CN1086270C - Antifungal composition and its preparation method - Google Patents
Antifungal composition and its preparation method Download PDFInfo
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- CN1086270C CN1086270C CN98124542A CN98124542A CN1086270C CN 1086270 C CN1086270 C CN 1086270C CN 98124542 A CN98124542 A CN 98124542A CN 98124542 A CN98124542 A CN 98124542A CN 1086270 C CN1086270 C CN 1086270C
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- CN
- China
- Prior art keywords
- bactericidal composition
- dispersant
- znso4
- preparation
- agno3
- Prior art date
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- 238000002360 preparation method Methods 0.000 title claims description 13
- 239000012871 anti-fungal composition Substances 0.000 title 1
- 239000010457 zeolite Substances 0.000 claims abstract description 15
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 13
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract 18
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract 6
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract 6
- 239000011686 zinc sulphate Substances 0.000 claims abstract 6
- 235000009529 zinc sulphate Nutrition 0.000 claims abstract 6
- 239000000203 mixture Substances 0.000 claims description 25
- 230000000844 anti-bacterial effect Effects 0.000 claims description 21
- 239000002002 slurry Substances 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000000470 constituent Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Inorganic materials [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims 2
- 239000002244 precipitate Substances 0.000 claims 1
- 239000004033 plastic Substances 0.000 abstract description 14
- 229920003023 plastic Polymers 0.000 abstract description 14
- 230000000845 anti-microbial effect Effects 0.000 abstract description 2
- 239000004599 antimicrobial Substances 0.000 abstract 2
- 239000002994 raw material Substances 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 abstract 1
- 239000011787 zinc oxide Substances 0.000 abstract 1
- 238000003756 stirring Methods 0.000 description 19
- 239000003242 anti bacterial agent Substances 0.000 description 14
- 239000011701 zinc Substances 0.000 description 12
- 230000003115 biocidal effect Effects 0.000 description 10
- 101710134784 Agnoprotein Proteins 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 230000004075 alteration Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 241000228197 Aspergillus flavus Species 0.000 description 1
- 244000063299 Bacillus subtilis Species 0.000 description 1
- 235000014469 Bacillus subtilis Nutrition 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 241000345998 Calamus manan Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241001478240 Coccus Species 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 241000191938 Micrococcus luteus Species 0.000 description 1
- 241000235526 Mucor racemosus Species 0.000 description 1
- 241000228153 Penicillium citrinum Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000001857 anti-mycotic effect Effects 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 239000002543 antimycotic Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000000369 enteropathogenic effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009313 farming Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 235000012950 rattan cane Nutrition 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229940100890 silver compound Drugs 0.000 description 1
- 150000003379 silver compounds Chemical class 0.000 description 1
- UEJSSZHHYBHCEL-UHFFFAOYSA-N silver(1+) sulfadiazinate Chemical compound [Ag+].C1=CC(N)=CC=C1S(=O)(=O)[N-]C1=NC=CC=N1 UEJSSZHHYBHCEL-UHFFFAOYSA-N 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention relates to an antimicrobial agent for plastic, which uses AgNO3, Zn (NO3)2, ZnSO4, ZnO, dispersants and zeolite as raw materials and is formed by controlling the proportion of components and adopting the definite steps. The antimicrobial agent has the characteristics of broad antimicrobial spectrum, good color stability, extensive application range, etc.
Description
The present invention relates to use compounds such as metallic compound such as silver, copper, zinc and activation silicon, boron, by the specific support appendix and make up and make antibacterial agent that is used for antibiotic plastic and preparation method thereof.
People have found that for a long time silver, copper, zinc metal and compound thereof have sterilizing function.Huang Lizhong has reported the application of silver compound aspect clinical medicine.As use AgNO
3Solution or collargol are handled wound, are used (noble metal, 1995,16 (2): 72) such as sulfadiazine silver is antimycotic, inhibition virus.Tokuyama disclosed by Cu in 95 years
2+, Zn
2+, Cr
3+The antibacterial components of making Deng the compound and the respective ligand of composition is used for the coating manufacturing, resists bacterium and algae (JP95-133444).It is not long that but the antibacterial functions that utilizes this metal compound prepares the history of antibiotic plastic.Up to the present, three phases has roughly been experienced in the antibacterial agent development that is used for antibiotic plastic:
1. soluble compound directly adds to and makes antibiotic plastic in the resin.But the antibiotic plastic of this method preparation not only performance descends, and the antibiotic term of validity is very short;
2. be that carrier appendix metal ion prepares antibacterial agent with the active carbon.But the antibiotic plastic with this antibacterial agent preparation is a black, and the scope of application has been subjected to very big restriction:
3. use the stronger material of chemical bond power to make carrier appendix antibacterial material and prepare antibacterial agent.
People such as the middle island of Kanebo Ltd and a man of virtue and ability, peace rattan acute hearing disclose the patent of " stable zeolite and preparation method thereof ", reported with the zeolite and be preparing carriers antibacterial agent (JP91-131513), the Yamamoto moral smelting of upright nitre Co., Ltd. discloses the patent of " glass-based water treatment agent " altogether, reported to be that the hillside plot farming of antibacterial agent (JP87-210098) Sumitomo Seika Co., Ltd of carrier discloses the patent of " preservative constituent for building " with the glass microballoon, reported to be the antibacterial agent (JP91-191145) of carrier with silica gel.And this class antibacterial agent has been applied to every field such as construction material, household electrical appliance gradually.
But the main active ingredient of inorganic antiseptic is generally compounds such as silver, zinc, copper at present, and general antibacterial agent all contains Ag
+Because Ag
+To photo-labile, easily deposit or use in cause variable color.This problem has seriously restricted the range of application of antibacterial agent, especially to fields such as the exigent household electrical appliances of outward appearance, calculators.
The present invention has overcome present antibacterial agent ubiquitous discoloration problem in preservation and use, and has proposed the new prescription of synthesizing new antibacterial agent and new preparation technology.The antibacterial agent non-toxic efficient broad-spectrum sterilization that makes, little to the mechanical property influence of plastics, and have excellent colour stability.
Antimicrobial composition of the present invention comprises following component and content (weight portion):
The preferable content of constituent content
AgNO
3 0-2
Zn(NO
3)
2 0.1-60 20-50
ZnSO
4 0-50 30-40
ZnO 5-80 20-50
Dispersant 0.5
Zeolite 100
Antibacterial inorganic preparation of compositions method of the present invention is carried out in the following order:
1. by weight with the AgNO of 0-2 part
3, 0.1-60 part Zn (NO
3)
2ZnSO with 0-50 part
4Be mixed with the AgNO of 0-5% respectively with deionized water
3Solution, 10%～saturated Zn (NO
3)
2And ZnSO
4Solution for later use.
2. at above-mentioned AgNO
3Add 100 parts of zeolites in the solution, form uniform slurries, be heated to 80 ℃～boiling, and under this temperature, keep stirring 20～100min, stop to stir and being cooled to room temperature with mechanical agitation or electromagnetic agitation, treat the slurries precipitated and separated after, topple over and fall supernatant.In the beds of precipitation, add above-mentioned Zn (NO then
3)
2And ZnSO
4Solution becomes electromagnetism to stir with mechanical agitation and is heated to 60～90 ℃ after material stirs into homogeneous slurry, reaction 60～300min.
3. add dispersant in above-mentioned slurries, stop heating after stirring, etc. after the system cooling slurries are dried, powder particle diameter is less than the pressed powder of 30 μ.
4. at the last ZnO powder that adds 5-80 part in the powder that obtains that goes on foot, mix, promptly obtain bactericidal composition of the present invention.
Preparation AgNO
3During solution, concentration is advisable with 0-2%, and excessive concentration can cause and adds behind the zeolite feeding-uply, influence subsequent process and operates.
Preparation Zn (NO
3)
2During solution, concentration is advisable with 30-40%.Concentration is crossed and low can be caused that metal ion appendix amount is on the low side, and workload is big when causing drying, energy waste.
Heating AgNO
3, temperature should be controlled at 94-99 ℃ and is advisable during the zeolite mixed serum, temperature is crossed and lowly can be caused that gas residual quantity increases in the zeolite, ion appendix ability drop, the high slightly then system boiling of temperature can cause that again moisture evaporation is too fast, operating difficulties.
Add Zn (NO
3)
2, ZnSO
4Behind the solution, slurry temperature should be controlled at 65～75 ℃ and be advisable.Temperature is too high, and moisture evaporation is too fast, influences the appendix reaction of ion.Temperature is low excessively, causes zeolite appendix amount to descend.
Above-mentioned dispersant is CA-977, HYDROPALAT or SN-DISPERSANT.
Escherichia coli, bacillus subtilis, staphylococcus aureus, Sarcina lutea, aspergillus flavus, Penicillium citrinum, Mucor racemosus, prunosus red coccus etc. all have good inhibitory effect during antibacterial inorganic composition that the present invention makes, and it is 0.05% to enteropathogenic E minimal bactericidal concentration (weight portion).
The present invention makes bactericidal composition and has good colour stability, and through 200hr standard uviol lamp accelerated ageing experiment, its result shows difference DELTA E≤2 of the aberration of its aberration and corresponding base material.
The present invention makes the inorganic antibacterial composition and can directly add plastics such as PVC, PE, PP, PS, ABS, PET, PBT, PA, TPU, PC, PMMA, SAN to and be prepared into antibiotic plastic, also can be prepared into earlier in the plastic basis material that antibacterial matrices adds above-mentioned kind again to and be prepared into antibiotic plastic.Having added its mechanical property of antibiotic plastic of the present composition and un-added corresponding base material plastics mechanical property differs and is no more than 10%.
Embodiment 1
The 100g zeolite is added in the 200ml deionized water, stirs and be heated to 98 ℃, keep 60min, stop thermal precipitation, topple over and fall supernatant.Zn (the NO that adds 3ml30%
3)
2The ZnSO of solution and 100ml40%
4Solution is heated with stirring to 65 ℃ of reaction 240min, adds the 0.5g dispersant, stirs 10min, stops heating.With the slurries oven dry, pulverize after the cooling.Add the 40gZnO powder then, mix, promptly get bactericidal composition of the present invention with high-speed mixer.
Embodiment 2
The 100g zeolite is added to the AgNO of the 200ml1% for preparing in advance
3In the solution, the back heat temperature raising to 95 ℃ that stirs keeps stirring 100min under this temperature, stops then stirring and heating, 30% the Zn (NO that adds after staticly settling that 200ml prepares in advance
3)
2Solution stirs and is heated to 75 ℃, and keeps stirring 300min under this temperature, adds the 0.5g dispersant again, stir 10min, stop heating, with the slurries oven dry, pulverize after the cooling, add 5 parts of ZnO powders then, mix, promptly get inorganic antibacterial composition of the present invention with high-speed mixer.
Embodiment 3
The 100g zeolite is added in the 200ml deionized water, is heated with stirring to 97 ℃, under this temperature, keep stirring 80min, stop heating and be cooled to 70 ℃, add the 40%ZnSO for preparing in advance
4Solution 100ml, and remain under 65 ± 3 ℃ of conditions and stir 200min, add dispersant 0.5g, stir 10min, stop after heating and stirring, the cooling slurries being dried, being pulverized, add the 30gZnO powder again, mix with high-speed mixer, promptly get bactericidal composition of the present invention.
Claims (6)
1. a bactericidal composition is characterized in that described composition comprises following component and content (weight
Part):
Constituent content
AgNO3 0-2
Zn(NO3)2 0.1-60
ZnSO4 40
ZnO 5-80
Dispersant 0.5
Zeolite 100
2. a kind of bactericidal composition according to claim 1 is characterized in that described composition comprises following component and content (weight portion):
Constituent content
AgNO3 0-2
Zn(NO3)2 20-50
ZnSO4 40
ZnO 20-50
Dispersant 0.5
Zeolite 100
3. a kind of bactericidal composition according to claim 1 is characterized in that described dispersant is CA-977, HYDROPALAT or SN-DISPERSANT.
4. the preparation method of a kind of bactericidal composition according to claim 1 is characterized in that step is carried out in the following order:
(1) by weight the ZnSO4 of 2 and 40 parts of the Zn (NO3) of the AgNO3 of 0-2 part, 0.1-60 part is mixed with the AgNO3 solution of 0-5% respectively with deionized water, 10%～saturated Zn (NO3) 2 and ZnSO4 solution for later use,
(2) in above-mentioned AgNO3 solution, add 100 parts of zeolites, be heated to 80 ℃～boiling, precipitate and topple over supernatant after in the slurries beds of precipitation, add above-mentioned Zn (NO3) 2 and ZnSO4 solution, be heated to 60～90 ℃, reaction 60～300min,
(3) add 0.5 part of dispersant in above-mentioned slurries, oven dry is ground into the pressed powder of particle diameter less than 30 μ,
(4) ZnO powder of adding 5-80 part in the above-mentioned pressed powder that obtains is made bactericidal composition of the present invention.
5. the preparation method of a kind of bactericidal composition according to claim 4.It is characterized in that described Zn (NO3) 2 is 20-40 part.
6. the preparation method of a kind of bactericidal composition according to claim 4.It is characterized in that described ZnO is 30-40 part.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98124542A CN1086270C (en) | 1998-11-12 | 1998-11-12 | Antifungal composition and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98124542A CN1086270C (en) | 1998-11-12 | 1998-11-12 | Antifungal composition and its preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1253729A CN1253729A (en) | 2000-05-24 |
| CN1086270C true CN1086270C (en) | 2002-06-19 |
Family
ID=5228694
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98124542A Expired - Fee Related CN1086270C (en) | 1998-11-12 | 1998-11-12 | Antifungal composition and its preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1086270C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100382706C (en) * | 2005-03-08 | 2008-04-23 | 中国农业科学院农业环境与可持续发展研究所 | Seeds capsule agent for preventing diseases spread by soil and seeds |
| JP5089055B2 (en) * | 2006-02-22 | 2012-12-05 | 株式会社シナネンゼオミック | Antibacterial zeolite and antibacterial composition |
| JP5027452B2 (en) | 2006-06-22 | 2012-09-19 | 株式会社シナネンゼオミック | Antibacterial zeolite particles and antibacterial resin composition |
| CN100479712C (en) * | 2007-09-13 | 2009-04-22 | 北京光华五洲纺织集团公司 | Health-care antimicrobial towel pillowcase |
| CN102550604A (en) * | 2011-12-22 | 2012-07-11 | 广东壮丽彩印股份有限公司 | Antibacterial agent, antibacterial gloss oil with antibacterial agent and preparation method and using method for antibacterial gloss oil |
| CN104206418A (en) * | 2014-08-07 | 2014-12-17 | 蔡惠萍 | Preparation method and application of discoloration-preventing powdery silver-containing anti-bacterial agent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60100504A (en) * | 1983-11-07 | 1985-06-04 | Zenji Hagiwara | Antibacterial composition and its production |
| JPH08268822A (en) * | 1995-03-31 | 1996-10-15 | Toppan Printing Co Ltd | Antibacterial agent and its production |
-
1998
- 1998-11-12 CN CN98124542A patent/CN1086270C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60100504A (en) * | 1983-11-07 | 1985-06-04 | Zenji Hagiwara | Antibacterial composition and its production |
| JPH08268822A (en) * | 1995-03-31 | 1996-10-15 | Toppan Printing Co Ltd | Antibacterial agent and its production |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1253729A (en) | 2000-05-24 |
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