CN106665651A - Preparation method of stable sepiolite antibacterial powder - Google Patents
Preparation method of stable sepiolite antibacterial powder Download PDFInfo
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- CN106665651A CN106665651A CN201710018614.6A CN201710018614A CN106665651A CN 106665651 A CN106665651 A CN 106665651A CN 201710018614 A CN201710018614 A CN 201710018614A CN 106665651 A CN106665651 A CN 106665651A
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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
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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
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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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- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
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- Environmental Sciences (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a preparation method of stable sepiolite antibacterial powder. The preparation method comprises the following steps: activating of sepiolite, antibacterial treatment of the sepiolite, silica coating and the like. According to the preparation method disclosed by the invention, acid and a surfactant are respectively adopted for modifying the sepiolite, so that the specific surface area of an antibacterial material can be increased, and the adsorption quantity of a carrier on silver ions, chitosan and the like is further increased; simple physical adsorption is changed into chemical adsorption, so that release of silver is slowed down, and the long-time antibacterial effect is kept; after the modified sepiolite is utilized for adsorbing nano silver and the chitosan, drying treatment and milling are carried out, antibacterial powder is dispersed into a water solution or an organic solvent, silicon compounds and catalysts are added for carrying out coating reaction, the stability of the obtained antibacterial powder is remarkably increased, and not only can antibacterial broad spectrum be still ensured under severe environment of acid, base, organism, strong ultraviolet radiation and the like, but also the release of antibacterial active components can be slowed down by coating one layer of SiO2, so that the service life of the stable sepiolite antibacterial powder is prolonged.
Description
Technical field
The invention belongs to field of material preparation, more particularly to a kind of preparation method of stable meerschaum antibacterial powder.
Background technology
In today of scientific and technological high speed development, how how to better control over and eliminate harmful microbe growth and breed
It is more effectively carried out antibacterial, sterilization, sterilization and diseases prevention and treatment, it has also become one closely bound up with human health and life to ask
Topic.It is contemplated that, the development ＆ production of efficient and long-acting stable antibacterial product will be Chinese national economy development service,
To improve the people's livelihood, quality contributes, and is to improve the very positive effect of China's economic benefit and social benefit performance.
Currently, inorganic antiseptic with respect to organic antibacterial agent have the advantages that more preferable heat-resisting quantity, safety avirulence and
Favored by people.The selection for being concentrated mainly on carrier of presently relevant document report, the preparation of antibiotic effective ingredient and
On carrying method, and the report for being processed further processing prepared to antibacterial powder after completing is few.
Li Feng (200610035616.0) the anti-settling wax liquors of polyethylene are that carrier loaded nanometer silver prepares antibacterial powder.Hu Guoqing
Adsorb shitosan or silver with clay or zirconium phosphate to prepare antibacterial powder Deng (02111595.8).Chengdu University of Technology Liu Jing etc.
(CN101142919) invention with meerschaum as carrier, load silver and zinc ion prepare antibacterial powder.Although their preparation process compared with
For simple, but in acid, under alkali or the actual environment such as organic, antimicrobial component be easily decomposed or discharge earlier so as to
Its service life is shortened, is unfavorable for being applied to the fields such as construction material, medical facilities and medical apparatus and instruments, articles for daily use.
The content of the invention
Present invention aims to above-mentioned prior art is not enough to provide a kind of preparation side of stable meerschaum antibacterial powder
Method.
The technical scheme is that：
A kind of preparation method of stable meerschaum antibacterial powder, including the coated with silica of meerschaum.
Further, the coated with silica of described meerschaum is：Meerschaum is pressed into solid-to-liquid ratio（Mass ratio）For 1:10~
20 are added in the mixed solution of silicon class compound, catalyst and solvent, 10 ~ 65 DEG C of 80 ~ 150min of reaction, filter, wash, do
It is dry to obtain product.
Further, in mixed solution, the mol ratio of silicon class compound, catalyst and solvent is 0.002 ~ 0.007：
0.008~0.016：0.65~0.95.
Further, described silicon class compound is the silicic acid such as tetraethyl orthosilicate, positive quanmethyl silicate, tetraethyl orthosilicate
The silicate such as ester, sodium silicate, potassium silicate, waterglass, MTES, ethyl triethoxysilane, the ethoxy of phenyl three
One kind in base silane, VTES and their methoxyl group and chlorosilane.
Further, described catalyst is ammonia, ethylenediamine, triethylamine, sulphuric acid, nitric acid, hydrochloric acid, acetic acid, oxalic acid, first
One kind in acid, benzenesulfonic acid, sodium borohydride.
Further, described solvent is the one kind in water, methanol, ethanol, acetone, toluene, dimethylformamide.
Further, the antimicrobial treatment before also coating including meerschaum, specially：Meerschaum after activation and 0.01 ~
The aqueous solution of the Antibacterial Constituents of 0.5mol/L, 10 ~ 85 DEG C of 1 ~ 72 h of stirring, filters, washs, and is then dried and carries out
Barreling.
Further, the aqueous solution of described Antibacterial Constituents is silver nitrate solution, and silver-colored ammonium complex liquid, silver oxalate are molten
One or more in liquid, silver acetate solution, Itrol. solution and shitosan.
Further, also including the activation of the meerschaum before antimicrobial treatment, the activation of meerschaum includes that the acid of meerschaum is living
Change and organic active.
Further, the activation of meerschaum is specially：Under the conditions of 25 ~ 125 DEG C, by solid-to-liquid ratio 1:10 ~ 20 in meerschaum
The acid solution for adding 0.2 ~ 5mol/L activates 2 ~ 12h, washing and filtering to neutrality, by solid-to-liquid ratio 1:10 ~ 30 acid activation Hai Pao
Organic solvent and water are added in stone, the concentration for controlling organic solvent is 0.004 ~ 0.1g/mL, and at 25 ~ 85 DEG C 2 ~ 20h is impregnated, and is taken out
Filter and with absolute ethanol washing 2 ~ 5 times, is dried and barreling, obtains Activated Sepiolite.
Further, described acid is the one kind in hydrochloric acid, nitric acid, sulphuric acid, oxalic acid.
Further, described organic solvent is cetyl trimethylammonium bromide (CTAB), dodecylbenzene sodium sulfonate
(SDBS), in sodium lauryl sulphate (SDS) one or more, more preferably cetyl trimethylammonium bromide
(SDBS）.
The beneficial effects of the present invention is：
（1）The present invention is modified respectively with surfactant using acid to meerschaum, can improve the specific surface area of anti-biotic material,
Further increase carrier to adsorbances such as silver ion, shitosans, and become chemisorbed from simple physical absorption, so
The release of silver can be slowed down, long-time antibacterial effect is kept.
（2）After the present invention is using modified meerschaum absorption nanometer silver and shitosan, dried, grinding, antibacterial
Powder is scattered in aqueous solution or organic solvent, and adds silicon class compound and catalyst to carry out coating reaction, the antibacterial for obtaining
Powder stability is significantly improved, can not only be organic in acid, alkali, and under the adverse circumstances such as strong ultra-vioket radiation broad-spectrum antibacterial property is still ensured that,
And one layer of SiO of cladding2The release of Antibacterial Constituents can also be slowed down, so as to extend its service life.
Specific embodiment
The present invention is described in further details with reference to specific embodiment, but the present invention is not limited to this.
Embodiment 1
（1）Meerschaum is activated：Under the conditions of 75 DEG C, meerschaum is 1 by solid-to-liquid ratio:15 carry out 0.75mol/L hydrochloric acid activation 10h, wash
Filtration is washed to neutrality, is 1 by solid-to-liquid ratio:15,0.05mol/L dodecylbenzene sodium sulfonate (SDBS) is added, under the conditions of 30 DEG C
Dipping 18h, sucking filtration and with absolute ethanol washing 3 times, drying, barreling is standby, prepared Activated Sepiolite；
（2）The Activated Sepiolite obtained in step (1) is added to into the AgNO of 0.1mol/L3In solution, 36h is stirred at room temperature, makes two
Person fully combines, and filters, and distilled water wash is dried to existing without Ag ions, and barreling is standby；
（3）It is 1 by solid-to-liquid ratio to take the antibacterial powder that step (2) obtains:15 are added in tetraethyl orthosilicate and vinegar aqueous acid, its
In, the mol ratio of water, tetraethyl orthosilicate and acetic acid is 0.833：0.005：0.009,90min is reacted under room temperature condition, filter, wash
Wash, be dried to obtain product；
（4）It is 1 by solid-to-liquid ratio to take the powder body that step (2) and (3) obtain:15 are added separately to 1mol/L HCl（Acid treatment）Or
1mol/L NaOH（Alkali process）Or dehydrated alcohol（Organic process）In, filter after 24h, wash, be dried to obtain product.
（5）The powder body ultra violet lamp 24h that step (2) and (3) obtain is taken respectively（Ultraviolet process）.
（6）By step（2）, step（3）The antibacterial powder for obtaining and step (4) and (5) process the antibacterial powder for obtaining and press respectively
In being placed in containing staphylococcus aureuses, escherichia coli, the Solid agar culture of Candida albicans into drug sheet, in 37 DEG C of bars
24h is cultivated under part.
Step（2）、（3）Gained antibacterial powder（Correspond respectively to coated with silica forward and backward）Inhibition zone be 5.1mm.
Without coated Si O2Antibacterial powder after acid, alkali, organic, ultraviolet process, inhibition zone difference 4.2mm, 3.8mm, 3.7mm,
4.6mm.Coated Si O2Inhibition zone of the antibacterial powder after acid, alkali, organic, ultraviolet process be respectively 4.9 mm, 4.5mm,
4.6mm, 4.9mm。
Result above shows, uncoated SiO2SiO is relatively coated2Antibacterial powder after acid, alkali, organic, ultraviolet process,
Inhibition zone reduces respectively 0.7mm, 0.7mm, 0.9mm, 0.3mm, and this is absolutely proved, although coated with silica could not be direct
Fungistatic effect is improved, antibacterial powder stability in the presence of a harsh environment has but been obviously improved.
Embodiment 2
（1）Meerschaum is activated：Under the conditions of 65 DEG C, meerschaum is 1 by solid-to-liquid ratio:15 carry out 1mol/L nitric acid activation 10h, washed
Filter to neutrality, be 1 by solid-to-liquid ratio:25,0.02mol/L dodecylbenzene sodium sulfonate (SDBS) is added, impregnate under the conditions of 30 DEG C
20h, sucking filtration and with absolute ethanol washing 3 times is dried, and barreling is standby, and Activated Sepiolite is obtained；
（2）The Activated Sepiolite obtained in step (1) is added separately in the chitosan solution of 0.09mol/L, is stirred at room temperature
24h, makes both fully combine, and filters, and is dried, and barreling is standby；
（3）It is 1 by solid-to-liquid ratio to take the antibacterial powder that step (2) obtains:15 are added in sodium silicate and salt aqueous acid, wherein,
The mol ratio of water, sodium silicate and hydrochloric acid is 0.733：0.010：0.011,90min is reacted under room temperature condition, filter, wash, be dried
Obtain product.
（4）It is 1 by solid-to-liquid ratio to take the powder body that step (2) and (3) obtain respectively:15 are added separately to 1mol/L HCl（Acid
Process）Or 1mol/L NaOH（Alkali process）Or dehydrated alcohol（Organic process）In, filter after 24h, wash, being dried to obtain product
Thing.
（5）The powder body ultra violet lamp 24h that step (2) and (3) obtain is taken respectively（Ultraviolet process）.
（6）Step（2）, step（3）The antibacterial powder for obtaining and step (4) and (5) process the antibacterial powder for obtaining and are pressed into respectively
During drug sheet is placed in containing staphylococcus aureuses, escherichia coli, the Solid agar culture of Candida albicans, in 37 DEG C of conditions
Lower culture 24h.
Step（2）、（3）The inhibition zone of gained antibacterial powder is 5.9mm.Without coated Si O2Antibacterial powder through acid, alkali,
After organic, ultraviolet process, inhibition zone difference 3.9mm, 3.8mm, 4.1mm, 4.5mm.Coated Si O2Antibacterial powder through acid,
Inhibition zone after alkali, organic, ultraviolet process is respectively 4.5 mm, 4.7mm, 4.6mm, 5.3mm.
Result above shows, uncoated SiO2SiO is relatively coated2Antibacterial powder after acid, alkali, organic, ultraviolet process,
Inhibition zone reduces respectively 0.6mm, 0.9mm, 0.5mm, 0.8mm, and this is absolutely proved, coated with silica has been obviously improved anti-
Mycopowder stability in the presence of a harsh environment, so as to increase the service life.
Claims (10)
1. a kind of preparation method of stable meerschaum antibacterial powder, it is characterised in that including the coated with silica of meerschaum.
2. the preparation method of stable meerschaum antibacterial powder according to claim 1, it is characterised in that described meerschaum
Coated with silica is：It is 1 that meerschaum is pressed into solid-to-liquid ratio:10 ~ 20 be added to silicon class compound, catalyst and solvent mixing it is molten
In liquid, 10 ~ 65 DEG C of 80 ~ 150min of reaction are filtered, wash, are dried to obtain product.
3. the preparation method of stable meerschaum antibacterial powder according to claim 2, it is characterised in that in mixed solution, silicon
The mol ratio of class compound, catalyst and solvent is 0.002 ~ 0.007：0.008~0.016：0.65~0.95.
4. the preparation method of stable meerschaum antibacterial powder according to claim 2, it is characterised in that described silicon class chemical combination
Thing is tetraethyl orthosilicate, positive quanmethyl silicate, tetraethyl orthosilicate, sodium silicate, potassium silicate, MTES, ethyl
One kind in triethoxysilane, phenyl triethoxysilane, VTES；Described catalyst be ammonia,
One kind in ethylenediamine, triethylamine, sulphuric acid, nitric acid, hydrochloric acid, acetic acid, oxalic acid, formic acid, benzenesulfonic acid, sodium borohydride；Described is molten
Agent is the one kind in water, methanol, ethanol, acetone, toluene, dimethylformamide.
5. the preparation method of stable meerschaum antibacterial powder according to claim 1, it is characterised in that also including meerschaum bag
Antimicrobial treatment before covering, specially：The aqueous solution of the Antibacterial Constituents of meerschaum and 0.01 ~ 0.5mol/L after activation is mixed
Close, 10 ~ 85 DEG C of 1 ~ 72 h of stirring are filtered, washed, and are then dried and carry out barreling.
6. the preparation method of stable meerschaum antibacterial powder according to claim 5, it is characterised in that described antibacterial activity
The aqueous solution of composition be silver nitrate solution, silver-colored ammonium complex liquid, silver oxalate solution, silver acetate solution, Itrol. solution and shell
One or more in polysaccharide.
7. the preparation method of stable meerschaum antibacterial powder according to claim 5, it is characterised in that also including antimicrobial treatment
The activation of front meerschaum, described meerschaum activation includes acid activation and the organic active of meerschaum.
8. the preparation method of stable meerschaum antibacterial powder according to claim 7, it is characterised in that the activation tool of meerschaum
Body is：Under the conditions of 25 ~ 125 DEG C, by solid-to-liquid ratio 1:10 ~ 20 add the acid solution of 0.2 ~ 5mol/L to activate 2 ~ 12h in meerschaum,
Washing and filtering to neutrality, by solid-to-liquid ratio 1:10 ~ 30 add organic solvent and water in the meerschaum of acid activation, control organic solvent
Concentration be 0.004 ~ 0.1g/mL, impregnate 2 ~ 20h at 25 ~ 85 DEG C, sucking filtration and with absolute ethanol washing 2 ~ 5 times, drying is simultaneously ground
Grind, obtain Activated Sepiolite.
9. the preparation method of stable meerschaum antibacterial powder according to claim 8, it is characterised in that described acid is salt
One kind in acid, nitric acid, sulphuric acid, oxalic acid.
10. the preparation method of stable meerschaum antibacterial powder according to claim 8, it is characterised in that described is organic molten
Agent is one or more in cetyl trimethylammonium bromide, dodecylbenzene sodium sulfonate, sodium lauryl sulphate.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108991014A (en) * | 2018-07-19 | 2018-12-14 | 湘潭大学 | A kind of preparation method of sepiolite supported chitosan-zinc antibacterial powder |
| 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 |
| CN109527077A (en) * | 2018-12-27 | 2019-03-29 | 湘潭大学 | A kind of method that sepiolite/essential oil composite material prevents and treats rod method after grape harvest |
| CN109593210A (en) * | 2018-12-13 | 2019-04-09 | 青岛理工大学 | Antifouling antibacterial sand of one kind and preparation method thereof |
| 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 |
| CN111603605A (en) * | 2020-06-22 | 2020-09-01 | 湘潭大学 | Inorganic rapid hemostatic material and preparation method thereof |
| 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 |
| CN112920491A (en) * | 2021-01-30 | 2021-06-08 | 杨辉 | Preparation method of EPE environment-friendly packaging material |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108991014A (en) * | 2018-07-19 | 2018-12-14 | 湘潭大学 | A kind of preparation method of sepiolite supported chitosan-zinc antibacterial powder |
| 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 |
| CN109593210B (en) * | 2018-12-13 | 2021-07-06 | 青岛理工大学 | Antifouling bacteriostatic sand and preparation method thereof |
| CN109593210A (en) * | 2018-12-13 | 2019-04-09 | 青岛理工大学 | Antifouling antibacterial sand of one kind and preparation method thereof |
| CN109527077A (en) * | 2018-12-27 | 2019-03-29 | 湘潭大学 | A kind of method that sepiolite/essential oil composite material prevents and treats rod method after grape harvest |
| 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 |
| CN111603605A (en) * | 2020-06-22 | 2020-09-01 | 湘潭大学 | Inorganic rapid hemostatic material and preparation method thereof |
| CN111603605B (en) * | 2020-06-22 | 2022-06-21 | 湘潭大学 | Inorganic rapid hemostatic material and preparation method thereof |
| 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 |
| CN112920491A (en) * | 2021-01-30 | 2021-06-08 | 杨辉 | Preparation method of EPE environment-friendly packaging material |
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Inventor after: Liu Pingle Inventor after: Wu Shengdao Inventor after: Hao Fang Inventor after: Xiong Wei Inventor after: Xiong Shaofeng Inventor after: Tan Jianjie Inventor after: Liu Pingle, Wu Shengtao, Hao Fangxiongwei, Xiong Shaofeng, Tan Jianjie, Ouyang Donghong, Ceng Zhaogang, Peng Shaolian Inventor after: Zeng Zhaogang Inventor after: Peng Shaolian Inventor before: Liu Pingle Inventor before: Wu Shengdao Inventor before: Hao Fang Inventor before: Xiong Wei Inventor before: Xiong Shaofeng |
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| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20170912 Address after: Donkey pond in Hunan province Xiangtan city 411105 District No. 27 Applicant after: Xiangtan University Applicant after: XIANGTAN YUANHAI SEPIOLITE NEW MATERIAL CO., LTD. Address before: Donkey pond in Hunan province Xiangtan city 411105 District No. 27 Applicant before: Xiangtan University |
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| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170517 |