CN100432157C - Siliver-carried micron kaolin and its prepn. method - Google Patents
Siliver-carried micron kaolin and its prepn. method Download PDFInfo
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- CN100432157C CN100432157C CNB2006100393896A CN200610039389A CN100432157C CN 100432157 C CN100432157 C CN 100432157C CN B2006100393896 A CNB2006100393896 A CN B2006100393896A CN 200610039389 A CN200610039389 A CN 200610039389A CN 100432157 C CN100432157 C CN 100432157C
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Abstract
The present invention discloses a preparation method for micrometre kaolin with strong practicability, which comprises: coal series kaolin is adopted and is continuously stirred and react with two groups of reagent at a certain temperature for several hours until sufficient reaction is carried out; the micrometre kaolin of the present invention is obtained after filtration, wash and drying. When the product is used for absorbing silver, a satisfactory effect can be obtained. The material used by the preparation method has the advantages of wide source, strong practicability, mild reaction condition and no need of special devices.
Description
Technical field
The present invention relates to the preparation method that micron kaolin carries silver.The invention still further relates to novel method for preparing micrometer kaolin.
Background technology
Silver uses as antiseptic-germicide and is of long duration, and nineteen thirty-nine Hill etc. has proved that with laboratory facilities silver ions has sterilizing ability.Suitable material must be arranged as carrier as antiseptic-germicide, in the existing report, generally adopt sepiolite, wilkinite, zeolite, phosphoric acid salt, adsorptivity silica gel and glass etc. to do inorganic carrier, constitute inorganic carrying silver antimicrobials.For example: at " preparation research of sepiolite carrying silver antimicrobials " (Wuhan University Of Science and Engineering's journal 2003.8, reported 63-66) that the use sepiolite carries silver as carrier, in " development of coal-based carrying silver antimicrobials " (Coal Chemical Industry 2005,4, reported 27-30) that the use shenfu coal carries silver as carrier, at " preparation technology of nano silver-supported antibacterial powder body material and performance " (Chinese pottery 2001,2, reported with the nanometer zirconium phosphate to be the nano silver-supported antibacterial powder body material of carrier 1-3), " carried silver-colored TiO
2The preparation of inorganic anti-bacterial agent and performance study " (functional materials 2005,3 has been reported with TiO in 474-476)
2Carry silver as carrier, (nonmetalliferous ore 2001,9 uses natural montmorillonite to carry silvery as carrier in 17-18) and is equipped with antiseptic-germicide " carry silver-colored bentonitic an anti-microbial property research ".Yet the carrier in these reports all must could carry silver through ion exchange exchange silver, and there is discoloration problem in the carrying silver antimicrobials of acquisition.
Kaolinic major ingredient is silicon oxide and aluminum oxide, if can might improve the stability of silver ions with it as carrier, to delay its variable color process.There is abundant kaolin resource in China, but poor because of its ion-exchange capacity, can't adopt above-mentioned ion-exchange techniques to form the inorganic carrier of silver.Simultaneously, existing kaolin product, fineness is not enough, uses as carrier as need, need carry out ultra-fine processing, to improve its specific surface area.
Summary of the invention
The object of the invention provides a kind of Siliver-carried micron kaolin, with as a kind of new inorganic antiseptic; Provide a kind of step of this Siliver-carried micron kaolin few simultaneously, easy to operate, cost is low, reaction conditions is gentle preparation method.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of Siliver-carried micron kaolin comprises the following steps:
(1) be 1: 0.2～1: 0.1～0.5: 4～10 to mix by weight with kaolin powder, basic cpd, urea, water, induction stirring was reacted 4 hours to 12 hours, and described basic cpd is selected from one or both in sodium hydroxide, the yellow soda ash;
(2) with kaolinic weight in the step (1) be 1 part benchmark, add 1～3 part of Glacial acetic acid again, 0.05～0.2 portion of anion surfactant continues reaction 4 hours to 12 hours, filters, washing, oven dry, obtains the white powder solid;
(3) get above-mentioned pulverulent solids, add in the argentiferous ion solution, induction stirring at least 15 minutes, suction filtration, washing obtain described Siliver-carried micron kaolin.
In the technique scheme, described anion surfactant adopts Sodium dodecylbenzene sulfonate.
Optimized technical scheme in described step (1), heats in the time of stirring, makes temperature of reaction be controlled at 0 ℃～150 ℃.In described step (2), heat during reaction, temperature is controlled at 0 ℃～150 ℃.
In the technique scheme, described argentiferous ion solution can be a silver nitrate solution, and concentration is between 0.02M to 0.06M.
The preferred suction silver time is between 30 minutes to 2 hours.
Another kind of technical scheme, described argentiferous ion solution is a silver ammino solution.
The present invention asks for protection the Siliver-carried micron kaolin that adopts technique scheme to prepare simultaneously.
Among the present invention, kaolin reacts with second group reagent behind the first group reagent intercalation again, is used as the carrier of inhaling silver at last.
Because the technique scheme utilization, the present invention compared with prior art has following advantage:
1. the present invention has obtained a kind of new inorganic antiseptic Siliver-carried micron kaolin, and kaolin is through ultra-fine processing on the one hand, and specific surface area is big, silver ions is had good absorption and slow releasing function, on the other hand, because the existence of aluminium, improve the stability of silver ions, delayed its variable color process;
2. the present invention make that the whole process of preparation intercalation step is few, thereby environmental pollution is less by to intercalator and selection of process parameters;
3. raw material consumption of the present invention is few, and wide material sources obtain easily;
4. the present invention is simple to operate, does not need mechanical mill, and equipment requirements is low;
5. the reaction conditions gentleness of the inventive method, the time is short, can finish whole process in one day.
Description of drawings
Accompanying drawing 1 is the raw materials used kaolinic scanning electron microscope particle diameter synoptic diagram of product of the present invention;
Accompanying drawing 2 is the scanning electron microscope particle diameter synoptic diagram of the embodiment of the invention one product.
Embodiment
Below the present invention is further described:
Embodiment one: get 5 gram Coaseries kaolins, add 2.5 gram sodium hydroxide, 2.5 gram urea, 40 ml deionized water 75 ℃ of following induction stirring 4 hours, add 10 milliliters of Glacial acetic acid, 0.1 gram Sodium dodecylbenzene sulfonate, continue reaction 4 hours, suction filtration, wash with hot deionized water, get white powder, after 105 ℃ of oven dry, promptly obtain a micron kaolin, be further used for preparing Siliver-carried micron kaolin, productive rate is 99.7%.
Referring to accompanying drawing 2, the scanning electron microscope particle diameter synoptic diagram of described invention product.
Embodiment two: get 8 parts in embodiment one gained soil, every part 1 gram respectively adds 0.02M silver nitrate solution 10ml, and 30 ℃ of following induction stirring times were respectively suction filtration, washing 15 minutes, 30 minutes, 1 hour, 1.5 hours, 2 hours, 2.5 hours, 4 hours, 5 hours.Filtrate is with the ammonium thiocyanate solution titration of 0.04M, with the ferric ammonium sulfate agent of giving instruction, measures the silver amount that absorbs, and calculates and inhales silver-colored rate, inhales silver-colored rate (%) and is followed successively by 95.3,96.1,96.4,95.3,95.1,98.0,99.0.Show that totally the reaction times is long more, it is high more to inhale silver-colored rate.But several flex points are arranged, illustrate that absorption and desorb reach balance and need the regular hour, based on absorption reaction, as 15 minutes, 30 minutes, desorb reacted strong gradually after 1 hour, reaches balance at last after 4～5 hours in the short period of time.
Embodiment three: get embodiment one gained soil 1 gram, add 0.06M silver nitrate solution 10ml, operation is with embodiment two.Inhale silver-colored rate from 58.7% to 73.3%, equally can with the proportional relation of time.Though the numerical value of the silver-colored rate of corresponding suction is lower than the value of embodiment two, and absorb the value of the amount of silver much larger than embodiment two.
Embodiment four: get embodiment one gained soil 1 gram, add 0.06M silver nitrate solution 10ml, 38 ℃ of following induction stirring 10 hours, suction filtration, washing, filtrate titration.Inhaling silver-colored rate is 56.4%.
Embodiment five: get embodiment one gained soil 1 gram, add 0.06M silver nitrate solution 10ml, add several nitric acid, 25 ℃ of following induction stirring 1 hour, suction filtration, washing, filtrate titration.Inhaling silver-colored rate only is 0.8%.
Embodiment six: get embodiment one gained soil 1 gram, add 0.06M silver nitrate solution 10ml, add several nitric acid, 60 ℃ of following induction stirring 4 hours, suction filtration, washing, filtrate titration.Inhaling silver-colored rate only is 2.8%.
Embodiment seven: get embodiment one gained soil 1 gram, add 0.06M silver ammino solution 10ml, 30 ℃ of following induction stirring 40 minutes, suction filtration, washing, filtrate titration.Inhaling silver-colored rate is 66.6%.
Claims (6)
1. the preparation method of a Siliver-carried micron kaolin is characterized in that, comprises the following steps:
(1) be 1: 0.2～1: 0.1～0.5: 4～10 to mix by weight with kaolin powder, basic cpd, urea, water, induction stirring was reacted 4 hours to 12 hours, and described basic cpd is selected from one or both in sodium hydroxide, the yellow soda ash;
(2) with kaolinic weight in the step (1) be 1 part benchmark, add 1～3 part of Glacial acetic acid again, 0.05～0.2 portion of anion surfactant continues reaction 4 hours to 12 hours, filters, washing, oven dry, obtains the white powder solid;
(3) get above-mentioned pulverulent solids, add in the argentiferous ion solution, induction stirring at least 15 minutes, suction filtration, washing obtain described Siliver-carried micron kaolin.
2. method for preparing micrometer kaolin according to claim 1 is characterized in that: described anion surfactant adopts Sodium dodecylbenzene sulfonate.
3. method for preparing micrometer kaolin according to claim 1 is characterized in that: described argentiferous ion solution is a silver nitrate solution, and concentration is between 0.02M to 0.06M.
4. method for preparing micrometer kaolin according to claim 3 is characterized in that: inhale the silver time between 30 minutes to 2 hours.
5. method for preparing micrometer kaolin according to claim 1 is characterized in that: described argentiferous ion solution is a silver ammino solution.
6. adopt the Siliver-carried micron kaolin of the method acquisition of claim 1.
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| CN100432157C true CN100432157C (en) | 2008-11-12 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101347124B (en) * | 2008-06-20 | 2011-05-18 | 中国高岭土公司 | Method for preparing silver-carrying ion and copper ion kaolin anti-bacteria agent |
| CN101983568A (en) * | 2010-11-25 | 2011-03-09 | 中国地质大学（武汉） | Halloysite Ag-carrying antibacterial agent and preparation method thereof |
| CN105983386B (en) * | 2015-02-26 | 2019-04-30 | 天津市四维康环保科技发展有限公司 | A kind of preparation method of non-woven fabrics |
| CN107099056B (en) * | 2017-04-07 | 2019-04-12 | 宁波大学 | A kind of composite bactericidal additive and preparation method thereof |
| CN114753144A (en) * | 2022-04-26 | 2022-07-15 | 扬州锦茂新材料科技有限公司 | After-finishing method of high-color-stability antibacterial fabric |
| CN115058150B (en) * | 2022-07-02 | 2023-04-28 | 苏州中亚油墨有限公司 | High-glossiness composite ink for film printing and preparation method thereof |
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Non-Patent Citations (4)
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| 载银沸石的抗菌性能及热稳定性研究. 李殿超等.非金属矿，第26卷第3期. 2003 |
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