CN106135275A - A kind of preparation method of the sepiolite antimicrobial powder of organically-modified and load silver ion - Google Patents

A kind of preparation method of the sepiolite antimicrobial powder of organically-modified and load silver ion Download PDF

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Publication number
CN106135275A
CN106135275A CN201610467775.9A CN201610467775A CN106135275A CN 106135275 A CN106135275 A CN 106135275A CN 201610467775 A CN201610467775 A CN 201610467775A CN 106135275 A CN106135275 A CN 106135275A
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sepiolite
modified
organically
silver ion
preparation
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CN201610467775.9A
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Inventor
刘平乐
吴生焘
郝芳
熊伟
熊绍锋
罗和安
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Xiangtan Yuanhai Sepiolite New Material Co Ltd
Xiangtan University
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Xiangtan Yuanhai Sepiolite New Material Co Ltd
Xiangtan University
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Priority to CN201610467775.9A priority Critical patent/CN106135275A/en
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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
    • 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
    • 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
    • A01N25/34—Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group

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  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • Agronomy & Crop Science (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses the preparation method of the sepiolite antimicrobial powder of a kind of organically-modified and load silver ion.The method includes the load of the organically-modified and silver ion of the pretreatment of sepiolite, sepiolite.The present invention selects sepiolite as carrier, cheap and easy to get, utilize organically-modified after sepiolite adsorbent solution in the antibacterial powder prepared by silver ion not only reduce industrial cost, and simplification of flowsheet；And it is nontoxic.In addition, the little consumption of products obtained therefrom of the present invention can obtain extraordinary adsorption effect, and processing rapidly, adsorbance is high, and antibacterial effect can keep the longer time, has preferable silver ion slow release.

Description

A kind of preparation method of the sepiolite antimicrobial powder of organically-modified and load silver ion
Technical field
The present invention relates to material preparation and field of chemical engineering, particularly to a kind of organically-modified and load silver ion sea The preparation method of afrodite antimicrobial powder.
Background technology
The application of current antibacterial powder is more and more extensive.From the daily fiber garment wearing, to the household electric of household Device, sanitary ceramic goods, plastic sheeting and steel plate for building, coating etc., antibacterial powder all or has played important Effect.
Inorganic antibacterial powder is usually and is made up of antibacterial components and carrier.Its preparation method is to have antibacterial ability by absorption Silver, the metal such as copper be fixed on the surface of inorganic carrier and prepare.In numerous inorganic carriers, sepiolite and bentonite, boiling These existing inorganic carriers of stone, phosphate, adsorptivity silica gel and glass are compared, and show the property of more preferable Adsorption For Ag ion Can, and bigger specific surface area, dispersiveness and heat endurance, it is allowed to have in the development of inorganic Ag-carried antibacterial powder wide Application prospect.
Chengdu University of Technology Liu Jing etc. (CN101142919) are with sepiolite as carrier, and load silver zinc ion prepares antibacterial powder. Although preparation process is relatively simple, low cost, but its physical adsorption process can not keep long antibacterial effect, and not Very low to silver-colored adsorbance through the sepiolite of modification.
It is high generally to there is industrial cost in existing antibacterial powder carrier, and complex process, slow release are undesirable, and silver-colored adsorbance is low Problem.Therefore, the present invention by selecting that deposit is abundant, industrial cost is low, specific surface area is big, high temperature resistant, resistance to acids and bases, nontoxic Sepiolite, as absorption carrier, carries out pretreatment and organically-modified process by simple method to sepiolite, improves carrier pair The absorption of silver particles, to overcome above-mentioned technical problem.
Content of the invention
It is an object of the invention to overcome the deficiencies in the prior art to provide a kind of organically-modified and load silver ion Hai Pao The preparation method of stone antimicrobial powder.
A kind of preparation method of the sepiolite antimicrobial powder of organically-modified and load silver ion, including the pre-place of sepiolite Reason, the load of organically-modified and silver ion of sepiolite, specifically include following steps:
(1) meerschaum pretreatment: raw ore sepiolite is 1:10 ~ 20 by solid-liquid mass ratio, with hydrochloric acid 25 ~ 125 DEG C under conditions of Pretreatment 2 ~ 12h, then suction filtration, the filter residue obtaining is dried；
(2) adding organic solvent and distilled water in step (1) gained sepiolite, sepiolite with the mass ratio of organic solvent is 0.2:0.1 ~ 1.2, impregnate 1 ~ 18h under the conditions of 25 ~ 85 DEG C, suction filtration with absolute ethanol washing 2 ~ 6 times, and drying, barreling must have Machine modified meerschaum；
(3) organically-modified for step (2) gained sepiolite or step (1) gained are pre-processed sepiolite and join silver ion solution In, it is sufficiently stirred for 1 ~ 72h, centrifugal rear distilled water washs 2 ~ 5 times, i.e. obtains sepiolite that is organically-modified and that load anion after being dried Antimicrobial powder.
Further, the concentration of hydrochloric acid used by step (1) is 0.2 ~ 5mol/L.
Further, the drying of step (1), temperature preferably 80 ~ 150 DEG C, time preferably 6 ~ 15h.
Further, the preferred cetyl trimethylammonium bromide of the organic solvent (CTAB) of step (2), detergent alkylate sulphur Acid sodium (SDBS), one or more in lauryl sodium sulfate (SDS).
Further, step (3) the preferred silver nitrate solution of silver ion solution, silver ammonium complex liquid, silver oxalate solution, acetic acid Silver solution, one or more in silver citrate solution, the concentration of silver ion solution is 0.01 ~ 0.5mol/L.
Further, in step (3), the organically-modified sepiolite of step (2) gained is or/and the pretreatment of step (1) gained is extra large Afrodite is 1:12 ~ 18 with the solid-liquid mass ratio of silver ion solution.
The beneficial effects of the present invention is:
The present invention selects sepiolite as carrier, cheap and easy to get, utilize organically-modified after sepiolite adsorbent solution in silver from Antibacterial powder prepared by Zi not only reduces industrial cost, and simplification of flowsheet；And it is nontoxic.In addition, gained of the present invention The little consumption of product can obtain extraordinary adsorption effect, and processes rapidly, and adsorbance is high, and antibacterial effect can be protected Hold the longer time, there is preferable silver ion slow release.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further details, but the present invention is not limited to this.
Embodiment 1
(1) meerschaum pretreatment: raw ore sepiolite is 1:15 by solid-to-liquid ratio, at 0.75mol/L, carries out hydrochloric acid under conditions of 75 DEG C Pretreatment 10h, the filter residue that suction filtration obtains is in 105 DEG C of dry 12h.The sepiolite obtaining is carried out BET sign, and result shows and compares table Area is from 70 m2/ g increases to 204m2/g。
(2) 0.2g neopelex (SDBS) is dissolved in 50mL water, and the sepiolite adding 1g step (1) to obtain exists Impregnating 18h under the conditions of 30 DEG C, suction filtration with absolute ethanol washing 3 times, drying, barreling is standby, prepared organically-modified sepiolite.
(3) sepiolite that the sepiolite obtaining in step (2) and step (1) obtain is added separately to 0.1mol/l's AgNO3In solution, solid-liquid mass ratio is that 1:15(sepiolite is to AgNO3Solution), it is sufficiently stirred for 36h, make both fully combine, from The heart, distilled water washs 3 times, is dried, and barreling is standby.The adsorbance of the silver of organically-modified sepiolite antibacterial powder is 145mg/g, and The adsorbance of the silver of not organically-modified sepiolite antibacterial powder is only 60mg/g.
(4) antibacterial powder that step (3) is made is pressed into drug sheet respectively to be placed in containing staphylococcus aureus, large intestine bar Bacterium, Candida albicans Solid agar culture in, under the conditions of 37 DEG C cultivate 24h.Organically-modified sepiolite antibacterial powder Inhibition zone is 13mm, and the inhibition zone of not organically-modified sepiolite antibacterial powder is 4mm.
Embodiment 2
(1) meerschaum pretreatment: raw ore sepiolite is 1:10 by solid-to-liquid ratio, at 1.5mol/L, carries out hydrochloric acid under conditions of 50 DEG C Pretreatment 8h, the filter residue that suction filtration obtains is in 105 DEG C of dry 12h.The sepiolite obtaining is carried out BET sign, and result shows and compares table Area is from 70 m2/ g increases to 194m2/g。
(2) 0.4g neopelex (SDBS) is dissolved in 50mL water, adds the sepiolite of 1g step (1) at 40 DEG C Under the conditions of dipping 10h, suction filtration with absolute ethanol washing 4 times, drying, barreling is standby, prepared organically-modified sepiolite.
(3) sepiolite that the sepiolite obtaining in step (2) and step (1) obtain is added separately to 0.2mol/l's AgNO3In solution, solid-liquid mass ratio is that 1:16(sepiolite is to AgNO3Solution), it is sufficiently stirred for 48h, make both fully combine, from The heart, distilled water washs 4 times, is dried, and barreling is standby.The adsorbance of organically-modified sepiolite antibacterial powder silver is 136mg/g, and not The adsorbance of organically-modified sepiolite antibacterial powder silver is 58mg/g.
(4) antibacterial powder that step (3) is made is pressed into drug sheet respectively to be placed in containing staphylococcus aureus, large intestine bar Bacterium, Candida albicans Solid agar culture in, under the conditions of 37 DEG C cultivate 24h, organically-modified sepiolite antibacterial powder Inhibition zone is 12mm, and the inhibition zone of not organically-modified sepiolite antibacterial powder is 3.9mm.
Embodiment 3
(1) meerschaum pretreatment: raw ore sepiolite is 1:20 by solid-to-liquid ratio, at .1.25mol/L, carries out salt under conditions of 25 DEG C Low-kappa number 4h, the filter residue that suction filtration obtains in 105 DEG C of dry 12h,.To obtain sepiolite and carry out BET sign, result shows and compares table Area is from 70 m2/ g increases to 186m2/g。
(2) 0.6g neopelex (SDBS) is dissolved in 50mL water, adds the sepiolite of 1g step (1) at 30 DEG C Under the conditions of dipping 18h, suction filtration with absolute ethanol washing 3 times, drying, barreling is standby, prepared organically-modified sepiolite.
(3) sepiolite that the sepiolite obtaining in step (2) and step (1) obtain is added separately to the silver-colored ammonium of 0.3mol/l In complex liquid, solid-liquid mass ratio is that 1:15(sepiolite is to silver ammonium complex liquid), it is sufficiently stirred for 36h, make both fully combine, from The heart, distilled water washs 3 times, is dried, and barreling is standby.The adsorbance of organically-modified sepiolite antibacterial powder silver is 125mg/g, and not The adsorbance of the silver of organically-modified sepiolite antibacterial powder is 54mg/g.
(4) antibacterial powder that step (3) is made is pressed into drug sheet respectively to be placed in containing staphylococcus aureus, large intestine bar Bacterium, Candida albicans Solid agar culture in, under the conditions of 37 DEG C cultivate 24h.Organically-modified sepiolite antibacterial powder Inhibition zone is 11mm, and the inhibition zone of not organically-modified sepiolite antibacterial powder is 3.6mm.
Embodiment 4
(1) meerschaum pretreatment: raw ore sepiolite is 1:15 by solid-to-liquid ratio, at 1mol/L, carries out hydrochloric acid pre-under conditions of 25 DEG C Processing 10h, suction filtration obtains filter residue in 105 DEG C of dry 12h.The sepiolite obtaining carries out BET sign, and result shows specific surface area From 70 m2/ g increases to 165m2/g。
(2) 1g neopelex (SDBS) is dissolved in 50mL water, adds the sepiolite of 1g step (1) at 30 DEG C of bars Impregnating 18h under part, suction filtration with absolute ethanol washing 3 times, drying, barreling is standby, prepared organically-modified sepiolite.
(3) sepiolite that the sepiolite obtaining in step (2) and step (1) obtain is added separately to 0.1mol/l's AgNO3In solution, solid-liquid mass ratio is that 1:12(sepiolite is to AgNO3Solution), it is sufficiently stirred for 36h, make both fully combine, from The heart, distilled water washs 3 times, is dried, and barreling is standby.The adsorbance of organically-modified sepiolite antibacterial powder silver is 123mg/g, and not The adsorbance of organically-modified sepiolite antibacterial powder silver is 60mg/g.
(4) antibacterial powder that step (3) is made is pressed into respectively drug sheet and is placed in containing in germy Solid agar culture, Cultivating 24h under the conditions of 37 DEG C, the inhibition zone of organically-modified sepiolite antibacterial powder is 10.9mm, and not organically-modified Hai Pao The inhibition zone of stone antibacterial powder is 3.9mm.

Claims (7)

1. one kind organically-modified and the preparation method of the sepiolite antimicrobial powder of load silver ion, it is characterised in that includes Hai Pao The pretreatment of stone, the load of organically-modified and silver ion of sepiolite.
2. the preparation method of the sepiolite antimicrobial powder of according to claim 1 organically-modified and load silver ion, it is special Levy and be, specifically include following steps:
(1) meerschaum pretreatment: raw ore sepiolite is 1:10 ~ 20 by solid-liquid mass ratio, with hydrochloric acid 25 ~ 125 DEG C under conditions of Pretreatment 2 ~ 12h, then suction filtration, the filter residue obtaining is dried；
(2) adding organic solvent and distilled water in step (1) gained sepiolite, sepiolite with the mass ratio of organic solvent is 0.2:0.1 ~ 1.2, impregnate 1 ~ 18h under the conditions of 25 ~ 85 DEG C, suction filtration with absolute ethanol washing 2 ~ 6 times, and drying, barreling must have Machine modified meerschaum；
(3) organically-modified for step (2) gained sepiolite or step (1) gained are pre-processed sepiolite and join silver ion solution In, it is sufficiently stirred for 1 ~ 72h, centrifugal rear distilled water washs 2 ~ 5 times, i.e. obtains organically-modified and load silver ion sepiolite after being dried Antimicrobial powder.
3. the preparation method of the sepiolite antimicrobial powder of according to claim 1 organically-modified and load silver ion, it is special Levying and being, used by step (1), the concentration of hydrochloric acid is 0.2 ~ 5mol/L.
4. the preparation method of the sepiolite antimicrobial powder of according to claim 1 organically-modified and load silver ion, it is special Levy and be, the drying of step (1), temperature preferably 80 ~ 150 DEG C, time preferably 6 ~ 15h.
5. the preparation method of the sepiolite antimicrobial powder of according to claim 1 organically-modified and load silver ion, it is special Levy and be, the preferred cetyl trimethylammonium bromide of the organic solvent (CTAB) of step (2), neopelex (SDBS), one or more in lauryl sodium sulfate (SDS).
6. the preparation method of the sepiolite antimicrobial powder of according to claim 1 organically-modified and load silver ion, it is special Levying and being, the silver ion solution of step (3) is silver nitrate solution, silver ammonium complex liquid, silver oxalate solution, silver acetate solution, lemon Acid silver solution in one or more, the concentration of silver ion solution is 0.01 ~ 0.5mol/L.
7. the preparation method of the sepiolite antimicrobial powder of according to claim 1 organically-modified and load silver ion, it is special Levy and be, in step (3), the organically-modified sepiolite of step (2) gained or/and step (1) gained pretreatment sepiolite with silver from The solid-liquid mass ratio of sub-solution is 1:12 ~ 18.
CN201610467775.9A 2016-06-24 2016-06-24 A kind of preparation method of the sepiolite antimicrobial powder of organically-modified and load silver ion Pending CN106135275A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106665651A (en) * 2017-01-11 2017-05-17 湘潭大学 Preparation method of stable sepiolite antibacterial powder
CN108677272A (en) * 2018-05-15 2018-10-19 华南理工大学 A kind of micro inorganic anti-bacterial fibre and preparation method thereof
CN109090140A (en) * 2018-10-09 2018-12-28 湘潭大学 The preparation method of chitin modified sepiolite supported zinc antibacterial powder
CN109122717A (en) * 2018-10-09 2019-01-04 湘潭大学 The preparation method of chitin modified sepiolite supported silver-colored antibacterial powder
CN109349272A (en) * 2018-10-09 2019-02-19 湘潭大学 A kind of preparation method of sepiolite supported Chitosan-Silver antibacterial powder
CN111357765A (en) * 2020-03-17 2020-07-03 长沙天源羲王材料科技有限公司 Preparation method of water-oil universal nano-silver antibacterial agent for antibacterial coating
CN112006031A (en) * 2020-08-25 2020-12-01 广东欧文莱陶瓷有限公司 Antibacterial agent for ceramics, antibacterial ceramics and preparation method thereof

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CN105638731A (en) * 2016-01-30 2016-06-08 湘潭大学 Preparation method of antibacterial sepiolite powder

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106665651A (en) * 2017-01-11 2017-05-17 湘潭大学 Preparation method of stable sepiolite antibacterial powder
CN108677272A (en) * 2018-05-15 2018-10-19 华南理工大学 A kind of micro inorganic anti-bacterial fibre and preparation method thereof
CN108677272B (en) * 2018-05-15 2020-09-22 华南理工大学 Micron-sized inorganic antibacterial fiber and preparation method thereof
CN109090140A (en) * 2018-10-09 2018-12-28 湘潭大学 The preparation method of chitin modified sepiolite supported zinc antibacterial powder
CN109122717A (en) * 2018-10-09 2019-01-04 湘潭大学 The preparation method of chitin modified sepiolite supported silver-colored antibacterial powder
CN109349272A (en) * 2018-10-09 2019-02-19 湘潭大学 A kind of preparation method of sepiolite supported Chitosan-Silver antibacterial powder
CN111357765A (en) * 2020-03-17 2020-07-03 长沙天源羲王材料科技有限公司 Preparation method of water-oil universal nano-silver antibacterial agent for antibacterial coating
CN111357765B (en) * 2020-03-17 2021-07-09 长沙天源羲王材料科技有限公司 Preparation method of water-oil universal nano-silver antibacterial agent for antibacterial coating
CN112006031A (en) * 2020-08-25 2020-12-01 广东欧文莱陶瓷有限公司 Antibacterial agent for ceramics, antibacterial ceramics and preparation method thereof
CN112006031B (en) * 2020-08-25 2021-09-14 广东欧文莱陶瓷有限公司 Antibacterial agent for ceramics, antibacterial ceramics and preparation method thereof

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Inventor after: Liu Pingle

Inventor after: Yang Jingyuan

Inventor after: Wu Shengdao

Inventor after: Hao Fang

Inventor after: Xiong Wei

Inventor after: Xiong Shaofeng

Inventor after: Luo Hean

Inventor after: Tan Jianjie

Inventor after: Chai Bin

Inventor after: Guo Yinglong

Inventor before: Liu Pingle

Inventor before: Wu Shengdao

Inventor before: Hao Fang

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Application publication date: 20161123