CN101044862A - Nanometer bentonite bactericidal materials, and its preparing method and application - Google Patents
Nanometer bentonite bactericidal materials, and its preparing method and application Download PDFInfo
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- CN101044862A CN101044862A CN 200610148306 CN200610148306A CN101044862A CN 101044862 A CN101044862 A CN 101044862A CN 200610148306 CN200610148306 CN 200610148306 CN 200610148306 A CN200610148306 A CN 200610148306A CN 101044862 A CN101044862 A CN 101044862A
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Abstract
An antibacterial nano-bentone material used for paint is prepared from the Ca-base bentone nanoparticles (70-99 Wt%) and RE ions (1-30) chosen from La, Ce, Pr, Nd, Sm, Eu, Y and Er through mechanically stirring said bentone, acidifying to become nanoparticles, and carrying RE ions.
Description
Technical field
The invention belongs to material technology field and depollution of environment field, particularly relating to a kind of is the preparation method and the application of the nano anti-biotic material of raw material with the bentonite raw ore.
Background technology
General anti-biotic material can be divided into according to forming: inorganic antibacterial material, organic anti-bacterial material and natural antibacterial material three parts, and natural antibacterial material is mainly the extract of natural plants, is subjected to the restriction of resource, and application has certain difficulty; The applicating history of organic anti-bacterial material existing three more than ten years though its sterilizing power is strong, effective, exists that safety is relatively poor, chemical stability is bad, poor heat resistance, easily produces drug resistance and can cause secondary pollution problems; Inorganic antibacterial material is generally by containing metal cation components such as silver, zinc, copper and inorganic carrier and form, play antibacterial effect by slow releasing function, have advantages such as safety, warm tolerance, persistence, but common antibacterial agent product form often is in a kind of nature of anti-biotic material at present, be generally the powder of conventional particle diameter, Powdered crystallite or liquid, do not reach nanoscale.In theory, the antibacterial agent of nano-scale can make the active easier bacterium inside that enters mutually, make the membranolysis of bacterium, and kill effectively and suppress bacterium, simultaneously, the bulk effect of nano particle uniqueness can improve active distribution consistency degree mutually greatly with surface-area effects, and the contact surface that increases itself and bacterium is long-pending, thereby further improves antimicrobial efficiency; Utilize the quantum size effect of nano particle and macro quanta tunnel effect etc. can improve its electronics and level structure characteristic, improve antibacterial ability.
Nano material is applied in the industrial production as anti-biotic material, also there are two problems at present, one be nano antibacterial agent preparation technology complicated, mostly reunite more serious, another be exactly the nano antibacterial agent relative cost than higher, cause can not get good application.
Summary of the invention
Technical problem to be solved
Technical problem to be solved by this invention provides a kind of nanometer bentonite bactericidal materials and its production and application, inhomogeneous to overcome existing nano anti-biotic material particle size, bad dispersibility, specific surface area influence that antibacterial effect, manufacturing price are higher, complex process, viscosity is low and the defective of easy reunion.
Technical scheme
One of technical scheme of the present invention provides a kind of nanometer bentonite bactericidal materials, particle diameter is 10～100 nanometers, form by rare earth ion and bentonite nano particle, its content is: rare earth ion 1～30%wt and bentonite nano particle 70%～99%wt, wherein, bentonite is a calcium-base bentonite, and rare earth ion is selected from La
3+, Ce
3+, Pr
3+, Nd
3+, Sm
3+, Eu
3+, Y
3+Or Er
3+In one or more.
Two of technical scheme of the present invention provides a kind of preparation method of above-mentioned nanometer bentonite bactericidal materials, comprises the steps:
(1) bentonite material adds the remodeling agent, stirs 0.5～1h processing of retrofiting;
(2) add the alkaline activation agent, fully stir 1～2h activation processing;
(3) 95 ℃～98 ℃ heating acidifying 3～4h, suction filtration, spend deionised water to pH be 6～7.
(4) with the bentonite filter cake dissolving that obtains, high-speed stirred 1～3h, centrifugal treating 10～30min under 1000～4000r/min makes nano-bentonite liquid;
(5) with nano-bentonite liquid 60～90 ℃ of vacuum dryings 5～8 hours, grind, it is standby to obtain nano-bentonite;
(6) the rare earth ion villaumite RECl of preparation 0.1～0.5mol/L
3XH
2The deionized water solution of O adds above-mentioned nano-bentonite, stirring reaction 1～4h;
(7) suction filtration washs 3～4 times, 60～90 ℃ of vacuum dryings 6～9 hours, grinds, and promptly obtains said nanometer bentonite bactericidal materials;
Wherein, bentonite is a calcium-base bentonite, and rare earth ion is selected from La
3+, Ce
3+, Pr
3+, Nd
3+, Sm
3+, Eu
3+, Y
3+Or Er
3+In one or more.
One of preferred version of the preparation method of above-mentioned nanometer bentonite bactericidal materials is that said remodeling agent is sodium carbonate or lithium carbonate.
Two of the preparation method's of above-mentioned nanometer bentonite bactericidal materials preferred version is that said alkaline activation agent is sodium hydroxide or sodium carbonate.
Three of the preparation method's of above-mentioned nanometer bentonite bactericidal materials preferred version is that the said mixing speed of step (4) is 600～1300r/min.
Five of the preparation method's of above-mentioned nanometer bentonite bactericidal materials preferred version is that the raw material proportioning that adopts in said step (1) and (2) comprises following component at least:
Bentonite raw ore 30～96%wt
Remodeling agent 0.5～10%wt
Alkaline activation agent 0～10%wt
Water
Three of technical scheme of the present invention provides a kind of nanometer bentonite bactericidal agent, and its composition is above-mentioned nanometer bentonite bactericidal materials and excipient.
The preferred version of above-mentioned nanometer bentonite bactericidal agent is that the sensitive bacteria of said antibacterial agent is Escherichia coli, staphylococcus aureus, bacillus wax, Bacillus megatherium or Candida albicans.
Beneficial effect
The nano anti-biotic material that makes of the present invention under the same conditions gained the nano particle diameter size evenly, better dispersed, because the particle diameter of this material is a nanoscale, so bigger surface area is arranged, antibacterial effect is obvious.
2. compare with general anti-biotic material cheap, raw material of the nano anti-biotic material that makes of the present invention is easy to get, and technology is simple, is suitable for industrial a large amount of production.
3. the sensitive bacteria of the nano anti-biotic material that makes of the present invention spectrum is wider, comprises important human pathogens such as Escherichia coli, staphylococcus aureus, bacillus wax, Bacillus megatherium, Candida albicans.
4. the nano anti-biotic material that makes of the present invention belongs to clay material, has good viscosity, and the particle-stabilised difficult reunion of nano-bentonite can be used for coating additive; Small particle diameter also helps preparing various antimicrobial products, as antibiotic paint, antibiotic paper product, antibiotic plastic etc.
Description of drawings
Fig. 1 is the transmission photo of nanometer bentonite bactericidal materials, and multiplication factor is 50,000 times.
Fig. 2 is the nanometer bentonite bactericidal agent that makes according to the embodiment 1 antibacterial photo to staphylococcus aureus:
1. nano-bentonite carries LaCl
3
2. nano-bentonite carries YCl
3
Fig. 3 is the nanometer bentonite bactericidal agent that makes according to the embodiment 1 antibacterial photo to colibacillus:
1. nano-bentonite carries LaCl
3
2. nano-bentonite carries PrCl
3
3. nano-bentonite carries NdCl
3
4. nano-bentonite carries CeCl
3
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, as the chemical products handbook, or the condition of advising according to manufacturer.Wherein used bacterial classification: Escherichia coli (8099), staphylococcus aureus (ATCC6538P), bacillus wax, Bacillus megatherium and Candida albicans are provided by Shanghai Pharmaceutical Inst., Chinese Academy of Sciences.All inorganic chemical reagents and organic solvent are available from Shanghai chemical reagent factory.
Take by weighing bentonite raw ore 15g and add the remodeling agent, add the processing of retrofiting of 0.5g sodium carbonate, stirring adds alkaline activation agent sodium hydroxide 1g half an hour, fully stirs the 60min activation processing, 98 ℃ of water-baths heating acidifying 3～4h, suction filtration, spending deionised water is 6 to pH, and with above-mentioned bentonite filter cake dissolving, high speed electric stirs 1h, centrifugal treating 20min under 1000r/min makes nano-bentonite liquid; Nano-bentonite liquid is ground after 6 hours 85 ℃ of vacuum dryings standby, the preparation 0.3mol/L RECl
3XH
2The deionized water solution of O adds an amount of above-mentioned nano-bentonite that makes, stirring reaction 2h, and suction filtration washs 3～4 times, grinds after 6 hours 80 ℃ of vacuum dryings, preserves.
Annotate: RE is selected from rare earth ion La
3+, Ce
3+, Pr
3+, Nd
3+, Sm
3+, Eu
3+, Y
3+Or Er
3+In one or more, such as rare earth La
3+And Ce
3+, Pr
3+And Nd
3+And Sm
3+, Eu
3+And Er
3+And Y
3+, Ce
3+And Sm
3+And Eu
3+And Er
3+And Y
3+, even 8 kinds of rare earth elements is whole, n kind RECl
3XH
2When O was raw material, with total mol number calculating raw material input amount of each rare earth villaumite, its reaction condition was identical with the single rare earth villaumite with process.
Embodiment 2
Take by weighing bentonite raw ore 20g and add the remodeling agent, add the processing of retrofiting of 1g sodium carbonate, stirring adds alkaline activation agent sodium hydroxide 1.5g half an hour, fully stirs the 60min activation processing, 95 ℃ of water-baths heating acidifying 3～4h, suction filtration, spending deionised water is 6 to pH, and with above-mentioned bentonite filter cake dissolving, high speed electric stirs 1h, centrifugal treating 25min under 1500r/min makes nano-bentonite liquid; Nano-bentonite liquid is ground after 6 hours 80 ℃ of vacuum dryings standby, the preparation 0.3mol/L RECl
3XH
2The deionized water solution of O adds an amount of above-mentioned nano-bentonite that makes, stirring reaction 2h, and suction filtration washs 3～4 times, grinds after 5 hours 90 ℃ of vacuum dryings, preserves.
Annotate: RE is selected from rare earth ion La
3+, Ce
3+, Pr
3+, Nd
3+, Sm
3+, Eu
3+, Y
3+Or Er
3+In one or more, such as rare earth La
3+And Ce
3+, Pr
3+And Nd
3+And Sm
3+, Eu
3+And Er
3+And Y
3+, Ce
3+And Sm
3+And Eu
3+And Er
3+And Y
3+, even 8 kinds of rare earth elements is whole, n kind RECl
3XH
2When O was raw material, with total mol number calculating raw material input amount of each rare earth villaumite, its reaction condition was identical with the single rare earth villaumite with process.
Take by weighing bentonite raw ore 30g and add the remodeling agent, add the processing of retrofiting of 1.5g sodium carbonate, stirring adds alkaline activation agent sodium hydroxide 2g half an hour, fully stirs the 60min activation processing, 98 ℃ of water-baths heating acidifying 3～4h, suction filtration, spending deionised water is 6 to pH, and with above-mentioned bentonite filter cake dissolving, high speed electric stirs 1h, centrifugal treating 20min under 1200r/min makes nano-bentonite liquid; Nano-bentonite liquid is ground after 7 hours 75 ℃ of vacuum dryings standby, the preparation 0.4mol/L RECl
3XH
2The deionized water solution of O adds an amount of above-mentioned nano-bentonite that makes, stirring reaction 2h, and suction filtration washs 3～4 times, grinds after 7 hours 70 ℃ of vacuum dryings, preserves.
Annotate: RE is selected from rare earth ion La
3+, Ce
3+, Pr
3+, Nd
3+, Sm
3+, Eu
3+, Y
3+Or Er
3+In one or more, such as rare earth La
3+And Ce
3+, Pr
3+And Nd
3+And Sm
3+, Eu
3+And Er
3+And Y
3+, Ce
3+And Sm
3+And Eu
3+And Er
3+And Y
3+, even 8 kinds of rare earth elements is whole, n kind RECl
3XH
2When O was raw material, with total mol number calculating raw material input amount of each rare earth villaumite, its reaction condition was identical with the single rare earth villaumite with process.
Embodiment 4
The nanometer bentonite bactericidal materials that Application Example 1-4 makes is cultivated altogether with pathogenic bacteria Escherichia coli, staphylococcus aureus, bacillus wax, Bacillus megatherium and Candida albicans respectively, carries out the experiment of inhibition zone and minimal inhibitory concentration; The result shows certain anti-microbial property, and minimum inhibition zone photo is seen accompanying drawing; The minimal inhibitory concentration experimental result is 500～700mg/L (minimal inhibitory concentration of People's Republic of China's chemical industry standard code compound can be used as antibacterial agent less than 800mg/L and uses, and the more for a short time antibacterial effect that shows of this value is good more).
Claims (8)
1. nanometer bentonite bactericidal materials, particle diameter is 10～100 nanometers, is made up of rare earth ion and bentonite nano particle, its content is: rare earth ion 1～30%wt and swelling scholar nano particle 70%～99%wt, wherein, bentonite is a calcium-base bentonite, and rare earth ion is selected from La
3+, Ce
3+, Pr
3+, Nd
3+, Sm
3+, Eu
3+, Y
3+Or Er
3+In one or more.
2. the preparation method of nanometer bentonite bactericidal materials according to claim 1 comprises the steps:
(1) bentonite material adds the remodeling agent, stirs 0.5～1h processing of retrofiting;
(2) add the alkaline activation agent, fully stir 1～2h activation processing;
(3) 95 ℃～98 ℃ heating acidifying 3～4h, suction filtration, spend deionised water to pH be 6～7.
(4) with the bentonite filter cake dissolving that obtains, high-speed stirred 1～3h, centrifugal treating 10～30min under 1000～4000r/min makes nano-bentonite liquid;
(5) with nano-bentonite liquid 60～90 ℃ of vacuum dryings 5～8 hours, grind, it is standby to obtain nano-bentonite;
(6) the rare earth ion villaumite RECl of preparation 0.1～0.5mol/L
3XH
2The deionized water solution of O adds above-mentioned nano-bentonite, stirring reaction 1～4h;
(7) suction filtration washs 3～4 times, 60～90 ℃ of vacuum dryings 6～9 hours, grinds, and promptly obtains said nanometer bentonite bactericidal materials;
Wherein, bentonite is a calcium-base bentonite, and rare earth ion is selected from La
3+, Ce
3+, Pr
3+, Nd
3+, Sm
3+, Eu
3+, Y
3+Or Er
3+In one or more.
3. the preparation method of nanometer bentonite bactericidal materials according to claim 2 is characterized in that, said remodeling agent is sodium carbonate or lithium carbonate.
4. the preparation method of nanometer bentonite bactericidal materials according to claim 2 is characterized in that, said alkaline activation agent is sodium hydroxide or sodium carbonate.
5. the preparation method of nanometer bentonite bactericidal materials according to claim 2 is characterized in that, the said mixing speed of step (4) is 600～1300r/min.
6. the preparation method of nanometer bentonite bactericidal materials according to claim 2 is characterized in that, the raw material proportioning that adopts in said step (1) and (2) comprises following component at least:
Bentonite raw ore 30～96%wt
Remodeling agent 0.5～10%wt
Alkaline activation agent 0～10%wt
Water.
7. nanometer bentonite bactericidal agent, its composition are described nanometer bentonite bactericidal materials of claim 1 and excipient.
8. nanometer bentonite bactericidal agent according to claim 7 is characterized in that, the sensitive bacteria of said antibacterial agent is Escherichia coli, staphylococcus aureus, bacillus wax, Bacillus megatherium or Candida albicans.
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|---|---|---|---|
| CN 200610148306 CN101044862A (en) | 2006-12-29 | 2006-12-29 | Nanometer bentonite bactericidal materials, and its preparing method and application |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610148306 CN101044862A (en) | 2006-12-29 | 2006-12-29 | Nanometer bentonite bactericidal materials, and its preparing method and application |
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| CN101044862A true CN101044862A (en) | 2007-10-03 |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103947674A (en) * | 2013-11-28 | 2014-07-30 | 龙岩学院 | Rare earth-salicylic acid-montmorillonite nanometer composite antiseptic and preparation method thereof |
| CN112661165A (en) * | 2020-12-10 | 2021-04-16 | 北京机械力化学研究院有限公司 | High-energy grinding preparation of rare earth-loaded bentonite and preparation method thereof |
| CN112705181A (en) * | 2020-12-10 | 2021-04-27 | 北京机械力化学研究院有限公司 | Preparation method for preparing unsteady-state rare earth bentonite by high-energy grinding |
| CN113337012A (en) * | 2021-05-28 | 2021-09-03 | 北京联飞翔科技股份有限公司 | Composite antibacterial agent, antibacterial master batch containing composite antibacterial agent and preparation method of antibacterial master batch |
-
2006
- 2006-12-29 CN CN 200610148306 patent/CN101044862A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103947674A (en) * | 2013-11-28 | 2014-07-30 | 龙岩学院 | Rare earth-salicylic acid-montmorillonite nanometer composite antiseptic and preparation method thereof |
| CN103947674B (en) * | 2013-11-28 | 2017-07-11 | 龙岩学院 | The rare earth complexes with salicylic acid montmorillonite-based nano complex antimicrobials and preparation method thereof |
| CN112661165A (en) * | 2020-12-10 | 2021-04-16 | 北京机械力化学研究院有限公司 | High-energy grinding preparation of rare earth-loaded bentonite and preparation method thereof |
| CN112705181A (en) * | 2020-12-10 | 2021-04-27 | 北京机械力化学研究院有限公司 | Preparation method for preparing unsteady-state rare earth bentonite by high-energy grinding |
| CN113337012A (en) * | 2021-05-28 | 2021-09-03 | 北京联飞翔科技股份有限公司 | Composite antibacterial agent, antibacterial master batch containing composite antibacterial agent and preparation method of antibacterial master batch |
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