CN1692735A - Antibiosis material of low cost, and its prepn. method - Google Patents

Antibiosis material of low cost, and its prepn. method Download PDF

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Publication number
CN1692735A
CN1692735A CN 200510046465 CN200510046465A CN1692735A CN 1692735 A CN1692735 A CN 1692735A CN 200510046465 CN200510046465 CN 200510046465 CN 200510046465 A CN200510046465 A CN 200510046465A CN 1692735 A CN1692735 A CN 1692735A
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Prior art keywords
tio
activation
biotic material
titaniferous
slag
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CN100381053C (en
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薛向欣
杨合
董学文
段培宁
刘卯
赵娜
姜涛
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Northeastern University China
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Northeastern University China
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Abstract

A low-cost antibacterial material is prepared from the Ti-contained material containing TiO2 (more than wt.%) and selective metal, metal compound or metal salt through grinding, proportional mixing, calcining, optical radiation and sealing.

Description

A kind of antibiosis material of low cost and manufacture method thereof
Technical field
The invention belongs to the anti-biotic material technical field, a kind of antibiosis material of low cost and manufacture method thereof promptly are provided.
Background technology
The reaction of semi-conducting material multiphase photocatalysis has obtained going deep into extensive studies, and the semiconductor light-catalyst of broad research has TiO at present 2, ZnO, CdS, WO 3, Fe 2O 3, PbS, SnO 2, In 2O 3, ZnS, SrTiO 3, SiO 2Deng tens kinds.These conductor oxidates all have certain photocatalytic activity, but wherein most of chemistry or photochemical corrosion of easily taking place.
TiO 2Having characteristics such as good chemical stability and nontoxic, non-secondary pollution, oxidability are strong, catalytic activity height, is good anti-biotic material, but pure TiO 2The cost height.
Though titanium is a kind of relatively rich in natural resources in China, most titanium resources mainly are and the iron symbiosis that grade is low, does not reach the level of direct development and use.Iron and Steel Enterprises in China extracts iron when developing iron resource in a large number in ilmenite, other element in the mineral is not then made full use of, and not only causes the wasting of resources, and forms a large amount of titanium-contained slags, contaminated environment.
Summary of the invention
The present invention proposes a kind of anti-biotic material of titaniferous, it is characterized in that adopting percetage by weight to calculate and contain TiO 2Titaniferous material greater than 16.03 is a raw material, and excites through levigate, calcination activation and illumination and to form.
Titaniferous anti-biotic material of the present invention, it is characterized in that can be in titaniferous material doping metals simple substance, metallic compound or slaine, with its anti-microbial property of further raising.
The invention allows for a kind of method of making above-mentioned titaniferous anti-biotic material, it is characterized in that calculating by weight percentage and contain TiO 2Titaniferous material greater than 16.03 is made raw material, is undertaken by following key step:
(1) grinding is with ball milling or the levigate titaniferous material of airflow milling, and its average grain diameter reaches below 2 microns, removes wherein iron filings with electromagnetic field;
(2) the doping batch mixing is milled to average grain diameter with metal simple-substance, metallic compound or slaine and reaches below 2 microns, evenly mixes with levigate titaniferous material;
(3) calcination activation is under 600～1000 degree celsius temperature, and roasting 1～3 hour is cooled to room temperature in the air;
(4) to excite and adopt wavelength be the UV-irradiation 5～50 minutes of 253.7 nanometers in illumination;
(5) sealing, packing.
Above-mentioned metal simple-substance can be Ca, Fe, Zn, and metal oxide can be MgO, CaO, V 2O 5, said metallic salt can be AgCl, BaSiO 3, CaCO 3Above-mentioned illumination excitation process also can adopt sunlight irradiation, and its light application time can be 10～60 minutes.
Anti-biotic material provided by the present invention is raw material with the titaniferous material, excites the technology manufacturing to form through simple grinding, high-temperature roasting activation and illumination.Its technology is easy, manufacturing cost is lower, product can be widely used in fields such as building materials, weaving, medical and health, chemical industry, not only solved the pollution problem that the stacking of a large amount of Ti-containing slags brings to environment, and developing and using limited titanium resource more effectively, have good social benefit and economic benefit.
Embodiment
Below in conjunction with concrete embodiment content of the present invention is described further and replenishes.
The titaniferous material that the present invention adopts comprises high titanium slag, ilmenite concentrate, Panzhihua Iron blast furnace slag (climbing slag) and Chengde Iron ﹠ Steel Corp.'s blast furnace slag (holding slag), and wherein high titanium slag is to come from jinzhou Ferroalloy Plant, and ilmenite concentrate is from Qinglan ore deposit, Hainan.
Embodiment 1
Slag is climbed in employing, wherein TiO 2Be 23.16wt%, contain the about 1.85wt% of Fe, contain SiO 224.01wt%, MgO 7.47wt%, Al 2O 313.49wt%, CaO 27.19wt%, V 2O 50.23wt% is a raw material.
Through fragmentation and grinding, its particle mean size reaches below 2 microns with above-mentioned titanium-contained slag.After the electromagnetism deironing, the titaniferous ground-slag is put into roaster, carry out activation processing, its technology is that micro mist is heated to 600 ℃, is incubated and naturally cools to room temperature after 3 hours.Not to wherein mixing.
With the ground-slag after the ultraviolet radiation activated of wavelength 253.7 nanometers 5 minutes, excite processing further.After above-mentioned ultraviolet excitation is handled, promptly made and contained TiO 2Anti-biotic material.Can dispatch from the factory after sealing, the packing.
Embodiment 2
Adopt the 50.89wt%TiO that contains of jinzhou Ferroalloy Plant 2High titanium slag is made raw material, the following operation of process:
(1) after grinding selects for use cracker that high titanium slag is crushed to about 100 microns, used ball milling again 48 hours, its average grain diameter reaches below 2 microns, and with electromagnetic field removal iron filings wherein, makes the Fe amount below 4wt%;
(2) the doping batch mixing adds the Zn powder of metal 5wt%, the MgO powder of 5wt%, the V of 20wt% 2O 5The AgCl powder of powder and 5wt% further is ground to average grain diameter again and reaches below 2 microns;
(3) calcination activation places roaster with above-mentioned micro mist, is heated at 800 ℃, is incubated 2 hours, is cooled to room temperature;
(4) illumination excites with the solar irradiation solarization and further excited processing in 60 minutes;
(5) sealing, packing.
Embodiment 3
Adopt Chengde Iron ﹠ Steel Corp.'s blast furnace slag to make raw material, in chemically examining this slag, contain TiO 2Be 16.03wt%, contain the about 0.40wt% of Fe, MgO 14.89wt%, Al 2O 324.94wt%, CaO 32.12wt%.The following operation of process:
(1) after grinding selects for use cracker that Chengde Iron ﹠ Steel Corp.'s blast furnace slag is crushed to about 100 microns, use ball milling about 8 hours again, its average grain diameter reaches below 2 microns, and is less because of iron content, need not use Magnetic Isolation;
(2) the doping batch mixing adds the AgCl micro mist of 12wt%, reaches below 2 microns with ball mill grinding to average grain diameter, and holds the slag micro powder mixing;
(3) slag micro powder that holds that contains AgCl that calcination activation is good with above-mentioned mixing places roaster, is heated to 1000 ℃, is incubated 1 hour, is cooled to room temperature;
(4) illumination excites the slag micro powder that holds that contains AgCl after the activation is shakeout, and is the UV-irradiation 50 minutes of 253.7 nanometers with wavelength, is further excited;
(5) sealing, packing.
Embodiment 4
Adopting the high titanium slag of jinzhou Ferroalloy Plant is raw material, contains TiO in chemically examining this slag 2Be 50.89wt%, contain the about 28.40wt% of Fe, SiO 2Be 4.64wt%, MgO 0.39wt%, Al 2O 32.14wt%, CaO0.46wt%, V are 0.049wt%.Make anti-biotic material of the present invention according to the following steps:
(1) grinding is with aforesaid embodiment 2;
(2) the doping batch mixing adds metal simple-substance Cu 2wt%, Zn 4wt%, compd A gCl 25wt% and CaCO 35wt% reaches below 2 microns with ball mill grinding to average grain diameter, with high titanium slag micro mist mixing mutually;
(3) the high titanium slag micro mist that contains AgCl that calcination activation is good with above-mentioned mixing places roaster, adopts different temperatures to activate, and temperature retention time all is decided to be 2 hours, and temperature is 600 ℃, 800 ℃, 1000 ℃, takes out to be cooled to room temperature;
(4) illumination excites the high titanium slag micro mist that contains AgCl after the activation is shakeout, and is the UV-irradiation 50 minutes of 253.7 nanometers with wavelength, is further excited;
(5) sealing, packing.
Get the anti-biotic material of different sintering temperature activation respectively, every part is standard with 0.75g.Select 0.75g to consider of the influence of the weight of sample,, thereby influence the accuracy of experimental result because medium is easy to be damaged under big pressure to meat extract peptone agar medium.In order to improve the mouldability of slag charge powder, when compressing tablet, add an amount of absolute ethyl alcohol, use the forming under the pressure of the mould of Φ 12mm behind the mixing at 10MPa, put into baking oven then and under 80 ℃ of conditions, dry stand-by.
The antibiotic property experiment is mainly investigated product to colibacillary kill activity, the Escherichia coli that bacterial strain is adopted international standards (ATCC8099 is a reference culture).Through behind the concentration proportioning, selecting concentration for use is that the Escherichia coli bacteria liquid of 106CFU/ml is as experimental subjects.Bacterium liquid is evenly coated in the sterile petri dish that contains meat extract peptone agar medium, make it form uniform bacterium liquid film, be placed on sample in the culture dish gently then, integral body is put into incubator and was cultivated 18 hours down in 37 ℃, bacterial growth situation around the observation sample, and measure antibacterial ring.Experimental result sees Table 1.
The anti-microbial property of titanium-contained slag behind the different sintering temperatures of table 1
Temperature Transparent antibacterial ring thickness (mm) On average
Sample one Sample two Sample three
????600℃ ????2.4 ????2.1 ????1.8 ????2.1
????800℃ ????4.1 ????3.4 ????3.8 ????3.8
????1000℃ ????1.8 ????2.3 ????1.9 ????2.0
Antibacterial ring is big more, and antibiotic property is good more, so as can be seen with 800 ℃ of temperature calcination activations, performance the best.
Embodiment 5
It is raw material, wherein TiO that slag is climbed in employing 2Be 23.16wt%, contain the about 1.85wt% of Fe, contain SiO 224.01wt%, MgO 7.47wt%, Al 2O 313.49wt%, CaO 27.19wt%, V 2O 50.23wt%.
(1) grinding selects for use cracker will climb slag crushing after about 100 microns, reaches below 2 microns with ball milling to its average grain diameter again;
(2) the doping batch mixing adds Cu 4wt%, Zn 2wt%, adds BaSO again 44wt% and V 2O 512wt% reaches below 2 microns with ball mill grinding to average grain diameter, and the batch mixing mixing;
(3) calcination activation places roaster with the titanium-contained slag micro mist of above-mentioned mixing, is heated to 800 ℃, is incubated 2 hours, takes out to be cooled to room temperature;
(4) illumination excites the doping titanium-contained slag micro mist after the activation is divided into three parts, after shakeouing respectively with the ultraviolet light of 253.7 nanometers auxilliary according to, sunshine directly shines and nature 30 minutes;
(5) sealing, packing.
The sample that the illumination that above-mentioned employing is different excites is investigated its antibacterial effect by embodiment 4 used antibiotic property experimental technique and steps, and present embodiment is experimental subjects with staphylococcus aureus (ATCC6538 reference culture), and is as shown in table 2.
Three kinds of illumination of table 2 excite the anti-microbial property of back titanium-contained slag
Illumination condition Transparent antibacterial ring thickness (mm) On average
Sample one Sample two
Nature ????3.1 ????3.2 ????3.15
Sunshine ????4.4 ????3.9 ????4.15
Ultraviolet light ????4.8 ????4.6 ????4.7
As seen after ultraviolet light and sunshine excited, the anti-microbial property of material truly had raising.
Embodiment 6
Adopt Chengde Iron ﹠ Steel Corp.'s blast furnace slag to make raw material, carry out according to the following steps:
(1) grinding is seen embodiment 3;
(2) the doping batch mixing adds the AgCl of 0.5wt%, 3.5wt%V 2O 5Use ball mill powder process, and with hold the slag micro powder mixing;
(3) calcination activation is seen embodiment 3;
(4) illumination excited micro mist is shakeout, with sunshine direct projection 60 minutes;
(5) sealing, packing.
Embodiment 7
Adopt the ilmenite concentrate of Hainan Qinglan to make raw material, this ore contains TiO 2Be 54.5wt%, contain the about 35.33wt% of Fe, step is as follows:
(1) grinding separates skill and technique with electromagnetism behind the grinding Fe amount is controlled at below the 4wt% with embodiment 2;
(2) the doping batch mixing is for the influence to anti-biotic material of the addition of AgCl relatively, add 5,10,20 respectively, the AgCl of 35wt%, make five kinds of samples together with the sample that does not add AgCl, be ground to average grain diameter and reach below 2 microns, evenly mix with the ilmenite concentrate micro mist behind the de-iron;
(3) the calcination activation method is with embodiment 2, and roasting condition is 800 ℃, is incubated 2 hours, is cooled to room temperature in the air;
(4) illumination excited UV-irradiation 30 minutes;
(5) sealing, packing.
Five samples that difference contained the AgCl amount carry out the anti-microbial property experiment by the method for embodiment 4, are experimental subjects with staphylococcus aureus (ATCC6538 reference culture).It the results are shown in table 3.
The anti-microbial property of the titanium-contained slag of three kinds of AgCl proportionings of table 3
AgCl％(wt％) Transparent antibacterial ring thickness (mm) On average
Sample one Sample two Sample three
????0％ ????4.6 ????4.4 ????5.0 ????4.7
????5％ ????6.5 ????6.5 ????6.5 ????6.5
????10％ ????6.5 ????7 ????6.5 ????6.7
????20％ ????7 ????7 ????6.5 ????6.8
????35％ ????7.5 ????7 ????7 ????7.2
Obviously, the introducing of silver ion has increased the anti-microbial property of titanium-contained slag, but higher relatively because of the AgCl cost, from practicality, needs only the AgCl that adds 0.1～5wt%.
Embodiment 8
Adopt the ilmenite concentrate of Hainan Qinglan to make raw material, its step repeats no more with embodiment 7.
In order to compare V 2O 5Addition to influence to anti-biotic material, in the doping compounding process, add 5,10,20 respectively, the V of 35wt% 2O 5, together with not adding V 2O 5Sample make five samples by method and the step of embodiment 7, the method for being narrated by embodiment 4 is carried out anti-microbial property test again, is experimental subjects with staphylococcus aureus (ATCC6538 reference culture).As shown in table 4.
The different V of table 4 2O 5The anti-microbial property of the titanium-contained slag of proportioning
V 2O 5％(wt％) Transparent antibacterial ring thickness (mm) On average
Sample one Sample two Sample three
????0％ ????4.6 ????4.4 ????5.0 ????4.7
????5％ ????9.5 ????9 ????10.5 ????9.7
????10％ ????9.5 ????9.5 ????10 ????9.7
????20％ ????9 ????9.5 ????9 ????9.1
????35％ ????9 ????9.5 ????10 ????9.5
Visible V in the table 2O 5Raising effect to titanium-contained slag micro mist anti-microbial property is more obvious.As long as add the V of 5wt% 2O 5Just can obtain remarkable result.

Claims (6)

1. a low cost is characterized in that adopting calculating by weight percentage containing TiO with the anti-biotic material that titaniferous material prepares 2Titaniferous material greater than 16.03% is a raw material, and excites through pulverizing, calcination activation and illumination and to form.
2. by the described TiO that contains of claim 1 2Anti-biotic material, it is characterized in that in the described material can doped metallic elements, metal oxide or slaine.
3. by the described TiO that contains of claim 2 2Anti-biotic material is characterized in that the described metallic element that mixes can be iron, zinc or copper.
4. by the described TiO that contains of claim 2 2Anti-biotic material is characterized in that the described metal oxide that mixes can be magnesia, aluminium oxide, calcium oxide or vanadium oxide.
5. by the described TiO that contains of claim 2 2Anti-biotic material is characterized in that the described slaine that mixes can be silver chlorate, barium sulfate or calcium carbonate.
6. a manufacturing is characterized in that being undertaken by following step by the method for the described anti-biotic material of claim 1:
(1) grinding with the titaniferous material ball mill grinding after, its average grain diameter reaches below 2 microns;
(2) the doping batch mixing adds metal simple-substance, metallic compound or slaine, is milled to average grain diameter and reaches below 2 microns, evenly mixes with levigate titaniferous material;
(3) calcination activation will mix contains TiO 2Micro mist is positioned over the roaster heat-activated, and activation temperature is 600～1000 ℃, is incubated 1～3 hour, is cooled to room temperature in the air;
(4) illumination excites the TiO that contains after the activation 2Micro mist shakeouts, and is auxilliary according to 5～50 minutes with the ultraviolet light of wavelength 253.7 nanometers, perhaps uses solar light irradiation 10～60 minutes;
(5) sealing, packing are dispatched from the factory.
CNB2005100464651A 2005-05-20 2005-05-20 Antibiosis material of low cost, and its prepn. method Expired - Fee Related CN100381053C (en)

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Cited By (7)

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CN105056269A (en) * 2015-08-28 2015-11-18 保护伞环保科技成都有限公司 Indoor air purification agent
CN106378126A (en) * 2016-08-16 2017-02-08 辽宁石油化工大学 A vanadium-doped titanium-containing blast furnace slag photocatalytic antibacterial material responsive to visible light and a preparing method thereof
WO2017045432A1 (en) * 2015-09-16 2017-03-23 苏州科大微龙农业科技有限公司 Nano-titanium and biological-sulfur-zinc-manganese mixture for melon powdery mildew
CN108772084A (en) * 2018-06-07 2018-11-09 郑州轻工业学院 TiO with photocatalysis antibacterial performance2/Cu2(OH)2CO3The preparation method and application of composite nano materials
CN108823671A (en) * 2018-07-13 2018-11-16 合肥洁诺医疗用品有限公司 A kind of preparation method of surgical operation towel antibiotic ultraviolet-resistant non-woven fabrics
CN112136830A (en) * 2020-09-15 2020-12-29 青岛亿恩方能源环保科技有限公司 Photocatalyst sterilization disinfectant based on Ag and N co-doped titanium dioxide/silver nitrate and preparation method and application thereof
CN113209959A (en) * 2021-05-12 2021-08-06 昆明理工大学 Preparation method of load type rod-shaped magnesium oxide composite antibacterial agent

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JPH06157224A (en) * 1992-11-27 1994-06-03 Sangi Co Ltd Antibacterial/antifungal agent for food or feed
CN1256868A (en) * 1998-12-16 2000-06-21 王志群 Compound silver series inorganic germifuge
CN1228397C (en) * 2002-05-20 2005-11-23 中山市华铿喷涂有限公司 Silver phosphate antibacterial modified titanium dioxide composite particle and its preparation method and use
CN1171669C (en) * 2002-05-31 2004-10-20 东北大学 Method for preparing photocatalysis material by using iron blast-furnace slag containing titanium

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105056269A (en) * 2015-08-28 2015-11-18 保护伞环保科技成都有限公司 Indoor air purification agent
WO2017045432A1 (en) * 2015-09-16 2017-03-23 苏州科大微龙农业科技有限公司 Nano-titanium and biological-sulfur-zinc-manganese mixture for melon powdery mildew
CN106378126A (en) * 2016-08-16 2017-02-08 辽宁石油化工大学 A vanadium-doped titanium-containing blast furnace slag photocatalytic antibacterial material responsive to visible light and a preparing method thereof
CN108772084A (en) * 2018-06-07 2018-11-09 郑州轻工业学院 TiO with photocatalysis antibacterial performance2/Cu2(OH)2CO3The preparation method and application of composite nano materials
CN108772084B (en) * 2018-06-07 2021-06-18 郑州轻工业学院 TiO with photocatalytic antibacterial property2/Cu2(OH)2CO3Preparation method and application of composite nano material
CN108823671A (en) * 2018-07-13 2018-11-16 合肥洁诺医疗用品有限公司 A kind of preparation method of surgical operation towel antibiotic ultraviolet-resistant non-woven fabrics
CN112136830A (en) * 2020-09-15 2020-12-29 青岛亿恩方能源环保科技有限公司 Photocatalyst sterilization disinfectant based on Ag and N co-doped titanium dioxide/silver nitrate and preparation method and application thereof
CN113209959A (en) * 2021-05-12 2021-08-06 昆明理工大学 Preparation method of load type rod-shaped magnesium oxide composite antibacterial agent
CN113209959B (en) * 2021-05-12 2023-01-24 昆明理工大学 Preparation method of load type rod-shaped magnesium oxide composite antibacterial agent

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