CN102428961A - Method for preparing nano MgO sustained-release sterilizing granules - Google Patents
Method for preparing nano MgO sustained-release sterilizing granules Download PDFInfo
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- CN102428961A CN102428961A CN2011103607192A CN201110360719A CN102428961A CN 102428961 A CN102428961 A CN 102428961A CN 2011103607192 A CN2011103607192 A CN 2011103607192A CN 201110360719 A CN201110360719 A CN 201110360719A CN 102428961 A CN102428961 A CN 102428961A
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Abstract
The invention discloses a method for preparing nano MgO sustained-release sterilizing granules. The method comprises the following steps of: 1) dissolving Fat-soluble chitosan in an aqueous solution of acetic acid to obtain a chitosan solution; 2) preparing an aqueous solution of sodium alga acid, and adding nano MgO powder to obtain a nano MgO turbid solution; 3) dripping the nano MgO turbid solution into the chitosan solution, stirring the reaction liquid for half an hour, and removing the liquid to obtain milky microspheres; 4) washing the obtained milky microspheres with distilled water; and 5) drying the microspheres to obtain the yellow nano MgO sustained-release sterilizing granules. The method has the advantages that: 1) raw materials such as sodium alga acid, chitosan and the like are wide in sources, low in prices, safe and nontoxic; 2) a gel is introduced, so that the nano MgO can be immobilized on a carrier and cannot be washed away by current; 3) through a sustained-release system, the pH of the system can be stabilized in an acceptable range; and 4) an operating process of reaction is simple, reaction conditions are easy to control, and the method is suitable for industrial production.
Description
Technical field
The invention belongs to the nano material preparation technical field, be specifically related to a kind of preparation method of nano-MgO slow-release disinfection particle.
Background technology
Nano-MgO is the meticulous inorganic material of a kind of new function that produces along with the development of nano material technology, has tangible small-size effect, skin effect, quantum size effect and macroscopical tunnel-effect.Show that after deliberation because the huge specific surface area of nano-MgO, a large amount of crystal defect and the positive charge effect of particle surface, nano-MgO is to bacterium, microorganisms such as gemma, virus show the very high activity of killing.With nano-TiO
2, other solid nano level bactericide such as Nano Silver, nanometer copper compare, nano-MgO low toxicity, cheap characteristic make it possibly become a kind of good drinking water disinfect.Yet, after nano-MgO places water, can form Mg (OH) with the water effect
2, a large amount of OH that it discharges
-System pH sharply is elevated to more than 10.0, and does not meet the requirement of drinking water quality.
The chitin-sodium alginate gel is a kind of slow-released system of comparative maturity, has been widely used in fields such as medicine, food, chemical fertilizer at present.Its raw material is easy to get, low price, and preparation condition is gentle, technology is simple and be easy to suitability for industrialized production.Owing to have CO in the air
2, nitrogen oxide etc. is prone to make the material of water acidification, therefore, only needs the accurately release rate of control nano-MgO, just might realize stablizing of system pH.
Based on this, the present invention realizes the accurately purpose of control nano material rate of release through the ratio of control nano-MgO and sustained-release gel, thereby reaches the requirement of stabilising system pH value and immobilization nano material.
Summary of the invention
The objective of the invention is to provides a kind of preparation method of nano-MgO slow-release disinfection particle to above-mentioned existing problems, solves the too high problem of bringing when nano-MgO is applied to water treatment of pH value.
Technical scheme of the present invention:
A kind of preparation method of nano-MgO slow-release disinfection particle, step is following:
1) fat-soluble shitosan is dissolved in the aqueous acetic acid under 100-120 ℃ of temperature, adds CaCl after being cooled to room temperature
22H
2O, the pH value is regulated to 5.0-5.5 with the NaOH aqueous solution in the dissolving back fully, makes chitosan solution;
2) preparation sodium alginate aqueous solution adds the nano-MgO powder and makes the turbid liquid of nano-MgO;
3) with the turbid liquid of nano-MgO with 2-3 drip/second speed splash in the chitosan solution, after dropwising above-mentioned reactant liquor is stirred half an hour under the 1000-1200rpm rotating speed, reject liquid obtains the milky microballoon;
4) with distilled water wash gained milky microballoon, up to the inorganic ion of removing microsphere surface fully;
5) above-mentioned microballoon was dried 2 hours down at 100-110 ℃ at least, can obtain yellow nano-MgO slow-release disinfection particle.
The concentration of volume percent of said aqueous acetic acid is 1-3%, and the amount ratio of shitosan and aqueous acetic acid is 4-8mg/ mL, CaCl
22H
2The amount ratio of O and aqueous acetic acid is 30-48mg/ mL.
The concentration of the said NaOH aqueous solution is 1mol/L.
Said nano-MgO powder average grain diameter is 10-80nm, and specific surface area is 30-50m
2/ g.
The concentration of said sodium alginate aqueous solution is 8-12mg/mL, and the amount ratio of nano-MgO powder and sodium alginate aqueous solution is 2-6mg/ mL.
The present invention utilizes the chitin-sodium alginate sustained-release gel to prepare the nano-MgO material.At first, in acetum, cooling back is to wherein adding calcium chloride, and regulation system pH is a faintly acid with the shitosan heating for dissolving; Secondly, the preparation sodium alginate aqueous solution, and to wherein adding the nano-MgO powder; Once more, draw the sodium alginate aqueous solution that is added with nano-MgO, slowly splash in the chitosan solution.After the last haptoreaction, take out gained Off-white solid microballoon, with distilled water wash back oven dry for several times.
Advantage of the present invention is:
Raw material such as shitosan that 1) the present invention selects for use, sodium alginate, wide material sources, cheap, and safety non-toxic are widely used in the processing and the environment remediation field of environmental pollution;
2) through the introducing of gel, can nano-MgO be fixed on the carrier, can not washed away by current;
3) through slow-released system, can system pH be stabilized in acceptable scope;
4) operation technology is simple, and condition is controlled easily, is easy to suitability for industrialized production.
Description of drawings
Fig. 1 is a nano-MgO slow-release disinfection particle made among the embodiment 1.
Fig. 2 is the milky microballoon that forms after the prepared nano-MgO slow-release disinfection particle entry swelling among the embodiment 1.
Fig. 3 is the situation of change of prepared nano-MgO slow-release disinfection particle pH in water among the embodiment 1.
Fig. 4 is the situation of change of total number of bacteria after the entry of prepared nano-MgO slow-release disinfection particle among the embodiment 2.
Embodiment
The present invention combines accompanying drawing to further specify through following examples, but the said technology contents of present embodiment only is illustrative, non-limiting, should not limit to protection scope of the present invention according to this.
Embodiment 1:
A kind of preparation method of nano-MgO slow-release disinfection particle, step is following:
1) the fat-soluble shitosan of 0.5 g being dissolved in concentration of volume percent under 100 ℃ of temperature is in 1% the 100mL aqueous acetic acid, adds 4.8 g CaCl after being cooled to room temperature
22H
2O, dissolving back is that the NaOH aqueous solution of 1mol/L is regulated the pH value to 5.0-5.5 with concentration fully, makes chitosan solution;
2) preparation concentration is the sodium alginate aqueous solution of 12mg/mL, adds 0.1 g nano-MgO powder, and nano-MgO powder average grain diameter is 10-80nm, and specific surface area is 30-50m
2/ g makes the turbid liquid of nano-MgO;
3) with the turbid liquid of nano-MgO with 2-3 drip/second speed splash in the chitosan solution, after dropwising above-mentioned reactant liquor is stirred half an hour under the 1000-1200rpm rotating speed, reject liquid obtains the milky microballoon;
4) with distilled water wash gained milky microballoon, up to the inorganic ion of removing microsphere surface fully;
5) above-mentioned microballoon was dried 2 hours down at 105 ℃, can obtain yellow nano-MgO slow-release disinfection particle.
Fig. 1 is the made nano-MgO slow-release disinfection particle of this embodiment; The milky microballoon of Fig. 2 for forming after this nano-MgO slow-release disinfection particle entry swelling.
Fig. 3 is the situation of change of the prepared nano-MgO slow-release disinfection of this embodiment particle pH in water.Show among the figure: with gained nano-MgO slow-release disinfection particle respectively with 10,20,50, the concentration of 80mg/L immerses in the water, each system pH all is stabilized between the 6.5-8.5 within the 120h.
Embodiment 2:
A kind of preparation method of nano-MgO slow-release disinfection particle, step is following:
1) the fat-soluble shitosan of 0.7g being dissolved in concentration of volume percent under 100 ℃ of temperature is in 2% the 100mL aqueous acetic acid, adds 3.6 g CaCl after being cooled to room temperature
22H
2O, dissolving back is that the NaOH aqueous solution of 1mol/L is regulated the pH value to 5.0-5.5 with concentration fully, makes chitosan solution;
2) preparation concentration is the sodium alginate aqueous solution of 12mg/mL, adds 0.3g nano-MgO powder, and nano-MgO powder average grain diameter is 10-80nm, and specific surface area is 30-50m
2/ g makes the turbid liquid of nano-MgO;
3) with the turbid liquid of nano-MgO with 2-3 drip/second speed splash in the chitosan solution, after dropwising above-mentioned reactant liquor is stirred half an hour under the 1000-1200rpm rotating speed, reject liquid obtains the milky microballoon;
4) with distilled water wash gained milky microballoon, up to the inorganic ion of removing microsphere surface fully;
5) above-mentioned microballoon was dried 2 hours down at 105 ℃, can obtain yellow nano-MgO slow-release disinfection particle.
Fig. 4 is the situation of change of total number of bacteria after the entry of the prepared nano-MgO slow-release disinfection of this embodiment particle.With gained nano-MgO slow-release disinfection particle respectively with 10,20,50, the concentration of 80mg/L immerses in the water; 5 days bacteriostatic test result shows: nano-MgO slow-release disinfection particle has obvious killing action to bacterium in the water in each system; And total number of bacteria can maintain below the 40CFU/mL in this reaction time, meets in the national water quality standard for drinking water requirement to total number of bacteria.
Claims (5)
1. the preparation method of a nano-MgO slow-release disinfection particle is characterized in that step is following:
1) fat-soluble shitosan is dissolved in the aqueous acetic acid under 100-120 ℃ of temperature, adds CaCl after being cooled to room temperature
22H
2O, the pH value is regulated to 5.0-5.5 with the NaOH aqueous solution in the dissolving back fully, makes chitosan solution;
2) preparation sodium alginate aqueous solution adds the nano-MgO powder and makes the turbid liquid of nano-MgO;
3) with the turbid liquid of nano-MgO with 2-3 drip/second speed splash in the chitosan solution, after dropwising above-mentioned reactant liquor is stirred half an hour under the 1000-1200rpm rotating speed, reject liquid obtains the milky microballoon;
4) with distilled water wash gained milky microballoon, up to the inorganic ion of removing microsphere surface fully;
5) above-mentioned microballoon was dried 2 hours down at 100-110 ℃ at least, can obtain yellow nano-MgO slow-release disinfection particle.
2. according to the preparation method of the said nano-MgO slow-release disinfection of claim 1 particle, it is characterized in that: the concentration of volume percent of said aqueous acetic acid is 1-3%, and the amount ratio of shitosan and aqueous acetic acid is 4-8mg/ mL, CaCl
22H
2The amount ratio of O and aqueous acetic acid is 30-48mg/ mL.
3. according to the preparation method of the said nano-MgO slow-release disinfection of claim 1 particle, it is characterized in that: the concentration of the said NaOH aqueous solution is 1mol/L.
4. according to the preparation method of the said nano-MgO slow-release disinfection of claim 1 particle, it is characterized in that: said nano-MgO powder average grain diameter is 10-80nm, and specific surface area is 30-50m
2/ g.
5. according to the preparation method of the said nano-MgO slow-release disinfection of claim 1 particle, it is characterized in that: the concentration of said sodium alginate aqueous solution is 8-12mg/mL, and the amount ratio of nano-MgO powder and sodium alginate aqueous solution is 2-6mg/ mL.
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| CN 201110360719 CN102428961B (en) | 2011-11-15 | 2011-11-15 | Method for preparing nano MgO sustained-release sterilizing granules |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106927718A (en) * | 2017-04-07 | 2017-07-07 | 佛山市蓝瑞欧特信息服务有限公司 | A kind of antimildew and antibacterial tile grout and preparation method thereof |
| CN112999334A (en) * | 2021-03-08 | 2021-06-22 | 中国药科大学 | Insulin heavy microsphere and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1373998A (en) * | 2002-03-28 | 2002-10-16 | 上海维安新材料研究中心有限公司 | Antiseptic glass pellet with slowly released component and its prepn |
| CN1440656A (en) * | 2003-03-20 | 2003-09-10 | 兴国纳米科技实业有限公司 | Nano composite antibacterial powder and its prepn process and application in promoting organism growth |
| CN1561744A (en) * | 2004-03-26 | 2005-01-12 | 北京化工大学 | Loaded nano magnesium oxide as bactericidal material |
| CN101690716A (en) * | 2009-10-13 | 2010-04-07 | 张亦军 | Calcium alginate-chitosan sustained-release microsphere carrying growth hormone and application thereof |
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2011
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1373998A (en) * | 2002-03-28 | 2002-10-16 | 上海维安新材料研究中心有限公司 | Antiseptic glass pellet with slowly released component and its prepn |
| CN1440656A (en) * | 2003-03-20 | 2003-09-10 | 兴国纳米科技实业有限公司 | Nano composite antibacterial powder and its prepn process and application in promoting organism growth |
| CN1561744A (en) * | 2004-03-26 | 2005-01-12 | 北京化工大学 | Loaded nano magnesium oxide as bactericidal material |
| CN101690716A (en) * | 2009-10-13 | 2010-04-07 | 张亦军 | Calcium alginate-chitosan sustained-release microsphere carrying growth hormone and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 方晶晶等: "纳米氧化镁灭菌效果与抑菌能力研究", 《海军医学杂志》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106927718A (en) * | 2017-04-07 | 2017-07-07 | 佛山市蓝瑞欧特信息服务有限公司 | A kind of antimildew and antibacterial tile grout and preparation method thereof |
| CN112999334A (en) * | 2021-03-08 | 2021-06-22 | 中国药科大学 | Insulin heavy microsphere and preparation method and application thereof |
| CN112999334B (en) * | 2021-03-08 | 2022-06-17 | 中国药科大学 | Insulin heavy microsphere and preparation method and application thereof |
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| CN102428961B (en) | 2013-07-17 |
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Granted publication date: 20130717 Termination date: 20131115 |