3: algal polysaccharides copper prevents and treats great Jiang Bacterial Leaf Blight
Using counter point, the plot great Jiang of susceptible bacteria venereal disease evil is selected, is algal polysaccharides copper, Bordeaux mixture for examination pesticide
(Inorganic Copper), point 3 processing (polysaccharide copper (preparing by 1 technique of embodiment), Bordeaux mixture, clear water control group), sprays for every 10-12 days
It applies once, continuous spraying 3 times.Laggard row index measurement in 14 days is sprayed, it is 2 weeks after spraying for the last time, experimental group great Jiang is whole
Harvest measures dry weight, and the results are shown in Table 1.
Control efficiency of the 1 algal polysaccharides copper of table to great Jiang Bacterial Leaf Blight
Go out from the experimental results, polysaccharide copper and Bordeaux mixture spray application on easy susceptible great Jiang, and it is withered can to mitigate bacillary leaf
The generation of disease symptoms, and the color of the blade of great Jiang is greener, the dry point of blade tip significantly reduces.Spray the blade performance of algal polysaccharides copper
It is dark green, grow vigorous, great Jiang dry weight increase.And compare and the dry point of blade tip then occur, yellowing leaf is more serious.From this test
Algal polysaccharides copper has certain fungistatic effect out, and promotes plant growth.
Claims (2)
1. a kind of algal polysaccharides copper complex for bactericide, it is characterised in that the algal polysaccharides copper complex is waterside
Tongue fur polysaccharide copper complex；
The copper complex formazan preparation method of sea grass polysaccharide the following steps are included:
1) sea grass polysaccharide extracts: crossing 20 meshes after Enteromorpha dries pulverizing, the water of 10-30 times of weight is added, stirs at 60-80 DEG C
It extracts 6 hours, 3500rpm is centrifuged 10 minutes or 600-1000 mesh filter-cloth filterings, obtains sea grass polysaccharide extracting solution；
2) preparation of sea grass polysaccharide copper: heating makes sea grass polysaccharide extracting solution be warming up to 70 DEG C, is slowly added to 2mol/L while stirring
Copper-bath, until generate precipitating until, adjust pH to 6.5-7.5,1-2 hours are stirred to react at 70 DEG C, reaction solution
Pass through the nanofiltration membrane of molecular cut off 2000Da again by 1000-1500 mesh filter-cloth filtering, concentrate spray drying obtains Enteromorpha
Polysaccharide copper complex.
2. algal polysaccharides copper complex described in claim 1 prepare feed addictive, the application in functional living being fertilizer.
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| CN201611056613.2A CN106496347B (en) | 2016-11-26 | 2016-11-26 | A kind of copper complex formazan preparation method of algal polysaccharides |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| CN111848827B (en) * | 2020-06-10 | 2023-05-16 | 青岛海大生物集团股份有限公司 | 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH03282367A (en) * | 1990-03-30 | 1991-12-12 | Snow Brand Milk Prod Co Ltd | Determination of free amino acids |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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Effective date of registration: 20190520 Address after: 266000 No. 127 Huizhiqiao Road, Qingdao High-tech Zone, Shandong Province Applicant after: Qingdao Seawin Biotech Group Co., Ltd. Address before: 266000 Room B-101, Science Park, Qingdao National University, 127 Huizhiqiao Road, Qingdao High-tech Zone, Shandong Province Applicant before: Qingdao Taihe Biological Technology Co., Ltd. |
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Address after: 266000 No. 127 Huizhiqiao Road, Qingdao High-tech Zone, Shandong Province Patentee after: Qingdao Haida biological Group Co.,Ltd. Address before: 266000 No. 127 Huizhiqiao Road, Qingdao High-tech Zone, Shandong Province Patentee before: QINGDAO SEAWIN BIOTECH GROUP Co.,Ltd. |
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