CN1385076A - Nano phosphate antibiosis composition and process for preparing same - Google Patents
Nano phosphate antibiosis composition and process for preparing same Download PDFInfo
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- CN1385076A CN1385076A CN 02102186 CN02102186A CN1385076A CN 1385076 A CN1385076 A CN 1385076A CN 02102186 CN02102186 CN 02102186 CN 02102186 A CN02102186 A CN 02102186A CN 1385076 A CN1385076 A CN 1385076A
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Abstract
The present invention relates to a nano phosphate antibacterial compound and its preparation method. Said invention adopts nano technology and utilizes the control of its components of NH4H2PO4, AgNO3, ZnSO4 and nano zirconium phosphate, etc. and their contents and steps of said preparation method to prepare said invented product. Said nano phosphate antibacterial compound possesses good colour stability, good antibacterial broad-spectrum property, good physical, mechanical and optical properties, can be used in the high temp. materials of ceramics and building material, and can obtain good antibacterial effect.
Description
Technical field: the present invention relates to a kind of inorganic antibacterial composition, especially for nano phosphate antibiosis composition in the processing of high-temperature materials such as pottery, building materials and preparation method thereof.
Background technology: in the application of ecological environment material nd, common organic antibacterial agent, inorganic antiseptic is because it is easy to change, defectives such as temperature tolerance difference, people can't have been satisfied to antibiotic, the requirement of environment purification and combination property, especially at pottery, environment building materials aspects such as building materials are particularly outstanding, for this reason, SUMITOMO CHEMICAL cement (strain) discloses a kind of antifouling paint series of patents (spy opens flat 8-143791.1996.), SHMITOMO CEMENTCO.LTD discloses a kind of composite antibiosis glaze patent (WO94/27442.1994.PCT/JP94/00873), and China Building Materials Academy discloses a kind of health care, the patent of antibiotic multifunction ceramic glaze and ceramic thereof (notification number 1151381).But above-mentioned antibacterial agent exists still that the antibacterial metal ions dissolution rate is wayward, and weather resistance is poor, especially is applied in other material deficiencies such as bad dispersibility.In addition, the application of antibacterial agent mainly is compound with other material, after in adding other material to, this material only has antibacterial functions, combination properties such as the physics of material, mechanics, optics all can not get improving, especially after being applied in the materials such as pottery, building materials, combination property difference etc. are excellent in outstanding.
Summary of the invention: the present invention is based on the problems referred to above, it mainly is the applying nano technology, new prescription of synthesis of nano phosphate antibiosis composition and preparation method thereof is proposed, solve the lability of existing antibacterial agent performance in the processing of high-temperature materials such as pottery, building materials, and nano phosphate antibiosis composition with combination properties such as good weather resisteant and physics, mechanics, optics, widen its range of application, improve application level.
Nano phosphate antibiosis composition of the present invention is to realize by following proportioning and preparation method.The component and the content of its proportioning is (weight portion): NH
4H
2PO
40.5～5 parts, AgNO
30.2～6 parts, ZnSO
42～80 parts, 0.5～2 part of dispersant, 100 parts of nanometer basic zirconium phosphates.Its component and content of optimizing proportioning is: NH
4H
2PO
40.5～4 parts, AgNO
30.2～5 parts, ZnSO
42～70 parts, 0.5～2 part of dispersant, 100 parts of nanometer basic zirconium phosphates.Its preparation method carries out according to the following steps: (1) gets ZrOCl according to 2: 1: 3 ratio
28H
2The O aqueous solution adds C
2O
4H
2Stir, add H again
3PO
4Be mixed with solution, the NaOH aqueous solution with 20% is regulated PH=4～6, precipitation, filtration, washing, drying make powder, again powder are placed autoclave, are medium with the deionized water, NaF is that mineralizer carries out hydro-thermal reaction, 100 ℃～330 ℃ of reaction temperatures, reaction time 2～5h, 1.5 ℃/min of heating rate.Make nanometer basic zirconium phosphate powder of the present invention.(2) by weight with 0.2～6 part AgNO
3Be made into 0%～5% AgNO with deionized water
3Solution is with 2～80 parts Z
nSO
4NH with 0.5～5 part
4H
2PO
4, be made into 10% to the full ZnSO that closes with deionized water
4Solution and NH
4H
2PO
4Solution for later use.(3) get 100 parts nanometer basic zirconium phosphate powder and add deionized water and make aqueous suspensions, add AgNO
3Solution is heated to 70 ℃～95 ℃ post precipitations, outwells supernatant, adds ZnSO again
4Solution and NH
4H
2PO
4Solution is heated to 80 ℃～100 ℃, carries out displacement reaction 2～6h.(4) after displacement reaction finishes, add 0.5～2 part dispersant, stir.(5), spend deionised water, oven dry, grinding with above-mentioned dope filtration, separation.(6) powder with oven dry carries out 900 ℃～1200 ℃ high temperature treatment 3-12h, obtains nano phosphate antibiosis composition of the present invention.
The nano phosphate antibiosis composition that the present invention makes, every after testing performance is: bacteriostasis rate: to Escherichia coli, staphylococcus aureus, Candida albicans bacteriostasis rate is 92%～99%, the minimum growth stops concentration (MIC) 62.5PPm; Antibiotic durability index: after 3 months, antibiotic rate still is 92%～99% through acid, alkaline medium dipping; Safety: per os determination of acute toxicity, true border innocuous substance; Warm tolerance: under 1000 ℃～1300 ℃ temperature, bacteriostasis rate is 99%, and silver-colored volatility only is 1.5%～2%; Value of chromatism: with aberration difference DELTA E≤0.7～1 of tester.Average particle size: press GB/T13221-91, X-ray small-angle scattering method, in the test of the little angle of 3014X optical diffraction instrument-Kratky angular instrument, average particle size is 50nm, and narrow distribution.Physical and mechanical property: composition of the present invention added in the pottery detect microhardness: detect at HX-1000J type microhardness testers: 600～630Mpa; Glossiness: use SS-75 type electric light gloss meter to detect: 100～105; Whiteness: use WSD-III type leucometer to detect: 80～88; Thermal shock resistance: 200 ℃～20 ℃ water once do not split; Water absorption rate: performance such as≤0.3% all meets national household china standard.
Embodiment: embodiment 1:(1), get ZrOCl according to 2: 1: 3 ratio
28H
2The O aqueous solution adds C
2O
4H
2Stir, add H again
3PO
4Be mixed with solution, regulate PH=4 with the 20%NaOH aqueous solution, precipitation, filtration, washing, drying make powder, powder are placed 250ml cartridge type autoclave again, are medium with the deionized water, NaF is that mineralizer carries out hydro-thermal reaction, 100 ℃～330 ℃ of reaction temperatures, reaction time 2～3h, 1.5 ℃/min of heating rate.Make nanometer basic zirconium phosphate powder of the present invention.(2) by weight with 0.2 part AgNO
3Be made into 0%～5% AgNO with deionized water
3Solution is with 2 parts ZnSO
4NH with 0.5 part
4H
2PO
4Be made into 10% to the full ZnSO that closes with deionized water
4Solution and NH
4H
2PO
4Solution for later use.(3) 100 parts nanometer basic zirconium phosphate powder is added deionized water and make aqueous suspensions, add AgNO
3Solution is heated to 70 ℃～95 ℃ post precipitations, outwells supernatant, adds ZnSO again
4Solution and NH
4H
2PO
4Solution is heated to 80 ℃～100 ℃, carries out displacement reaction 2～6h.(4) after displacement reaction finishes, add (OX-3000) dispersant of 0.5 part, stir.(5), spend deionised water, oven dry, grinding with above-mentioned dope filtration, separation.(6) powder with oven dry carries out handling 3～12h under 900 ℃～1200 ℃ high temperature, obtains nano phosphate antibiosis composition of the present invention.
Embodiment 2: according to the method for embodiment 1, the proportioning of getting component and content is (weight portion): 5 parts NH
4H
2PO
4, 6 parts AgNO
3, 80 parts ZnSO
4, 2 parts dispersant, 100 parts nanometer basic zirconium phosphate, under 1200 ℃ of high temperature, handle 6h.
Embodiment 3: according to the method for embodiment 1, the optimization proportioning of getting component and content is (weight portion): 4 parts NH
4H
2PO
4, 5 parts AgNO
3, 70 parts ZnSO
4, 2 parts dispersant, 100 parts nanometer basic zirconium phosphate, under 1100 ℃ of high temperature, handle 8h.
Embodiment 4: according to the method for embodiment 1, the best proportioning of getting component and content is (weight portion): 2 parts NH
4H
2PO
4, 4 parts AgNO
3, 40 parts ZnSO
4, 1.5 dispersant, 100 parts of nanometer basic zirconium phosphates, under 1150 ℃ of high temperature, handle 8h.
Claims (4)
1. nano phosphate antibiosis composition, its component and content are:
Constituent content
NH
4H
2PO
4 0.5～5
AgNO
3 0.2～6
ZnSO
4 2～80
Dispersant 0.5～2
Nanometer basic zirconium phosphate 100
Above proportioning is weight portion
2. the described a kind of nano phosphate antibiosis composition of root a tree name claim 1, its component and content are:
Constituent content
NH
4H
2PO
4 0.5～4
AgNO
3 0.2～5
ZnSO
4 2～70
Dispersant 0.5～2
Nanometer basic zirconium phosphate 100
Above proportioning is weight portion
3. the described a kind of nano phosphate antibiosis composition of root a tree name claim 1, dispersant wherein is: OX-N120 or HDP-3000.
4. the described a kind of nano phosphate antibiosis composition of root a tree name claim 1, the preparation method of said composition follows these steps to carry out:
(1) according to 2: 1: 3 ratio, gets ZrOCl
28H
2The O aqueous solution adds C
2O
4H
2Stir, add H again
3PO
4Be mixed with solution, the NaOH aqueous solution with 20% is regulated pH=4～6, precipitation, filtration, washing, drying make powder, again powder are placed autoclave, are medium with the deionized water, NaF is that mineralizer carries out hydro-thermal reaction, 100 ℃～330 ℃ of reaction temperatures, reaction time 2～5h, 1.5 ℃/min of heating rate.Make nanometer basic zirconium phosphate powder of the present invention.
(2) by weight with 0.2～6 part AgNO
3Be made into 0%～5% AgNO with deionized water
3Solution is with 2～80 parts ZnSO
4NH with 0.5～5 part
4H
2PO
4, be made into 10% to the full ZnSO that closes with deionized water
4Solution and NH
4H
2PO
4Solution for later use.
(3) get 100 parts nanometer basic zirconium phosphate powder and add deionized water and make aqueous suspensions, add AgNO
3Solution is heated to 70 ℃～95 ℃ post precipitations, outwells supernatant, adds ZnSO again
4Solution and NH
4H
2PO
4Solution is heated to 80 ℃～100 ℃, carries out displacement reaction 2～6h.
(4) after displacement reaction finishes, add 0.5～2 part dispersant, stir.
(5), spend deionised water, oven dry, grinding with above-mentioned dope filtration, separation.
(6) powder with oven dry carries out 900 ℃～1200 ℃ high temperature treatment 3～12h, obtains nano phosphate antibiosis composition of the present invention.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021021864A CN1316894C (en) | 2002-01-21 | 2002-01-21 | Nano phosphate antibiosis composition and process for preparing same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021021864A CN1316894C (en) | 2002-01-21 | 2002-01-21 | Nano phosphate antibiosis composition and process for preparing same |
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| Publication Number | Publication Date |
|---|---|
| CN1385076A true CN1385076A (en) | 2002-12-18 |
| CN1316894C CN1316894C (en) | 2007-05-23 |
Family
ID=4739681
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021021864A Expired - Fee Related CN1316894C (en) | 2002-01-21 | 2002-01-21 | Nano phosphate antibiosis composition and process for preparing same |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100382705C (en) * | 2003-06-10 | 2008-04-23 | 香港理工大学 | Multifunctional broad spectrum nanometer antibiotic material and its preparation method |
| CN102239887A (en) * | 2010-12-03 | 2011-11-16 | 三达膜科技（厦门）有限公司 | Preparation method of nanoscale zirconium phosphate silver-carrying composite inorganic antimicrobial agent |
| CN102763678A (en) * | 2012-08-01 | 2012-11-07 | 晋大纳米科技（厦门）有限公司 | Method for preparing cubic zirconium phosphate silver-carrying antimicrobial powder |
| CN104170820A (en) * | 2013-05-22 | 2014-12-03 | 上海奇维纺织科技有限公司 | Nano-zinc protective silver ion-containing inorganic antibacterial powder and preparation method |
| CN111226917A (en) * | 2020-03-26 | 2020-06-05 | 深圳市亚微新材料有限公司 | Preparation method of zirconium hydrogen phosphate nano-silver antibacterial composite material |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0559308A (en) * | 1991-08-30 | 1993-03-09 | Toagosei Chem Ind Co Ltd | Antibacterial coating composition |
| JPH07165478A (en) * | 1993-12-13 | 1995-06-27 | Toagosei Co Ltd | Antimicrobial porcelain or enameled product |
-
2002
- 2002-01-21 CN CNB021021864A patent/CN1316894C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100382705C (en) * | 2003-06-10 | 2008-04-23 | 香港理工大学 | Multifunctional broad spectrum nanometer antibiotic material and its preparation method |
| CN102239887A (en) * | 2010-12-03 | 2011-11-16 | 三达膜科技（厦门）有限公司 | Preparation method of nanoscale zirconium phosphate silver-carrying composite inorganic antimicrobial agent |
| CN102239887B (en) * | 2010-12-03 | 2013-06-05 | 三达膜科技（厦门）有限公司 | Preparation method of nanoscale zirconium phosphate silver-carrying composite inorganic antimicrobial agent |
| CN102763678A (en) * | 2012-08-01 | 2012-11-07 | 晋大纳米科技（厦门）有限公司 | Method for preparing cubic zirconium phosphate silver-carrying antimicrobial powder |
| CN104170820A (en) * | 2013-05-22 | 2014-12-03 | 上海奇维纺织科技有限公司 | Nano-zinc protective silver ion-containing inorganic antibacterial powder and preparation method |
| CN111226917A (en) * | 2020-03-26 | 2020-06-05 | 深圳市亚微新材料有限公司 | Preparation method of zirconium hydrogen phosphate nano-silver antibacterial composite material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1316894C (en) | 2007-05-23 |
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Assignee: Huamei Sanitaryware Co., Ltd. Assignor: Taiyuan University of Technology Contract fulfillment period: 2008.2.13 to 2013.2.12 contract change Contract record no.: 2009440001093 Denomination of invention: Nano phosphate antibiosis composition and process for preparing same Granted publication date: 20070523 License type: Exclusive license Record date: 2009.8.6 |
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| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.2.13 TO 2013.2.12; CHANGE OF CONTRACT Name of requester: MEIHUA SANITARY APPLIANCE CO., LTD. Effective date: 20090806 |
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Granted publication date: 20070523 Termination date: 20150121 |
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