CN101513190A - Inorganic anti-bacterium mildewproof additive, preparation method and application thereof - Google Patents
Inorganic anti-bacterium mildewproof additive, preparation method and application thereof Download PDFInfo
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- CN101513190A CN101513190A CNA2009100645744A CN200910064574A CN101513190A CN 101513190 A CN101513190 A CN 101513190A CN A2009100645744 A CNA2009100645744 A CN A2009100645744A CN 200910064574 A CN200910064574 A CN 200910064574A CN 101513190 A CN101513190 A CN 101513190A
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Abstract
The invention discloses an inorganic anti-bacterium mildewproof additive, a preparation method and application thereof. The additive is mineral powder containing Ag element and long chain alkyl ammonium salts, and is characterized in that the mineral powder is turface or vermiculite power, and, by weight percentage, comprises 1.5 to 7.0 percent of the Ag element in the mineral powder, and 5 to 30 percent of the long chain alkyl ammonium salts in the mineral powder. The preparation method comprises the following steps: carrying out sodium treatment on the mineral powder; adsorbing Ag ions among laminations of the mineral powder; introducing the long chain alkyl ammonium salts into the laminations of the mineral power carrying Ag; carrying out organic intercalation treatment on the turface or the vermiculite carrying Ag by amphipathy performance of the long chain alkyl ammonium salts. Compared with inorganic antibacterial agents carrying Ag independently and supported by the long chain alkyl ammonium salt columns independently, when the turface or the vermiculite powder with anti-bacterium function is applied to plastic and other base materials, the product can not be easily discolored, has long-term inhabitation on bacteria and fungus, greatly reduces cost, and widening the application field.
Description
Technical field:
The present invention relates to a kind of anti-bacterium mildewproof additive, excellent its relates to a kind of inorganic anti-bacterium mildewproof additive and its production and use that is applied in the goods such as fiber, plastics, paint, coating.
Background technology:
Montmorillonite or vermiculite one class layer silicate mineral have 2: 1 construction unit layers on crystal structure, layer structure can expand when heating, has very strong absorption affinity and cation exchange capacity (CEC).Silver ion is incorporated between montmorillonite or vermiculite layers by cation exchange reaction, just can obtains having the montmorillonite or the vermiculite that bacterium and mould are all had antibacterial action.This inorganic antiseptic have antibiotic wide spectrum, safe, do not have advantage such as volatilization, so can be widely used in the goods such as fiber, plastics, paint, coating.
But the montmorillonite or the vermiculite powder that contain silver ion harden after oven dry seriously, and when joining matrixes such as plastics, relatively poor with the matrix bond ability, deployment conditions is not good, and product properties can be subjected to very big influence; Because silver ion is stable inadequately, separate out in a large number easily simultaneously, make the antibacterial effect of goods not good; In " novel plastic material technology prescription " (first volume), Beijing: China Light Industry Press, 2000.Author Deng Shunyang points out: silver ion is separated out easily oxidation stain of back, can make goods variable color such as plastics heavier, and application is subjected to very big restriction, and therefore present research all is devoted to improve the discoloration problem of antibacterial agent.The binding ability of base materials such as antibacterial additives and plastics also remains further to be improved simultaneously.
Summary of the invention:
The object of the invention is to prepare a kind ofly both to have been had the antibacterial functions characteristic and improves greatly with the plastic substrate binding ability and disperse good inorganic anti-bacterium mildewproof additive in plastic substrate.
Another object of the present invention provides a kind of preparation method with inorganic anti-bacterium mildewproof additive of antibacterial functions characteristic.
Another object of the present invention is the application of exploitation inorganic anti-bacterium mildewproof additive.
Technical scheme of the present invention realizes in the following manner:
A kind of inorganic anti-bacterium mildewproof additive, it is the ore powder of a kind of Ag of containing element and long chain alkyl ammonium salt, it is characterized in that: ore powder is montmorillonite or vermiculite powder, by weight percentage: the content of Ag element in ore powder is 1.5～7.0%, and long chain alkyl ammonium salt content in ore powder is 5～30%.
Described long chain alkyl ammonium salt is a cationic surface active agent, and its molecular structural formula is:
N=12,14,16 or 18 wherein; X is Br or Cl.
By weight percentage, the content of described Ag element in the montmorillonite powder is 1.5～5%, and the content of long chain alkyl ammonium salt in the montmorillonite powder is 5～25%.
Described long chain alkyl ammonium salt is DTAB or softex kw or TTAB.
By weight percentage, the content of described Ag element in the vermiculite powder is 3～7%, and the content of long chain alkyl ammonium salt in the vermiculite powder is 15～30%.
Described long chain alkyl ammonium salt is tetradecyl trimethyl ammonium chloride, octadecyl trimethylammonium bromide or softex kw.
The preparation method of described inorganic anti-bacterium mildewproof additive may further comprise the steps:
(1) with granularity≤200 purpose ore powders, together with its 20～50% sodium salts that account for the ore powder gross weight, add water and stir, make concentration and be 5～30% suspension ore pulp, at 40～90 ℃, stirring condition reaction 12～24 hours down;
(2) behind the centrifugal or filtering means dehydration, make 10～30% water slurry ore pulp again, add 5～15% the Ag salt that accounts for the ore powder gross weight, at 40～80 ℃, stirring condition reaction 3～6 hours down;
(3) behind the centrifugal or filtering means dehydration, make 10～30% water slurry ore pulp again, add 10～120% the long chain alkyl ammonium salt that accounts for the ore powder gross weight, at 60～90 ℃, stirring condition reaction 12～24 hours down;
(4) behind the centrifugal or filtering means dehydration, the ore powder of gained is placed the vacuum drying oven baking part of anhydrating not being higher than under 80 ℃ of temperature, products therefrom is the ore powder with antibacterial functions characteristic.
Described sodium salt is NaCl, NaNO
3, Na
2CO
3, NaHCO
3, Na
2SO
4In a kind of or several.
Described Ag salt is AgNO
3
The application of described anti-bacterium mildewproof additive in the organic polymer preparation.
Good effect of the present invention is:
Parents' performance of long chain alkyl ammonium salt, montmorillonite or the vermiculite that carries Ag carried out the organic intercalation processing, the inorganic antiseptic pillared with carrying separately Ag and independent long chain quaternary compared, this has the montmorillonite of antibacterial functions characteristic or vermiculite powder when using in matrix materials such as plastics, goods are not easy to change, bacterium and fungi are had long-acting inhibition, and cost reduces significantly simultaneously, and application is widened.
Long chain alkyl ammonium salt is a kind of amphiphatic cationic surfactant, be introduced into carry an Ag montmorillonite, vermiculite after, its an end adsorbed close plays the good restraining effect to stripping and the variable color of Ag on the silicate surface layer of montmorillonite or vermiculite; After long chain alkyl ammonium salt is incorporated into and carries between Ag montmorillonite or vermiculite layers, the interlamellar spacing of montmorillonite or vermiculite significantly improves, superficial layer has hydrophobicity simultaneously, when this antibacterial agent adds in the matrix materials such as plastics, be stripped from easily, degree of scatter improves in matrix, with the binding ability raising of matrix; Long chain alkyl ammonium salt itself also has very strong antibacterial action, it is incorporated into carries between Ag montmorillonite or vermiculite layers, and it and Ag can produce synergy, and year Ag montmorillonite or vermiculite are improved the antibacterial ability of bacterium and fungi.
Embodiment
The preparation method's of montmorillonite with antibacterial functions characteristic of the present invention or vermiculite powder the first step is montmorillonite or vermiculite to be carried out sodium handle, make sodium ions content raising between montmorillonite or vermiculite layers, because of when cation exchange reaction, sodium ion is easier to be exchanged with Ag ion and long chain alkyl ammonium salt, has improved the cation exchange capacity (CEC) of montmorillonite or vermiculite.
Preparation method's second step is with the interlayer of Ag ionic adsorption to montmorillonite or vermiculite, easily decomposes variable color because of Ag sees light, and this step reaction notes lucifuge, and should go on foot used Ag salting liquid simultaneously can recycling.
Preparation method's the 3rd step is that long chain alkyl ammonium salt is incorporated between the montmorillonite or vermiculite layers that carries Ag, reaches the expansion montmorillonite, and the interlamellar spacing of vermiculite suppresses the effect of Ag stripping.
Preparation method's the 4th step is that montmorillonite or the vermiculite powder that Ag and long chain alkyl ammonium salt have the antibacterial functions characteristic that contain with gained carries out fine grinding, improves its dispersion grade in matrix materials such as plastics.
The present invention preparation contain Ag and long chain alkyl ammonium salt has the montmorillonite of antibacterial functions characteristic or the anti-bacterium mildewproof additive that the vermiculite powder is applicable to organic polymers such as plastics, coating, hydrogel, composition is added in the sterilization that also can be used as simultaneously in the animal feed.
The invention will be further described below in conjunction with specific embodiment:
Embodiment 1
(1) taking by weighing the 10kg granularity is 200 purpose montmorillonites, together with the NaCl of 2kg, adds 25kg water and stirs, and makes the suspension ore pulp, and at 40 ℃, stirring condition reacted 12 hours down;
(2) behind the centrifugal or filtering means dehydration, wash with water 3～5 times, remove the Cl ion in the montmorillonite, add 90kg water and stir, make the suspension ore pulp, add the AgNO of 0.5kg
3, at 40 ℃, stirring condition reacted 3 hours down;
(3) behind the centrifugal or filtering means dehydration, wash with water 3～5 times, remove the Ag ion on montmorillonite surface, add 40kg water and stir, make the suspension ore pulp, add the DTAB of 1kg, at 60 ℃, stirring condition reaction 12 hours down;
(4) behind the centrifugal or filtering means dehydration, wash 3～5 times, the montmorillonite of gained is placed the vacuum drying oven baking part of anhydrating under 80 ℃ of temperature, products therefrom is the inorganic anti-bacterium mildewproof additive with antibacterial functions characteristic, is ground to 400 orders, and pack is preserved.
By detecting, the content of Ag element in the gained montmorillonite is 1.5%, and the content of quaternary ammonium salt is 5%.Test inhibition zone and the antibiotic rate of this antibiotic montmorillonite powder by inhibition zone test method(s) and triangular flask shaking test method to Escherichia coli and staphylococcus aureus.
Result of the test shows: this antibiotic montmorillonite all has tangible bacteriostasis to Escherichia coli and staphylococcus aureus, is 1.5mm to colibacillary inhibition zone width, is 2.0mm to the inhibition zone width of staphylococcus aureus; To the antibiotic rate of Escherichia coli and staphylococcus aureus all greater than 90%.
Embodiment 2
(1) taking by weighing the 10kg granularity is 200 purpose vermiculites, together with the NaNO of 3kg
3, add 40kg water and stir, make the suspension ore pulp, at 60 ℃, stirring condition reacted 16 hours down;
(2) behind the centrifugal or filtering means dehydration, wash with water 3～5 times, remove the Cl ion in the vermiculite, add 70kg water and stir, make the suspension ore pulp, add the AgNO of 1kg
3, at 60 ℃, stirring condition reacted 4 hours down;
(3) behind the centrifugal or filtering means dehydration, wash with water 3～5 times, remove the Ag ion on vermiculite surface, add 25kg water and stir, make the suspension ore pulp, add the tetradecyl trimethyl ammonium chloride of 4kg, at 70 ℃, stirring condition reaction 16 hours down;
(4) behind the centrifugal or filtering means dehydration, wash 3～5 times, the vermiculite of gained is placed the vacuum drying oven baking part of anhydrating under 80 ℃ of temperature, products therefrom is the vermiculite powder with antibacterial functions characteristic, is ground to 400 orders, and pack is preserved.
By detecting, the content of Ag element in the gained vermiculite is 3%, and the content of quaternary ammonium salt is 15%.
Result of the test shows: this antibiotic vermiculite all has tangible bacteriostasis to Escherichia coli and staphylococcus aureus, is 2.5mm to colibacillary inhibition zone width, is 3.0mm to the inhibition zone width of staphylococcus aureus; To the antibiotic rate of Escherichia coli and staphylococcus aureus all greater than 95%.
Embodiment 3
(1) taking by weighing the 10kg granularity is 200 purpose montmorillonites, together with the Na of 4kg
2CO
3, add 70kg water and stir, make the suspension ore pulp, at 80 ℃, stirring condition reacted 20 hours down;
(2) behind the centrifugal or filtering means dehydration, wash with water 3～5 times, remove the Cl ion in the montmorillonite, add 40kg water and stir, make the suspension ore pulp, add the AgNO of 1.2kg
3, at 70 ℃, stirring condition reacted 5 hours down;
(3) behind the centrifugal or filtering means dehydration, wash with water 3～5 times, remove the Ag ion on montmorillonite surface, add 90kg water and stir, make the suspension ore pulp, add the softex kw of 8kg, at 80 ℃, stirring condition reaction 20 hours down;
(4) behind the centrifugal or filtering means dehydration, wash 3～5 times, the montmorillonite of gained is placed the vacuum drying oven baking part of anhydrating under 80 ℃ of temperature, products therefrom is the montmorillonite powder with antibacterial functions characteristic, is ground to 400 orders, and pack is preserved.
By detecting, the content of Ag element in the gained montmorillonite is 5%, and the content of quaternary ammonium salt is 25%.
Result of the test shows: this antibiotic montmorillonite all has tangible bacteriostasis to Escherichia coli and staphylococcus aureus, is 3.5mm to colibacillary inhibition zone width, is 3.8mm to the inhibition zone width of staphylococcus aureus; To the antibiotic rate of Escherichia coli and staphylococcus aureus all greater than 98%.
Embodiment 4
(1) taking by weighing the 10kg granularity is 200 purpose vermiculites, together with the NaHCO of 5kg
3, add 90kg water and stir, make the suspension ore pulp, at 90 ℃, stirring condition reacted 24 hours down;
(2) behind the centrifugal or filtering means dehydration, wash with water 3～5 times, remove the Cl ion in the vermiculite, add 25kg water and stir, make the suspension ore pulp, add the AgNO of 1.5kg
3, at 80 ℃, stirring condition reacted 6 hours down;
(3) behind the centrifugal or filtering means dehydration, wash with water 3～5 times, remove the Ag ion on vermiculite surface, add 40kg water and stir, make the suspension ore pulp, add the octadecyl trimethylammonium bromide of 12kg, at 90 ℃, stirring condition reaction 24 hours down;
(4) behind the centrifugal or filtering means dehydration, wash 3～5 times, the gained vermiculite is placed the vacuum drying oven baking part of anhydrating under 80 ℃ of temperature, products therefrom is the vermiculite powder with antibacterial functions characteristic, is ground to 400 orders, and pack is preserved.
By detecting, the content of Ag element in the gained vermiculite is 7%, and the content of quaternary ammonium salt is 30%.
Result of the test shows: this antibiotic vermiculite all has tangible bacteriostasis to Escherichia coli and staphylococcus aureus, is 4.5mm to colibacillary inhibition zone width, is 5.0mm to the inhibition zone width of staphylococcus aureus; To the antibiotic rate of Escherichia coli and staphylococcus aureus all greater than 99%.
Embodiment 5
Process route by embodiment 1 prepares antibiotic montmorillonite, and different is that the content of Ag element in the antibiotic montmorillonite of gained is 3.4%, and quaternary ammonium salt is a TTAB, and the content in the antibiotic montmorillonite of gained is 17%.Its antibacterial tests is the result show: this product is to being 2.3mm to colibacillary inhibition zone width, is 2.8mm to the inhibition zone width of staphylococcus aureus; To the antibiotic rate of Escherichia coli and staphylococcus aureus all greater than 95%.
Embodiment 6
Process route by embodiment 2 prepares antibiotic vermiculite, different is that the content of Ag element in the antibiotic vermiculite powder of gained is 5.5%, quaternary ammonium salt is a softex kw, and the content of softex kw in the antibiotic vermiculite powder of gained is 20%.Its antibacterial tests is the result show: this product is to being 3.4mm to colibacillary inhibition zone width, is 3.8mm to the inhibition zone width of staphylococcus aureus; To the antibiotic rate of Escherichia coli and staphylococcus aureus all greater than 98%.
Embodiment 7
After the antibiotic vermiculite powder that the foregoing description is made mixes in the high speed kneader with nylon 6, nylon 66 respectively with certain proportion, use the double screw extruder extruding pelletization, make anti-bacteria nylon 6 and anti-bacteria nylon 66.
The antibacterial experiment result shows: when antimicrobial powder content was 2%, antibiotic rate was 74%, and when antimicrobial powder content was 5%, antibiotic rate was 90%, and when antimicrobial powder content was 10%, antibiotic rate was 96%.
Embodiment 8
The antibiotic montmorillonite powder that the foregoing description is made evenly mixes with nylon salt with certain proportion, and polymerization in autoclave makes anti-bacteria nylon 66.The antibacterial experiment result shows that antibiotic rate is 70% when antimicrobial powder content is 2%, and when antimicrobial powder content was 5%, antibiotic rate was 90%.
Claims (10)
1, a kind of inorganic anti-bacterium mildewproof additive, it is the ore powder of a kind of Ag of containing element and long chain alkyl ammonium salt, it is characterized in that: ore powder is montmorillonite or vermiculite powder, by weight percentage: the content of Ag element in ore powder is 1.5～7.0%, and long chain alkyl ammonium salt content in ore powder is 5～30%.
2, inorganic anti-bacterium mildewproof additive according to claim 1 is characterized in that: described long chain alkyl ammonium salt is a cationic surface active agent, and its molecular structural formula is:
N=12,14,16 or 18 wherein; X is Br or Cl.
3, inorganic anti-bacterium mildewproof additive according to claim 2 is characterized in that: by weight percentage: the content of Ag element in the montmorillonite powder is 1.5～5%, and the content of long chain alkyl ammonium salt in the montmorillonite powder is 5～25%.
4, inorganic anti-bacterium mildewproof additive according to claim 3 is characterized in that: long chain alkyl ammonium salt is DTAB or softex kw or TTAB.
5, inorganic anti-bacterium mildewproof additive according to claim 2 is characterized in that: by weight percentage: the content of Ag element in the vermiculite powder is 3～7%, and the content of long chain alkyl ammonium salt in the vermiculite powder is 15～30%.
6, inorganic anti-bacterium mildewproof additive according to claim 5 is characterized in that: long chain alkyl ammonium salt is tetradecyl trimethyl ammonium chloride, octadecyl trimethylammonium bromide or softex kw.
7, a kind of preparation method according to claim 1,2,3,4,5 or 6 described inorganic anti-bacterium mildewproof additives may further comprise the steps:
(1) with granularity≤200 purpose ore powders, together with its 20～50% sodium salts that account for the ore powder gross weight, add water and stir, make concentration and be 5～30% suspension ore pulp, at 40～90 ℃, stirring condition reaction 12～24 hours down;
(2) behind the centrifugal or filtering means dehydration, make 10～30% water slurry ore pulp again, add 5～15% the Ag salt that accounts for the ore powder gross weight, at 40～80 ℃, stirring condition reaction 3～6 hours down;
(3) behind the centrifugal or filtering means dehydration, make 10～30% water slurry ore pulp again, add 10～120% the long chain alkyl ammonium salt that accounts for the ore powder gross weight, at 60～90 ℃, stirring condition reaction 12～24 hours down;
(4) behind the centrifugal or filtering means dehydration, the ore powder of gained is placed the vacuum drying oven baking part of anhydrating not being higher than under 80 ℃ of temperature, products therefrom is the ore powder with antibacterial functions characteristic.
8, the preparation method of inorganic anti-bacterium mildewproof additive according to claim 7 is characterized in that: described sodium salt is NaCl, NaNO
3, Na
2CO
3, NaHCO
3, Na
2SO
4In a kind of or several.
9, the preparation method of inorganic anti-bacterium mildewproof additive according to claim 7 is characterized in that: described Ag salt is AgNO
3
10, a kind of according to claim 1,2,3,4, the application of 5 or 6 described anti-bacterium mildewproof additives in the organic polymer preparation.
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|---|---|---|---|---|
| CN103891775A (en) * | 2013-11-28 | 2014-07-02 | 龙岩学院 | Zinc-carrying nano organic montmorillonite antimicrobial agent and preparation method thereof |
| CN104719339A (en) * | 2013-12-24 | 2015-06-24 | 比亚迪股份有限公司 | Antibacterial material as well as preparation method and application thereof |
| CN105519577A (en) * | 2016-01-11 | 2016-04-27 | 济南康众医药科技开发有限公司 | Novel application of Smecta in controlling vegetable diseases |
| CN108823971A (en) * | 2018-06-22 | 2018-11-16 | 合肥洁诺医疗用品有限公司 | A kind of preparation method for non-woven fabrics antibacterial agent |
| CN109287656A (en) * | 2018-10-31 | 2019-02-01 | 浙江海洋大学 | A kind of high polymer finishing coat wall preparation method for removing mould mildew resistant spraying agent |
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| CN112876811A (en) * | 2021-01-18 | 2021-06-01 | 安徽牛元新材料有限公司 | Mildew-proof seam beautifying agent and preparation method thereof |
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2009
- 2009-04-03 CN CNA2009100645744A patent/CN101513190A/en active Pending
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| US11098177B2 (en) | 2013-09-30 | 2021-08-24 | Arkema Inc. | Heat stabilized polyvinylidene fluoride polymer composition |
| CN103891775A (en) * | 2013-11-28 | 2014-07-02 | 龙岩学院 | Zinc-carrying nano organic montmorillonite antimicrobial agent and preparation method thereof |
| CN104719339A (en) * | 2013-12-24 | 2015-06-24 | 比亚迪股份有限公司 | Antibacterial material as well as preparation method and application thereof |
| CN105519577A (en) * | 2016-01-11 | 2016-04-27 | 济南康众医药科技开发有限公司 | Novel application of Smecta in controlling vegetable diseases |
| CN108823971A (en) * | 2018-06-22 | 2018-11-16 | 合肥洁诺医疗用品有限公司 | A kind of preparation method for non-woven fabrics antibacterial agent |
| CN109287656A (en) * | 2018-10-31 | 2019-02-01 | 浙江海洋大学 | A kind of high polymer finishing coat wall preparation method for removing mould mildew resistant spraying agent |
| CN109439033A (en) * | 2018-10-31 | 2019-03-08 | 浙江海洋大学 | A kind of inorganic coating wall is with removing mould mildew resistant spraying agent |
| CN109439033B (en) * | 2018-10-31 | 2021-02-09 | 浙江海洋大学 | Mildew-removing and mildew-proof spray for inorganic coating wall |
| CN110037017A (en) * | 2019-05-06 | 2019-07-23 | 宁夏大学 | It is modified montmorillonite used and load plants essential oil antibacterial powder and preparation method thereof |
| CN112876811A (en) * | 2021-01-18 | 2021-06-01 | 安徽牛元新材料有限公司 | Mildew-proof seam beautifying agent and preparation method thereof |
| CN114045005A (en) * | 2021-10-22 | 2022-02-15 | 安徽弘源化工科技有限公司 | Melamine finishing powder with antibacterial property |
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Open date: 20090826 |