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CN108502916A - A kind of novel nano zinc oxide material prepares and application - Google Patents

A kind of novel nano zinc oxide material prepares and application Download PDF

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Publication number
CN108502916A
CN108502916A CN201810604369.1A CN201810604369A CN108502916A CN 108502916 A CN108502916 A CN 108502916A CN 201810604369 A CN201810604369 A CN 201810604369A CN 108502916 A CN108502916 A CN 108502916A
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CN
China
Prior art keywords
oxide material
zinc oxide
nano zinc
novel nano
prepares
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Pending
Application number
CN201810604369.1A
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Chinese (zh)
Inventor
徐进
徐勇
孙月华
王传荣
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XUANCHENG JINGRUI NEW MATERIAL CO Ltd
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XUANCHENG JINGRUI NEW MATERIAL CO Ltd
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Priority to CN201810604369.1A priority Critical patent/CN108502916A/en
Publication of CN108502916A publication Critical patent/CN108502916A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00Compounds of zinc
    • C01G9/02Oxides; Hydroxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

It prepares and applies the invention discloses a kind of novel nano zinc oxide material, belong to nano-powder preparing technical field, include the following steps:1. preparing zinc-containing solution;2. preparing aqueous slkali;3. mixing;4. precipitating;5. separation and drying;6. pre-treatment;7. impregnating;8. roasting.The novel nano zinc oxide material prepare and be used to prepare nanoscale Zinc material, the nano oxidized zinc product prepared by the more existing preparation method of the preparation method is not easy to reunite, and more easily and organic matter it is compatible, improve the product quality of nano zine oxide.

Description

A kind of novel nano zinc oxide material prepares and application
Technical field
The present invention relates to nano-powder preparing technical fields, prepare and answer in particular to a kind of novel nano zinc oxide material With.
Background technology
Nano zine oxide (ZnO) grain size is a kind of high-end high function fine inorganic product, table between 1-100 nm Reveal many special properties, such as non-migratory, fluorescence, piezoelectricity, absorption and scatters ultraviolet ability, using its The marvellous performance of light, electricity, magnetic, sensitivity etc., can manufacture gas sensor, fluorophor, rheostat, UV shielding material, Image recording material, piezoelectric material, varistor, effective catalyst, magnetic material and plastic film etc..Microcosmic variation is very More people can't see the excellent specific property of nano material, and by practice, present nano zine oxide is excellent with its in every field such as rubber Characteristic have been more and more widely used.
Nano zine oxide itself is since size is smaller, and grain size is thinner, and surface energy is also higher, leads to itself and organic matter group It point is difficult to compatible, it is easy to reunite together, it is necessary to which existing nano zine oxide preparation method is made improvements.
Invention content
In view of the above technical problems, a kind of novel nano zinc oxide material of the present invention is prepared and is used to prepare Nanoscale Zinc material, the nano oxidized zinc product prepared by the more existing preparation method of the preparation method are not easy to reunite, and It is more easily compatible with organic matter, improve the product quality of nano zine oxide.
To achieve the above object, prepared by a kind of novel nano zinc oxide material designed by the present invention, includes the following steps:
1. preparing zinc-containing solution:Two water zinc acetates are dissolved in dimethylformamide to form zinc-containing solution, and described molten containing zinc Capping agent is added in liquid;
2. preparing aqueous slkali:Potassium hydroxide is dissolved in propyl alcohol to form aqueous slkali;
3. mixing:The zinc-containing solution and the aqueous slkali are mixed, to react, form reaction solution;
4. precipitating:Precipitating reagent is added in the reaction solution to generate precipitation;
5. separation and drying:The precipitation is separated and is dried to get nano zinc oxide material;
6. pre-treatment:By the nano zinc oxide material using being stirred in citric acid solution, filter is then obtained by filtration Cake;
7. impregnating:The filter cake is impregnated into the cyclohexane solution of chloroform, maceration extract is obtained;
8. roasting:The maceration extract is evaporated, and is placed in Muffle furnace and roasts 1.5 ~ 3 hours with 400 ~ 550 DEG C to get novel Nano zinc oxide material.
As a preferred embodiment of the above technical solution, step 1. described in capping agent be octylame.
As a preferred embodiment of the above technical solution, the mole of the potassium hydroxide in the aqueous slkali relative to reaction needed for It is excessive for mole.
Reaction is as follows:
As a preferred embodiment of the above technical solution, step 4. described in precipitating reagent be acetone.
As a preferred embodiment of the above technical solution, step is 5. middle detaches precipitation using membrane filtration module.
As a preferred embodiment of the above technical solution, step is 5. middle is dried precipitation using vacuum drier.
As a preferred embodiment of the above technical solution, step 6. described in citric acid solution pH value be 3.8 ~ 4.2 between.
As a preferred embodiment of the above technical solution, 7. middle dip time is 30 ~ 120 minutes to step.
As a preferred embodiment of the above technical solution, step 8. in heating rate be 4.5 ~ 4.8 DEG C it is per minute.
The embodiment of the present invention compared with prior art, has the following advantages and advantageous effect:
Novel nano zinc oxide material described in the embodiment of the present invention prepares and is used to prepare nanoscale Zinc material, should Nano oxidized zinc product prepared by the more existing preparation method of preparation method is not easy to reunite, and be easier and organic matter it is compatible, Improve the product quality of nano zine oxide.
Specific implementation mode
With reference to specific embodiment, the present invention is described in further detail:
The embodiment of the present application is used to prepare nanoscale Zinc material, receiving prepared by the more existing preparation method of the preparation method Rice zinc oxide product be not easy to reunite, and be easier and organic matter it is compatible, improve the product quality of nano zine oxide.
Embodiment 1:A kind of novel nano zinc oxide material preparation, includes the following steps:
1. preparing zinc-containing solution:Two water zinc acetates are dissolved in dimethylformamide to form zinc-containing solution, and described molten containing zinc Octylame is added in liquid;
2. preparing aqueous slkali:Potassium hydroxide is dissolved in propyl alcohol to form aqueous slkali, the potassium hydroxide in the aqueous slkali rubs Excessive 10% for your the amount mole required relative to reaction;
3. mixing:The zinc-containing solution and the aqueous slkali are mixed, to react, form reaction solution;
4. precipitating:Acetone is added in the reaction solution to generate precipitation;
5. separation and drying:By the precipitation using membrane filtration module to detach and being dried using vacuum drier, Up to nano zinc oxide material;
6. pre-treatment:By the nano zinc oxide material use pH value for 4.0 citric acid solution in be stirred, then Filter cake is obtained by filtration;
7. impregnating:The filter cake is impregnated into the cyclohexane solution of chloroform, dip time is 90 minutes, obtains maceration extract;
8. roasting:The maceration extract is evaporated, and is placed in Muffle furnace and heats up, being 4.6 DEG C with rate per minute is warming up to 500 DEG C roasting 2 hours to get novel nano zinc oxide material.
Embodiment 2:A kind of novel nano zinc oxide material preparation, includes the following steps:
1. preparing zinc-containing solution:Two water zinc acetates are dissolved in dimethylformamide to form zinc-containing solution, and described molten containing zinc Octylame is added in liquid;
2. preparing aqueous slkali:Potassium hydroxide is dissolved in propyl alcohol to form aqueous slkali, the potassium hydroxide in the aqueous slkali rubs Excessive 10% for your the amount mole required relative to reaction;
3. mixing:The zinc-containing solution and the aqueous slkali are mixed, to react, form reaction solution;
4. precipitating:Acetone is added in the reaction solution to generate precipitation;
5. separation and drying:By the precipitation using membrane filtration module to detach and being dried using vacuum drier, Up to nano zinc oxide material;
6. pre-treatment:By the nano zinc oxide material use pH value for 4.0 citric acid solution in be stirred, then Filter cake is obtained by filtration;
7. impregnating:The filter cake is impregnated into the cyclohexane solution of chloroform, dip time is 60 minutes, obtains maceration extract;
8. roasting:The maceration extract is evaporated, and is placed in Muffle furnace and heats up, being 4.7 DEG C with rate per minute is warming up to 500 DEG C roasting 2 hours to get novel nano zinc oxide material.
Embodiment 3:A kind of novel nano zinc oxide material preparation, includes the following steps:
1. preparing zinc-containing solution:Two water zinc acetates are dissolved in dimethylformamide to form zinc-containing solution, and described molten containing zinc Octylame is added in liquid;
2. preparing aqueous slkali:Potassium hydroxide is dissolved in propyl alcohol to form aqueous slkali, the potassium hydroxide in the aqueous slkali rubs Excessive 20% for your the amount mole required relative to reaction;
3. mixing:The zinc-containing solution and the aqueous slkali are mixed, to react, form reaction solution;
4. precipitating:Acetone is added in the reaction solution to generate precipitation;
5. separation and drying:By the precipitation using membrane filtration module to detach and being dried using vacuum drier, Up to nano zinc oxide material;
6. pre-treatment:By the nano zinc oxide material use pH value for 4.2 citric acid solution in be stirred, then Filter cake is obtained by filtration;
7. impregnating:The filter cake is impregnated into the cyclohexane solution of chloroform, dip time is 30 minutes, obtains maceration extract;
8. roasting:The maceration extract is evaporated, and is placed in Muffle furnace and heats up, being 4.8 DEG C with rate per minute is warming up to 400 DEG C roasting 3 hours to get novel nano zinc oxide material.
Embodiment 4:A kind of novel nano zinc oxide material preparation, includes the following steps:
1. preparing zinc-containing solution:Two water zinc acetates are dissolved in dimethylformamide to form zinc-containing solution, and described molten containing zinc Octylame is added in liquid;
2. preparing aqueous slkali:Potassium hydroxide is dissolved in propyl alcohol to form aqueous slkali, the potassium hydroxide in the aqueous slkali rubs Excessive 5% for your the amount mole required relative to reaction;
3. mixing:The zinc-containing solution and the aqueous slkali are mixed, to react, form reaction solution;
4. precipitating:Acetone is added in the reaction solution to generate precipitation;
5. separation and drying:By the precipitation using membrane filtration module to detach and being dried using vacuum drier, Up to nano zinc oxide material;
6. pre-treatment:By the nano zinc oxide material use pH value for 3.8 citric acid solution in be stirred, then Filter cake is obtained by filtration;
7. impregnating:The filter cake is impregnated into the cyclohexane solution of chloroform, dip time is 120 minutes, obtains maceration extract;
8. roasting:The maceration extract is evaporated, and is placed in Muffle furnace and heats up, being 4.5 DEG C with rate per minute is warming up to 550 DEG C roasting 1.5 hours to get novel nano zinc oxide material.

Claims (9)

1. prepared by a kind of novel nano zinc oxide material, which is characterized in that include the following steps:
1. preparing zinc-containing solution:Two water zinc acetates are dissolved in dimethylformamide to form zinc-containing solution, and described molten containing zinc Capping agent is added in liquid;
2. preparing aqueous slkali:Potassium hydroxide is dissolved in propyl alcohol to form aqueous slkali;
3. mixing:The zinc-containing solution and the aqueous slkali are mixed, to react, form reaction solution;
4. precipitating:Precipitating reagent is added in the reaction solution to generate precipitation;
5. separation and drying:The precipitation is separated and is dried to get nano zinc oxide material;
6. pre-treatment:By the nano zinc oxide material using being stirred in citric acid solution, filter is then obtained by filtration Cake;
7. impregnating:The filter cake is impregnated into the cyclohexane solution of chloroform, maceration extract is obtained;
8. roasting:The maceration extract is evaporated, and is placed in Muffle furnace and roasts 1.5 ~ 3 hours with 400 ~ 550 DEG C to get novel Nano zinc oxide material.
2. a kind of novel nano zinc oxide material according to claim 1 prepares and application, it is characterised in that:Step 1. in The capping agent is octylame.
3. a kind of novel nano zinc oxide material according to claim 1 prepares and application, it is characterised in that:The alkali soluble The mole of potassium hydroxide in liquid is excessive for the mole needed for reaction.
4. a kind of novel nano zinc oxide material according to claim 1 prepares and application, it is characterised in that:Step 4. in The precipitating reagent is acetone.
5. a kind of novel nano zinc oxide material according to claim 1 prepares and application, it is characterised in that:Step 5. in Precipitation is detached using membrane filtration module.
6. a kind of novel nano zinc oxide material according to claim 1 prepares and application, it is characterised in that:Step 5. in Precipitation is dried using vacuum drier.
7. a kind of novel nano zinc oxide material according to claim 1 prepares and application, it is characterised in that:Step 6. in Between the pH value of the citric acid solution is 3.8 ~ 4.2.
8. a kind of novel nano zinc oxide material according to claim 1 prepares and application, it is characterised in that:Step 7. in Dip time is 30 ~ 120 minutes.
9. a kind of novel nano zinc oxide material according to claim 1 prepares and application, it is characterised in that:Step 8. in Heating rate be 4.5 ~ 4.8 DEG C it is per minute.
CN201810604369.1A 2018-06-13 2018-06-13 A kind of novel nano zinc oxide material prepares and application Pending CN108502916A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111573712A (en) * 2020-05-26 2020-08-25 安徽锦华氧化锌有限公司 Preparation method for improving antibacterial property of nano zinc oxide

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101965315A (en) * 2008-03-10 2011-02-02 塔塔化学有限公司 Process for the preparation of nano zinc oxide particles
CN105000589A (en) * 2015-07-20 2015-10-28 苏州宇希新材料科技有限公司 Citric acid-modified nanometer zinc oxide
CN105036177A (en) * 2015-07-20 2015-11-11 苏州宇希新材料科技有限公司 Preparation method of nano-zinc oxide

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101965315A (en) * 2008-03-10 2011-02-02 塔塔化学有限公司 Process for the preparation of nano zinc oxide particles
CN105000589A (en) * 2015-07-20 2015-10-28 苏州宇希新材料科技有限公司 Citric acid-modified nanometer zinc oxide
CN105036177A (en) * 2015-07-20 2015-11-11 苏州宇希新材料科技有限公司 Preparation method of nano-zinc oxide

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111573712A (en) * 2020-05-26 2020-08-25 安徽锦华氧化锌有限公司 Preparation method for improving antibacterial property of nano zinc oxide

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Application publication date: 20180907

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