CN108308176A - Diatom soil matrix plants antimicrobial composite material and preparation method - Google Patents
Diatom soil matrix plants antimicrobial composite material and preparation method Download PDFInfo
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- CN108308176A CN108308176A CN201810031045.3A CN201810031045A CN108308176A CN 108308176 A CN108308176 A CN 108308176A CN 201810031045 A CN201810031045 A CN 201810031045A CN 108308176 A CN108308176 A CN 108308176A
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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
- 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
- A01N25/08—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 solids as carriers or diluents
-
- 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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
-
- 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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
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- Plant Pathology (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Agronomy & Crop Science (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
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- Natural Medicines & Medicinal Plants (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention relates to a kind of diatom soil matrix plants antimicrobial composite material and preparation method, preparation method includes：Diatomite modified：Diatomite is mixed with aluminum salt solution, is stirred, and sodium hydroxide solution is added, filtering, dry, grinding obtain modification infusorial earth；Natural antibacterial plant extract：Natural antibacterial plant is crushed, sieving, obtains dry powder；By dry powder ethanol water ultrasonic extraction, filtering, concentration obtain antibacterial plant extract；Load：The modification infusorial earth, antibacterial plant extract and water are mixed, stirring, filtering, drying obtain diatom soil matrix plants antimicrobial composite material.The present invention utilizes natural plants antiseptic, and method is simple, environmentally protective, and nontoxic and production cost is low.
Description
Technical field
The present invention relates to a kind of anti-biotic material field, more particularly to a kind of diatom soil matrix plants antimicrobial composite material and its
Preparation method.
Background technology
Due to the relative closure of indoor environment, a large amount of of air-conditioning use and raise the reasons such as pet and easily microorganism made largely to grow
It is raw, thus indoor microbial contamination is becoming the principal element for endangering health.The days such as various construction materials and household electrical appliances
Increasing antibacterial functions with product can effectively solve to inhibit the growth of microorganism to infect, and research and development are novel, efficient, nontoxic, lasting
Anti-biotic material have realistic meaning and vast market prospect.
Existing anti-biotic material is broadly divided into three classes：The first kind is inorganic antibacterial material, mainly there is oxide photocatalysis material
Material and metal ion metal oxide type, have many advantages, such as antibacterial wide spectrum, it is long-acting, do not generate drug resistance, heat resistance, but cost
It is higher；Second class is organic anti-bacterial material, mainly have quaternary ammonium salt, quaternary phosphine salt, biguanides, alcohols, phenols, organic metal,
Arsenic pyridine class, imidazoles, antibacterial timeliness is good, but there are toxicity it is big, persistence is poor, drug resistance the problems such as；Third class is natural anti-
Bacterium material, including plant source, animal sources, microbial source natural antibacterial material apply more natural antibacterial material main at present
Include the chitin extracted from animal, chitosan and insect antibiotic property albumen etc., and to the natural plants with antibacterial action
Development and application are abundant not enough.
Diatomite is the siliceous porous sedimentary rock that diatom is formed through geologic process.Main chemical compositions are noncrystal two
Silica also contains a small amount of Al2O3、Fe2O3, CaO, MgO etc..Since diatomite is stablized with performance, large pore volume, aperture be big,
The features such as large specific surface area, strong adsorption capacity, as filter aid, adsorbent and support applications in fine chemistry industry, daily
The fields such as chemical industry.Using diatomite as carrier loaded plants antimicrobial ingredient, novel, nontoxic, the environmentally friendly diatom soil matrix of exploitation is planted
Object anti-biotic material, and be applied to gradually attract attention in the materials such as diatom ooze, coating.
Invention content
It is a primary object of the present invention to provide a kind of novel diatom soil matrix plants antimicrobial composite material and its preparation side
Method, the technical problem to be solved is that making it utilize natural plants antiseptic, method is simple, environmentally protective, nontoxic and produce
It is at low cost, thus more suitable for practicality.
The object of the invention to solve the technical problems is realized using following technical scheme.It proposes according to the present invention
A kind of diatom soil matrix plants antimicrobial composite material preparation method comprising：
Diatomite modified：Diatomite is mixed with aluminum salt solution, is stirred, and sodium hydroxide solution is added, filter, is dry,
Grinding, obtains modification infusorial earth；
Natural antibacterial plant extract：Natural antibacterial plant is crushed, sieving, obtains dry powder；By dry powder ethanol water
Ultrasonic extraction, filtering, concentration, obtains antibacterial plant extract；
Load：The modification infusorial earth, antibacterial plant extract and water are mixed, stirring, filtering, drying obtain silicon
Diatomaceous earth base plants antimicrobial composite material.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
Preferably, the preparation method of diatom soil matrix plants antimicrobial composite material above-mentioned, wherein the diatomite, aluminium salt
Weight ratio with sodium hydroxide is 1:0.5-3:0.2-2.
Preferably, the preparation method of diatom soil matrix plants antimicrobial composite material above-mentioned, wherein the aluminium salt is nitric acid
At least one of aluminium, aluminium chloride and aluminum sulfate.
Preferably, the preparation method of diatom soil matrix plants antimicrobial composite material above-mentioned, wherein the diatomite modified
Drying temperature be 50-80 DEG C, drying time 3-10h.
Preferably, the preparation method of diatom soil matrix plants antimicrobial composite material above-mentioned, wherein the natural antibacterial is planted
Object is at least one of granatum, camphortree leaf, argy wormwood, ginkgo leaf and leaf of bamboo.
Preferably, the preparation method of diatom soil matrix plants antimicrobial composite material above-mentioned, wherein the natural antibacterial is planted
Sieving in object extraction is sieved for 80-300 mesh；
The volume fraction of the ethanol water is 50-70%；
The weight ratio of the dry powder and ethanol water is 1:10-30；
The time of the ultrasonic extraction of the natural antibacterial plant extract is 20-60min, and the temperature of concentration is 50-80 DEG C.
Preferably, the sieving in the natural antibacterial plant extract is sieved for 120-200 mesh；
Preferably, the preparation method of diatom soil matrix plants antimicrobial composite material above-mentioned, wherein the modification of the load
The weight ratio of diatomite, antibacterial plant extract and water is 1:0.125-1:20-50.
Preferably, the preparation method of diatom soil matrix plants antimicrobial composite material above-mentioned, wherein the stirring of the load
Intensity is 300-800rpm, mixing time 0.5-7h；
The drying temperature of the load is 50-80 DEG C, drying time 3-10h.
The object of the invention to solve the technical problems is also realized using technical solution below.It proposes according to the present invention
A kind of diatom soil matrix plants antimicrobial composite material, be prepared by method above-mentioned；The diatom soil matrix plants antimicrobial is multiple
Condensation material, in terms of parts by weight comprising：
Modification infusorial earth：1 part；
Antibacterial plant extract：0.125-1 parts.
By above-mentioned technical proposal, under diatom soil matrix plants antimicrobial composite material and preparation method of the present invention at least has
Row advantage：
1) present invention replaces applying more organic antibacterial agent and inorganic antiseptic, method letter using plants antimicrobial extract
Single, environmentally protective, nontoxic and production cost is low, and the natural antibacterial plant utilized belongs to renewable resource, while being agriculture
Byproduct makes natural resources be fully utilized, and alleviate environmental pressure and can generate economic benefit；
2) present invention has carried out simple extraction to natural antibacterial plant, can effectively obtain antibacterial active principle, removes
It is easy to cause the invalid components of plant moldy metamorphism itself, while in turn avoiding the complicated technological process of plant essence extraction, operation
It is simple for process effective, it is easy to industrialized production；
3) antibacterial plant extract is loaded on modification infusorial earth, can be protected using modification infusorial earth as carrier by the present invention
The antibacterial ability of plants antimicrobial ingredient is held, while the application environment of plants antimicrobial ingredient can be expanded.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, it is described in detail as after with presently preferred embodiments of the present invention below.
Specific implementation mode
It is of the invention to reach the technological means and effect that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Preferred embodiment, to diatom soil matrix plants antimicrobial composite material and preparation method its specific embodiment party proposed according to the present invention
Formula, structure, feature and its effect are described in detail as after.In the following description, different " embodiment " or " embodiment " refers to
It is not necessarily the same embodiment.In addition, the special characteristic, structure or feature in one or more embodiments can be by any suitable shape
Formula combines.
A kind of preparation method for diatom soil matrix plants antimicrobial composite material that one embodiment of the present of invention proposes, packet
It includes：
Diatomite modified：Diatomite is mixed with aluminum salt solution, is stirred, and sodium hydroxide solution is added dropwise, filtering,
50-80 DEG C of dry 3-10h, grinding, obtain modification infusorial earth；
Natural antibacterial plant extract：Natural antibacterial plant is crushed, crosses 80-300 mesh sieve, obtains dry powder；By dry powder body
Fraction be 50-70% ethanol water ultrasonic extraction 20-60min, filtering, 50-80 DEG C be concentrated under reduced pressure into constant weight, obtain antibacterial
Plant extracts；
Load：It is 1 by weight by the modification infusorial earth, antibacterial plant extract and water:0.125-1:20-50 is mixed
It closes, 300-800rpm stirs 0.5-7h, and filtering, 50-80 DEG C of dry 3-10h obtain diatom soil matrix plants antimicrobial composite material.
Preferably, the weight ratio of diatomite, aluminium salt and sodium hydroxide is 1:0.5-3:0.2-2.
Preferred aluminium salt is at least one of aluminum nitrate, aluminium chloride and aluminum sulfate.
Preferably, natural antibacterial plant is at least one of granatum, camphortree leaf, argy wormwood, ginkgo leaf and leaf of bamboo.
Preferably, the sieving in natural antibacterial plant extract was 120-200 mesh sieve；
Preferably, the weight ratio of dry powder and ethanol water is 1:10-30；
Another embodiment of the present invention proposes a kind of diatom soil matrix plants antimicrobial composite material, prepared by method above-mentioned and
；The diatom soil matrix plants antimicrobial composite material, in terms of parts by weight comprising：
Modification infusorial earth：1 part；
Antibacterial plant extract：0.125-1 parts.
Embodiment 1
A kind of preparation method for diatom soil matrix plants antimicrobial composite material that one embodiment of the present of invention proposes, packet
It includes：
Diatomite modified：Weigh 23.8g Al (NO3)3·9H2O is scattered in 500mL deionized waters, has been evenly stirred until
Fully dissolved, is added 10g diatomite, and magnetic agitation is uniform；It weighs 4.8g NaOH to be scattered in 300mL deionized waters, stir evenly
To being completely dissolved, sodium hydroxide solution is obtained；Sodium hydroxide solution is added dropwise to diatomite and aluminum nitrate mixed solution, is mixed
Close suspension；Mixing suspension is carried out the first filter cake is filtered by vacuum to obtain, the first filter cake is dried using air dry oven,
Drying temperature is 60 DEG C, is then ground the first filter cake being completely dried, obtains modification infusorial earth.
Natural antibacterial plant extract：Granatum is crushed, 200 mesh sieve is crossed, dry powder is made；10g dry powder is taken to be placed in beaker,
The ethanol water that 150g volume fractions are 70% is added, utilizes supersonic cell pulverizer, ultrasound assisted extraction 0.5h, vacuum
Suction filtration obtains extracting solution；By 65 DEG C of reduced pressures of extracting solution, recycling design recycles, until extracting solution is concentrated under reduced pressure into constant weight and obtains
To about 5g pomegranate rind extracts.
Pomegranate rind extract is diluted 10 times, with nutrient broth medium, staphylococcus aureus bacteria suspension (bacteria concentration
104-2×104Cfu/mL) by volume 1:3:1 shakes even, takes the mixed liquor 1mL injections after (37 DEG C) of constant temperature oscillation 10h sterile flat
Ware, the fluid nutrient medium for being then injected into 55 DEG C of 30mL shake up, after solidification 37 DEG C of constant temperature incubations for 24 hours, pomegranate rind extract it is antibacterial
Rate is more than 95%.
Load：It is completely dissolved in pomegranate rind extract 2.5g in 150mL deionized waters, modification infusorial earth 5g, room temperature is added
The second filter cake is filtered by vacuum to obtain after magnetic agitation intensity is 500rpm in lower magnetic agitation 3h, is filtered second using air dry oven
Cake is dried, and drying temperature is 60 DEG C, is then ground the second filter cake, obtains diatom soil matrix plants antimicrobial composite wood
Material.
Another embodiment of the present invention proposes a kind of diatom soil matrix plants antimicrobial composite material, by the method system of embodiment 1
It is standby and obtain.The diatom soil matrix plants antimicrobial composite material of embodiment 1 is subjected to antibiotic property detection：Diatom soil matrix plants antimicrobial is compound
Material 1g is scattered in 10mL deionized waters, with nutrient broth medium, staphylococcus aureus bacteria suspension (bacteria concentration 104-2
×104Cfu/mL) by volume 1:3:1 difference mixing takes the mixed liquor 1mL injections after (37 DEG C) oscillation 10h of constant temperature sterile flat
Ware, the fluid nutrient medium for being then injected into 55 DEG C of 30mL shake up, and 37 DEG C of constant temperature incubations for 24 hours, observe bacterium colony growing state after solidification,
Bacteriostasis rate is 60%.
Embodiment 2
A kind of preparation method for diatom soil matrix plants antimicrobial composite material that one embodiment of the present of invention proposes, packet
It includes：
Diatomite modified：Weigh 23.8g Al (NO3)3·9H2O is scattered in 500mL deionized waters, has been evenly stirred until
Fully dissolved, is added 10g diatomite, and magnetic agitation is uniform；It weighs 4.8g NaOH to be scattered in 300mL deionized waters, stir evenly
To being completely dissolved, sodium hydroxide solution is obtained；Sodium hydroxide solution is added dropwise to diatomite and aluminum nitrate mixed solution, is mixed
Close suspension；Mixing suspension is carried out the first filter cake is filtered by vacuum to obtain, the first filter cake is dried using air dry oven,
Drying temperature is 60 DEG C, is then ground the first filter cake being completely dried, obtains modification infusorial earth.
Natural antibacterial plant extract：Granatum is crushed, 200 mesh sieve is crossed, dry powder is made；10g dry powder is taken to be placed in beaker,
The ethanol water that 150g volume fractions are 70% is added, utilizes supersonic cell pulverizer, ultrasound assisted extraction 0.5h, vacuum
Suction filtration obtains extracting solution；By 65 DEG C of reduced pressures of extracting solution, recycling design recycles, until extracting solution is concentrated under reduced pressure into constant weight and obtains
To about 5g pomegranate rind extracts.
Pomegranate rind extract is diluted 10 times, with nutrient broth medium, staphylococcus aureus bacteria suspension (bacteria concentration
104-2×104Cfu/mL) by volume 1:3:1 shakes even, takes the mixed liquor 1mL injections after (37 DEG C) of constant temperature oscillation 10h sterile flat
Ware, the fluid nutrient medium for being then injected into 55 DEG C of 30mL shake up, after solidification 37 DEG C of constant temperature incubations for 24 hours, pomegranate rind extract it is antibacterial
Rate is more than 95%.
Load：Pomegranate rind extract 5g is completely dissolved in 150mL deionized waters, addition modification infusorial earth 5g, under room temperature
The second filter cake is filtered by vacuum to obtain after magnetic agitation intensity is 500rpm in magnetic agitation 3h, using air dry oven by the second filter cake
It is dried, drying temperature is 60 DEG C, is then ground the second filter cake, obtains diatom soil matrix plants antimicrobial composite material.
Another embodiment of the present invention proposes a kind of diatom soil matrix plants antimicrobial composite material, by the method system of embodiment 2
It is standby and obtain.The diatom soil matrix plants antimicrobial composite material of embodiment 2 is subjected to antibiotic property detection：Diatom soil matrix plants antimicrobial is compound
Material 1g is scattered in 10mL deionized waters, with nutrient broth medium, staphylococcus aureus bacteria suspension (bacteria concentration 104-2
×104Cfu/mL) by volume 1:3:1 difference mixing takes the mixed liquor 1mL injections after (37 DEG C) oscillation 10h of constant temperature sterile flat
Ware, the fluid nutrient medium for being then injected into 55 DEG C of 30mL shake up, and 37 DEG C of constant temperature incubations for 24 hours, observe bacterium colony growing state after solidification,
Bacteriostasis rate is more than 95%.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, according to
According to the technical spirit of the present invention to any simple modification, equivalent change and modification made by above example, this hair is still fallen within
In the range of bright technical solution.
Claims (9)
1. a kind of preparation method of diatom soil matrix plants antimicrobial composite material, which is characterized in that it includes：
Diatomite modified：Diatomite is mixed with aluminum salt solution, is stirred, and sodium hydroxide solution is added, filtering, dry, grinding,
Obtain modification infusorial earth；
Natural antibacterial plant extract：Natural antibacterial plant is crushed, sieving, obtains dry powder；By dry powder ethanol water ultrasound
Extraction, filtering, concentration, obtains antibacterial plant extract；
Load：The modification infusorial earth, antibacterial plant extract and water are mixed, stirring, filtering, drying obtain diatomite
Base plants antimicrobial composite material.
2. the preparation method of diatom soil matrix plants antimicrobial composite material according to claim 1, which is characterized in that described
The weight ratio of diatomite, aluminium salt and sodium hydroxide is 1:0.5-3:0.2-2.
3. the preparation method of diatom soil matrix plants antimicrobial composite material according to claim 1, which is characterized in that described
Aluminium salt is at least one of aluminum nitrate, aluminium chloride and aluminum sulfate.
4. the preparation method of diatom soil matrix plants antimicrobial composite material according to claim 1, which is characterized in that described
The drying temperature of diatomite modified is 50-80 DEG C, drying time 3-10h.
5. the preparation method of diatom soil matrix plants antimicrobial composite material according to claim 1, which is characterized in that described
Natural antibacterial plant is at least one of granatum, camphortree leaf, argy wormwood, ginkgo leaf and leaf of bamboo.
6. the preparation method of diatom soil matrix plants antimicrobial composite material according to claim 1, which is characterized in that described
Sieving in natural antibacterial plant extract is sieved for 80-300 mesh；
The volume fraction of the ethanol water is 50-70%；
The weight ratio of the dry powder and ethanol water is 1:10-30；
The time of the ultrasonic extraction of the natural antibacterial plant extract is 20-60min, and the temperature of concentration is 50-80 DEG C.
7. the preparation method of diatom soil matrix plants antimicrobial composite material according to claim 1, which is characterized in that described
The weight ratio of the modification infusorial earth of load, antibacterial plant extract and water is 1:0.125-1:20-50.
8. the preparation method of diatom soil matrix plants antimicrobial composite material according to claim 1, which is characterized in that described
The stirring intensity of load is 300-800rpm, mixing time 0.5-7h；
The drying temperature of the load is 50-80 DEG C, drying time 3-10h.
9. a kind of diatom soil matrix plants antimicrobial composite material, which is characterized in that by claim 1-8 any one of them method systems
It is standby and obtain；The diatom soil matrix plants antimicrobial composite material, in terms of parts by weight comprising：
Modification infusorial earth：1 part；
Antibacterial plant extract：0.125-1 parts.
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