CN103305063A - Preparation method for curdlan-nano-copper compound antibacterial gel - Google Patents
Preparation method for curdlan-nano-copper compound antibacterial gel Download PDFInfo
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- CN103305063A CN103305063A CN2013102070409A CN201310207040A CN103305063A CN 103305063 A CN103305063 A CN 103305063A CN 2013102070409 A CN2013102070409 A CN 2013102070409A CN 201310207040 A CN201310207040 A CN 201310207040A CN 103305063 A CN103305063 A CN 103305063A
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Abstract
The invention belongs to the field of compound antibacterial materials, and provides a preparation method for a curdlan-nano-copper compound antibacterial gel. According to the method, a suspension is formed by dispersing curdlan in water, and curdlan heated can form a three-dimensional helical structure, so that the structure can fix nano-copper, thereby slowing down particle aggregation and delaying oxidation. Therefore, the antibacterial capacity of nano-copper is further exerted. The preparation method comprises the following steps: (1) preparation of a potassium borohydride liquor; (2) preparation of a nano-copper sol; (3) preparation of a curdlan suspension; (4) preparation of the curdlan-nano-copper compound antibacterial gel. The antibacterial gel prepared by the method is sealed by oil at normal temperature, and nano-copper particles still have better antibacterial effect after the gel is placed four 2 months. The preparation process is simple and the production cost is low, so that the gel is suitable for large-scale production.
Description
Technical field
The invention belongs to the composite antibacterial material field, relate to the preparation method of a kind of curdlan-Nanometer Copper composite antibiosis colloid.
Background technology
Before thousands of years, the alloy of copper (bronze) has been used to make cooker, then is widely used in again a plurality of fields of people's productive life.Various metal nano materials constantly were produced out after nanotechnology occurred, the most important purposes of metal nano material is as antiseptic-germicide, Nanometer Copper is considered to one of good metal nano material of Comparison of effect on sterilization, its advantage not only is lower cost and antibacterial ability preferably, also because the copper trace element that to be human body necessary and micro-copper are harmless.Good dispersiveness is the prerequisite that Nanometer Copper and microorganism are in contact with one another and act on, for solving the dispersion problem of Nanometer Copper, some investigators adopt various tensio-active agents, polymer substance etc. to stop the reunion of nanometer copper particle, thereby make the Nanometer Copper powder, but the long-term placement of nanometer copper particle is easily reunited, oxidation, the less stable of powder is so long-term sterilizing ability is restricted.Also have some investigators to adopt TiO
2, SiO
2, the material such as zeolite is as solid support material, make the anti-biotic material that antibiotic effective constituent has made copper-loaded ion with cupric ion, but adopt SiO
2, zeolite during as carrier its use be subjected to the restriction of carrier physical aspect, germ-killing efficiency is lower and range of application is narrower.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, provide that a kind of technique is simple, the preparation method of the antibiotic colloid of curdlan-Nanometer Copper of good anti-bacterial effect.
The preparation method of the antibiotic colloid of a kind of curdlan-Nanometer Copper comprises the steps:
(1) preparation solution of potassium borohydride: take by weighing POTASSIUM BOROHYDRIDE, be dissolved in the water, be mixed with the solution of potassium borohydride that concentration is 1.6g/L;
(2) preparation of Nanometer Copper colloidal sol: at first take by weighing copper sulfate, be dissolved in the water, compound concentration is the copper-bath of 1.2g/L; And then take by weighing sodium lauryl sulphate and polyvinylpyrrolidone, and joining in the copper-bath, stirring and dissolving obtains mixing solutions; Mixing solutions is warming up to 40～50 ℃, under agitation condition, adds the solution of potassium borohydride of step (1) preparation, treat solution from the light blue reddish-brown that changes into, continue to stir 3～5min, obtain Nanometer Copper colloidal sol.
(3) preparation of curdlan dispersion suspension liquid: take by weighing curdlan, be added to the water, after being stirred to curdlan under the normal temperature and being stable dispersion suspension, progressively be warming up to again 40～45 ℃, stand-by;
(4) preparation of antibiotic colloid: with the Nanometer Copper colloidal sol of the curdlan dispersion suspension liquid of step (3) preparation and step (2) the preparation volume ratio with 1:1, under 40 ℃ of conditions, mix; To be mixedly mixed solution is moved into constant temperature oven after evenly, under 80～85 ℃ of conditions, be incubated 3～4 hours, obtain the antibiotic colloid of curdlan-Nanometer Copper.
In the such scheme, the amount of substance of the described POTASSIUM BOROHYDRIDE of step (1) is 3 times of amount of substance of the described copper sulfate of step (2).
In the such scheme, the described sodium lauryl sulphate of step (2) and polyvinylpyrrolidine, according to copper sulfate: sodium lauryl sulphate: the mass ratio of polyvinylpyrrolidone is that the ratio of 1:2.2～2.6:3.5～4.5 is added.
In the such scheme, the rotating speed of the described stirring of step (2) is 300～400r/min.
In the such scheme, the mass volume ratio of the described curdlan of step (3) and water is that 1.6g～2.2g:100ml(W/V), the rotating speed of described stirring is 300～500r/min, and churning time is 24h～36h.
In the such scheme, the described rotating speed that mixes of step (4) is 400～500r/min, churning time 30min.
Know-why of the present invention: the present invention utilizes curdlan can be dispersed in water formation suspension, curdlan can form spiral structure after being heated to certain temperature, this structure can be fixed Nanometer Copper, thereby it is oxidized to delay it, slow down the reunion of nano particle, improve the stability of particle, and then make Nanometer Copper can give full play to its antibacterial ability.
Beneficial effect of the present invention:
(1) preparation technology of the present invention is simple, and production cost is low, applicable to scale operation.
(2) curdlan is good to the dissemination of Nanometer Copper among the present invention, can postpone the oxidized of nanometer copper particle, uses oil seal under the normal temperature, places after 2 months, and nanometer copper particle still possesses preferably antibacterial effect.
Embodiment
In order to understand better the present invention, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to following example.
Embodiment 1
The preparation method of the antibiotic colloid of a kind of curdlan-Nanometer Copper comprises the steps:
(1) solution of preparation POTASSIUM BOROHYDRIDE: take by weighing the 0.016g POTASSIUM BOROHYDRIDE and be dissolved in the 10ml water, preparation obtains solution of potassium borohydride, and is for subsequent use;
(2) preparation of Nanometer Copper colloidal sol: take by weighing 0.06g copper sulfate, join in the 50ml water, be mixed with the copper-bath that concentration is 1.2g/L; Take by weighing respectively 0.144g sodium lauryl sulphate and 0.24g polyvinylpyrrolidone and add in the above-mentioned copper-bath, the rotating speed stirring and dissolving 1h with 300r/min obtains mixing solutions; Then mixing solutions being warming up to 42 ℃, is the solution of potassium borohydride that adds step (1) preparation under the agitation condition of 300r/min at rotating speed, this moment solution immediately by the light blue reddish-brown that changes into, continue stir about 3min and namely obtain Nanometer Copper colloidal sol;
(3) preparation of the aqueous dispersions of curdlan: take by weighing the 0.96g curdlan and place beaker, add 60ml water, under normal temperature, stir 24h take rotating speed as 300r/min, after curdlan disperses fully, be warming up to 40 ℃ stand-by;
(4) preparation of antibiotic colloid: the Nanometer Copper colloidal sol (the two volume ratio is 1:1) that the curdlan aqueous dispersions that step (3) is prepared and step (2) prepare adds in the beaker, under 40 ℃ of conditions, mix, rotating speed is 400r/min, stirs 30min.After finishing mixing mixed solution is moved into constant temperature oven, insulation is 3 hours under 85 ℃ of conditions, namely obtains the antibiotic colloid of curdlan-Nanometer Copper.
With this curdlan-Nanometer Copper antibiosis rubber body and function Viscotrol C sealing, place after 2 months, again according to national standard HG/T3050-2007 antibiotic paint-antibacterium performance test method, carry out antibacterial test, the result shows, the antibiotic colloid of this curdlan-Nanometer Copper is that 32mg/L(is in Nanometer Copper to colibacillary minimal bactericidal concentration), minimal bactericidal concentration to streptococcus aureus is that 16mg/L(is in Nanometer Copper), sterilization effect is good, and meet national standard HG/T3050-2007 antibiotic paint-antibacterium performance index regulation: inorganic antiseptic is lower than 800mg/L to the minimal inhibitory concentration of intestinal bacteria and streptococcus aureus.
Embodiment 2
The preparation of a kind of curdlan-Nanometer Copper composite antibiosis colloid, it may further comprise the steps:
(1) the water liquid of preparation POTASSIUM BOROHYDRIDE: take by weighing the 0.032g POTASSIUM BOROHYDRIDE and be dissolved in the 20ml water, preparation obtains solution of potassium borohydride, and is for subsequent use;
(2) preparation of Nanometer Copper colloidal sol: take by weighing 0.12g copper sulfate, join in the 100ml water, be mixed with the copper-bath that concentration is 1.2g/L; Take by weighing respectively 0.264g sodium lauryl sulphate and 0.42g polyvinylpyrrolidone again and join in the above-mentioned copper-bath, the rotating speed stirring and dissolving 1h with 400r/min obtains mixing solutions; Then mixing solutions being warming up to 40 ℃, is the solution of potassium borohydride that adds step (1) preparation under the agitation condition of 400r/min at rotating speed, this moment solution immediately by the light blue reddish-brown that changes into, continue stir about 5min and namely obtain the Nanometer Copper sol solution;
(3) preparation of the aqueous dispersions of curdlan: get under the 2.4g curdlan adding 120ml normal temperature condition and stir 36h take rotating speed as 500r/min, after curdlan disperses fully, be warming up to 45 ℃, stand-by;
(4) preparation of antibiotic colloid: the aqueous dispersions of the curdlan of step (3) preparation and the Nanometer Copper sol solution (the two volume ratio is 1:1) of step (2) preparation are added in the beaker, under 40 ℃ of conditions, mix, rotating speed is 500r/min, stirs 30min.After finishing mixing mixed solution is moved into constant temperature oven, insulation is 4 hours under 80 ℃ of conditions, namely obtains the antibiotic colloid of curdlan-Nanometer Copper.
With this curdlan-Nanometer Copper antibiosis rubber body and function Viscotrol C sealing, place after 2 months, again according to national standard HG/T3050-2007 antibiotic paint-antibacterium performance test method, carry out antibacterial test, the result shows, the antibiotic colloid of this curdlan-Nanometer Copper is that 32mg/L(is in Nanometer Copper to colibacillary minimal bactericidal concentration), minimal bactericidal concentration to streptococcus aureus is that 16mg/L(is in Nanometer Copper), sterilization effect is good, and meet national standard HG/T3050-2007 antibiotic paint-antibacterium performance index regulation: inorganic antiseptic is lower than 800mg/L to the minimal inhibitory concentration of intestinal bacteria and streptococcus aureus.
Embodiment 3
The preparation of a kind of curdlan-Nanometer Copper composite antibiosis colloid, it may further comprise the steps:
(1) contain the preparation of the water liquid of POTASSIUM BOROHYDRIDE: take by weighing the 0.016g POTASSIUM BOROHYDRIDE and be dissolved in the 10ml water, preparation obtains solution of potassium borohydride, and is for subsequent use;
(2) preparation of Nanometer Copper colloidal sol: take by weighing 0.06g copper sulfate, join in the 50ml water, be mixed with the copper-bath that concentration is 1.2g/L; Take by weighing respectively 0.156g sodium lauryl sulphate and 0.27g polyvinylpyrrolidone again and join in the above-mentioned copper-bath, the rotating speed stirring and dissolving 1h with 350r/min obtains mixing solutions; Then mixing solutions being warming up to 45 ℃, is the aqueous solution that the 350r/min agitation condition adds the POTASSIUM BOROHYDRIDE of step (1) preparation at rotating speed, and solution continues stir about 4min and namely obtains Nanometer Copper colloidal sol immediately by the light blue reddish-brown that changes into;
(3) contain the preparation of the dispersion liquid of curdlan: get the 1.32g curdlan and add in the 60ml water, stir 30h take rotating speed as 400r/min under the normal temperature, after curdlan disperses fully, be warming up to 43 ℃ stand-by;
(4) preparation of antibiotic colloid: the described mixed solution that contains curdlan dispersion liquid 50ml and Nanometer Copper colloidal sol (the two volume ratio is 1:1) of step (3) is added in the reactor, be to mix 30min under the 450r/min condition at 40 ℃ of rotating speeds, under 83 ℃ of conditions, be incubated 3.5 hours after mixing, namely obtain the antibiotic colloid of curdlan-Nanometer Copper.
With this curdlan-Nanometer Copper antibiosis rubber body and function Viscotrol C sealing, place after 2 months, again according to national standard HG/T3050-2007 antibiotic paint-antibacterium performance test method, carry out antibacterial test, the result shows, the antibiotic colloid of this curdlan-Nanometer Copper is that 32mg/L(is in Nanometer Copper to colibacillary minimal bactericidal concentration), minimal bactericidal concentration to streptococcus aureus is that 16mg/L(is in Nanometer Copper), sterilization effect is good, and meet national standard HG/T3050-2007 antibiotic paint-antibacterium performance index regulation: inorganic antiseptic is lower than 800mg/L to the minimal inhibitory concentration of intestinal bacteria and streptococcus aureus.
Obviously, above-described embodiment only is to be the example done of explanation clearly, and is not the restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give all embodiments exhaustive.And the apparent variation of therefore amplifying or change still are within the protection domain of the invention.
Claims (6)
1. the preparation method of the antibiotic colloid of curdlan-Nanometer Copper is characterized in that comprising the steps:
(1) preparation solution of potassium borohydride: take by weighing POTASSIUM BOROHYDRIDE, be dissolved in the water, be mixed with the solution of potassium borohydride that concentration is 1.6g/L;
(2) preparation of Nanometer Copper colloidal sol: at first take by weighing copper sulfate, be dissolved in the water, compound concentration is the copper-bath of 1.2g/L; And then take by weighing sodium lauryl sulphate and polyvinylpyrrolidone, and joining in the copper-bath, stirring and dissolving obtains mixing solutions; Mixing solutions is warming up to 40～50 ℃, under agitation condition, adds the solution of potassium borohydride of step (1) preparation, treat solution from the light blue reddish-brown that changes into, continue to stir 3～5min, obtain Nanometer Copper colloidal sol;
(3) preparation of curdlan dispersion suspension liquid: take by weighing curdlan, be added to the water, after being stirred to curdlan under the normal temperature and being stable dispersion suspension, progressively be warming up to again 40～45 ℃, stand-by;
(4) preparation of antibiotic colloid: with the Nanometer Copper colloidal sol of the curdlan dispersion suspension liquid of step (3) preparation and step (2) the preparation volume ratio with 1:1, under 40 ℃ of conditions, mix; To be mixedly mixed solution is moved into constant temperature oven after evenly, under 80～85 ℃ of conditions, be incubated 3～4 hours, obtain the antibiotic colloid of curdlan-Nanometer Copper.
2. described method according to claim 1, the amount of substance that it is characterized in that the described POTASSIUM BOROHYDRIDE of step (1) are 3 times of amount of substance of the described copper sulfate of step (2).
3. described method according to claim 1, it is characterized in that the described sodium lauryl sulphate of step (2) and polyvinylpyrrolidine, its consumption is according to copper sulfate: sodium lauryl sulphate: the mass ratio of polyvinylpyrrolidone is that the ratio of 1:2.2～2.6:3.5～4.5 is added.
4. described method according to claim 1 is characterized in that the rotating speed of the described stirring of step (2) is 300～400r/min.
5. described method according to claim 1, the mass volume ratio that it is characterized in that the described curdlan of step (3) and water is that 1.6g～2.2g:100ml(W/V), the rotating speed of described stirring is 300～500r/min, churning time is 24h～36h.
6. described method according to claim 1 is characterized in that the described rotating speed that mixes of step (4) is 400～500r/min, churning time 30min.
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Cited By (5)
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| CN106383234A (en) * | 2016-08-31 | 2017-02-08 | 上海科华生物工程股份有限公司 | Coating method for retinol-binding protein detection reagent |
| CN106805251A (en) * | 2017-01-18 | 2017-06-09 | 福建农林大学 | A kind of polypeptide condenses polysaccharide plural gel and preparation method thereof |
| CN107685151A (en) * | 2017-08-28 | 2018-02-13 | 江西赣大材料技术研究有限公司 | A kind of preparation method of the compound antibacterial solid sols of nanometer of copper epoxy |
| CN113694250A (en) * | 2021-07-19 | 2021-11-26 | 暨南大学 | Preparation method and application of curdlan antibacterial hydrogel loaded with nano silver particles |
| CN117183033A (en) * | 2023-11-07 | 2023-12-08 | 江苏佳伯荣林业股份有限公司 | Density board with antibacterial function |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106383234A (en) * | 2016-08-31 | 2017-02-08 | 上海科华生物工程股份有限公司 | Coating method for retinol-binding protein detection reagent |
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| CN107685151A (en) * | 2017-08-28 | 2018-02-13 | 江西赣大材料技术研究有限公司 | A kind of preparation method of the compound antibacterial solid sols of nanometer of copper epoxy |
| CN113694250A (en) * | 2021-07-19 | 2021-11-26 | 暨南大学 | Preparation method and application of curdlan antibacterial hydrogel loaded with nano silver particles |
| CN117183033A (en) * | 2023-11-07 | 2023-12-08 | 江苏佳伯荣林业股份有限公司 | Density board with antibacterial function |
| CN117183033B (en) * | 2023-11-07 | 2024-02-27 | 江苏佳伯荣林业股份有限公司 | Density board with antibacterial function |
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