CN108975384A - A kind of nano zine oxide and its low temperature preparation method - Google Patents
A kind of nano zine oxide and its low temperature preparation method Download PDFInfo
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- CN108975384A CN108975384A CN201811105378.2A CN201811105378A CN108975384A CN 108975384 A CN108975384 A CN 108975384A CN 201811105378 A CN201811105378 A CN 201811105378A CN 108975384 A CN108975384 A CN 108975384A
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a kind of nano zine oxide and its low temperature preparing methods to realize watery fusion for 2-3 parts of 4-6 parts of sylvite, 3-4 parts of lithium salts and sodium salt mixed meltings at a temperature of 200~500 DEG C；It adds 1-7 parts of zinc salts and stirs several hours at a temperature of 200~500 DEG C, obtain the nano zine oxide of small size after drying then is cleaned multiple times in gained solid-state fused salt.Since sylvite, lithium salts and sodium salt all have preferable solubility, advantage soluble easily in water and low-melting, so that liquid fused salt obtained is easily uniformly mixed.Liquid fused salt can intensified response object mobility, the solid-state fused salt of generation can also be separated well, to avoid reuniting.Preparation method provided by the invention can carry out under cryogenic, so that zinc salt nucleated directly in low-temperature molten salt is grown to nano zine oxide, without carrying out high-temperature calcination, so that simple process, easy to operate.The nano zine oxide of preparation of the embodiment of the present invention has the characteristics of crystallinity is high, size uniformity, large specific surface area.
Description
Technical field
The present invention relates to inorganic functional material technical field more particularly to a kind of nano zine oxide and its low temperature preparation sides
Method.
Background technique
Nano zine oxide is a kind of new inorganic material of multifunctionality, and granular size is about at 1~100 nanometer, simultaneously
Double grading with nano material and conventional oxidation zinc.Nano zine oxide is compared with conventional oxidation zinc product, specific surface area
Greatly, chemical activity is high, and product fineness, chemical purity and shape of particle, which can according to need, to be adjusted, and has photochemistry
Effect and preferably cover it is imparted can, UV shielding rate is up to 98%；Meanwhile it also has antibacterial bacteriostatic, taste of dispelling
A series of special performances such as anti-enzyme show the performances such as unique electricity, magnetic, sound, light, heat.Therefore, nano zine oxide is as important
Novel inorganic functional material be widely used in the fields such as rubber industry, ink fuel, fine ceramics industry.
Currently, the conventional means for preparing nano zine oxide is sluggish precipitation, specific embodiment will be matched centainly
Zinc nitrate and urea are dissolved in distilled water respectively, mix the two after being completely dissolved, and quantitative surfactant is added, stirring
After be heated to assigned temperature, stop after being reacted to the time required, obtain presoma basic zinc carbonate.It is used after natural cooling
Distilled water and dehydrated alcohol washing are finally separated (precipitating) again, dry and roasting process obtains nano zine oxide fission.
Although sluggish precipitation has low in cost, simple operation and other advantages, however in the precipitating for preparing nano zine oxide
In the process, it often will form the lump of reunion, which needs the sintering processes of higher temperature that can just eliminate.But due to aggregate
Biggish stomata can be generated during the sintering process, so that the process of elimination is very difficult, lead to the quality of nano zine oxide obtained
It is bad.
Summary of the invention
The present invention provides a kind of nano zine oxide and its low temperature preparing methods, to solve to use existing preparation method system
The bad problem of the quality of the nano zine oxide obtained.
In a first aspect, the present invention provides a kind of nano zine oxide, the nano zine oxide by following portions by weight original
Material is made: 4-6 parts of sylvite；3-4 parts of lithium salts；2-3 parts of sodium salt；1-7 parts of zinc salt.
Optionally, the sylvite uses potassium chloride, potassium nitrate, potassium sulfate, potassium carbonate, potassium iodide, one of potassium bromide
Or it is several.
Optionally, the lithium salts uses lithium chloride, lithium nitrate, lithium sulfate, one or more of lithium carbonate.
Optionally, the sodium salt uses sodium chloride, sodium nitrate, sodium sulphate, sodium carbonate, sodium bicarbonate, sodium sulfite, phosphoric acid
Sodium, sodium dihydrogen phosphate, sodium iodide, one or more of sodium bromide.
Optionally, the zinc salt uses zinc chloride, zinc sulfate, zinc nitrate, zinc carbonate, basic zinc carbonate, zinc dihydrogen phosphate
One or more of.
Second aspect, the present invention also provides a kind of low temperature preparing methods of nano zine oxide, and the method includes following
Step:
4-6 parts of raw material sylvite, 3-4 parts of lithium salts and 2-3 parts of sodium salt are mixed in proportion, at a temperature of 200 DEG C~500 DEG C,
Liquid fused salt is obtained after magnetic agitation is handled；
1-7 parts of zinc salts are added in the liquid fused salt, at a temperature of 200 DEG C~500 DEG C, is mixed and is cooled down
After processing, solid-state fused salt is obtained；
Using deionized water, the cleaning more than or equal to 5 times is carried out to the solid-state fused salt；Using drying box to cleaning after
Solid-state fused salt be dried, cooled to room temperature obtains nano zine oxide.
Optionally, the magnetic agitation time uses 30 minutes~60 minutes.
Optionally, the time of the mixing uses 12 hours~48 hours.
Optionally, the drying temperature of the drying box uses 80 DEG C~120 DEG C, and drying time is small using 12 hours~36
When.
From the above technical scheme, nano zine oxide and its low temperature preparation method provided in an embodiment of the present invention, by potassium
2-3 parts of 4-6 parts of salt, 3-4 parts of lithium salts and sodium salt mixed meltings at a temperature of 200~500 DEG C realize watery fusion；Add 1-7
Part zinc salt stirs several hours at a temperature of 200 DEG C~500 DEG C, then by gained solid-state fused salt be cleaned multiple times it is dry after obtain it is small
The nano zine oxide of size.Since sylvite, lithium salts and sodium salt all have preferable solubility, soluble easily in water and low-melting excellent
Point, so that liquid fused salt obtained is easily uniformly mixed.Liquid fused salt can intensified response object mobility, also can consolidating generation
State fused salt separates well, to avoid reuniting.Preparation method provided by the invention can carry out under cryogenic, so that zinc
Salt nucleated directly in low-temperature molten salt is grown to nano zine oxide, without carrying out high-temperature calcination, so that simple process, operation side
Just, and raw material is easy to get, is low in cost, is environmental-friendly, and entire reaction process does not need special installation, is conducive to industrialized production.
The nano zine oxide of preparation of the embodiment of the present invention has the characteristics of crystallinity is high, size uniformity, large specific surface area.
Detailed description of the invention
In order to illustrate more clearly of technical solution of the present invention, letter will be made to attached drawing needed in the embodiment below
Singly introduce, it should be apparent that, for those of ordinary skills, without any creative labor,
It is also possible to obtain other drawings based on these drawings.
Fig. 1 is the flow chart of the low temperature preparation method of nano zine oxide provided in an embodiment of the present invention；
Fig. 2 is the X-ray diffracting spectrum of nano zine oxide prepared by the embodiment of the present invention 1；
Fig. 3 is the transmission electron microscope figure of nano zine oxide prepared by the embodiment of the present invention 2；
Fig. 4 is nitrogen adsorption-desorption curve figure of nano zine oxide prepared by the embodiment of the present invention 3.
Specific embodiment
Nano zine oxide provided in an embodiment of the present invention, using molten salt preparation method, by the way that zinc salt is introduced liquid fused salt
In, make to react mobility enhancing in the liquid phase, diffusion rate significantly improves.Simultaneously because fused salt is applied in the powder of generation
Between grain, the interconnection of particle, therefore powder soilless sticking made from molten-salt growth method is prevented, or only weakly agglomerated, obtain high quality
Nano zine oxide.
In the present embodiment, liquid fused salt is made of the raw material of following portions by weight: 4-6 parts of sylvite, 3-4 parts of lithium salts and sodium salt
2-3 parts.
By taking the gross mass of sylvite, lithium salts and sodium salt is 10g-11g as an example, according to aforementioned proportion by the gross mass of three raw materials
Control is 10g-11g, it would be possible that existing several proportions are including but not limited to such as under type: (1) 5g sylvite, 3g lithium salts,
2g sodium salt；(2) 6g sylvite, 3g lithium salts, 2g sodium salt；(3) 4g sylvite, 4g lithium salts, 2g sodium salt；(4) 5g sylvite, 3g lithium salts, 3g sodium
Salt；(5) 2g+3g sylvite, 2g+1g lithium salts, 2g sodium salt；(6) 3g+3g sylvite, 2g+1g lithium salts, 2g sodium salt.
Has the characteristics that solubility using sylvite, i.e., since sylvite is most of soluble easily in water, and than other salt mines
The solubility of object also wants larger, therefore is one of the raw material for preparing liquid fused salt with sylvite, and rate of dissolution can be improved.This implementation
In example, sylvite uses potassium chloride, potassium nitrate, potassium sulfate, potassium carbonate, potassium iodide, one or more of potassium bromide.
Lithium salts is also soluble easily in water, and fusing point is low, and using lithium salts as one of the raw material of preparation liquid fused salt, dissolution speed can be improved
Rate is easier to melt.In the present embodiment, lithium salts uses lithium chloride, lithium nitrate, lithium sulfate, one or more of lithium carbonate.
Sodium salt has the characteristics that soluble easily in water, and solubility is big, can using sodium salt as one of the raw material of preparation liquid fused salt
Rate of dissolution is improved, is easier to melt.In the present embodiment, sodium salt uses sodium chloride, sodium nitrate, sodium sulphate, sodium carbonate, bicarbonate
Sodium, sodium sulfite, sodium phosphate, sodium dihydrogen phosphate, sodium iodide, one or more of sodium bromide.
After preparing liquid fused salt using sylvite, lithium salts and sodium salt, to obtain the smaller and uniform nano zine oxide of size,
1-7 parts of zinc salt need to be added in liquid fused salt.
Zinc salt have it is soluble easily in water, be dissolved in the feature of methanol, ethyl alcohol, glycerol, acetone, ether etc., solubility is larger, fusing point
It is low, using zinc salt as the raw material for preparing nano zine oxide, rate of dissolution can be improved, be easier to melt, be uniformly mixed.The present embodiment
In, zinc salt uses zinc chloride, zinc sulfate, zinc nitrate, zinc carbonate, basic zinc carbonate, one or more of zinc dihydrogen phosphate.
The embodiment of the present invention has size smaller, uniform, matter according to above-mentioned raw materials and its nano zine oxide of proportion preparation
Measure good, low in cost advantage.
The embodiment of the present invention prepares nano zine oxide according to following processing steps, due to the fusing point of sylvite, lithium salts and sodium salt
It is lower, it is ensured that nano zine oxide to can be obtained under cryogenic, without carrying out high-temperature calcination.As it can be seen that the present embodiment mentions
The method and process of confession is simple, easy to operate, is conducive to industrialized production, and the nano zine oxide prepared has crystallinity height, ruler
It is very little uniform, the characteristics of large specific surface area.
Specifically, as shown in Figure 1, a kind of low temperature preparation method of nano zine oxide provided in this embodiment, including it is following
Step:
S1,4-6 parts of raw material sylvite, 3-4 parts of lithium salts and 2-3 parts of sodium salt are mixed in proportion, in 200 DEG C~500 DEG C temperature
Under, liquid fused salt is obtained after magnetic agitation is handled；
Wherein, the whipping temp of magnetic agitation use 200 DEG C~500 DEG C temperature, the magnetic agitation time using 30 minutes~
60 minutes.
According to aforementioned proportion, raw material sylvite, lithium salts and sodium salt are uniformly mixed, the magnetic agitation 30 at 200 DEG C~500 DEG C
It is melted to complete within~60 minutes.Since sylvite, lithium salts and sodium salt all have, soluble easily in water, solubility is big, low-melting advantage, because
This, can satisfy in cryogenic conditions, and three is melted and is uniformly mixed.
The liquid fused salt obtained after melting, both the mobility of intensified response object (sylvite, lithium salts and sodium salt), was also convenient for subsequent
The solid-state fused salt of generation is separated well in step, to avoid reuniting.
S2,1-7 parts of zinc salts are added in the liquid fused salt, at a temperature of 200 DEG C~500 DEG C, through be mixed and
After cooling treatment, solid-state fused salt is obtained；
Wherein, the time of mixing uses 12 hours~48 hours.
The zinc salt of certain mass is added in the liquid fused salt that step S1 is obtained, stirs 12 at a temperature of 200 DEG C~500 DEG C
~48 hours, solid-state fused salt can be obtained to after reaction, carry out cooling treatment.
The additional amount of zinc salt is 1-7 parts, and optimal addn is 3 parts.
S3, using deionized water, the cleaning more than or equal to 5 times is carried out to the solid-state fused salt；Using drying box to clear
Solid-state fused salt after washing is dried, and cooled to room temperature obtains nano zine oxide.
Wherein, the drying temperature of drying box uses 80 DEG C~120 DEG C, and drying time uses 12 hours~36 hours.
Cooling obtained solid is cleaned multiple times with deionized water, 12~36 hours dry at 80~120 DEG C, natural cooling
The nano zine oxide of small size is just obtained to room temperature.
Solid-state fused salt after cooling is started the cleaning processing, that is, washes off extra sylvite, lithium salts and sodium salt, usual situation
Under, it needs to clean 5 times or more, can just regard as cleaning up.
It after cleaning, is dried, cooled to room temperature, can be obtained that cleanliness is good, and size is smaller and equal
One nano zine oxide.
From the above technical scheme, the low temperature preparation method of nano zine oxide provided in an embodiment of the present invention, will be certain
Sylvite, lithium salts and the sodium salt of ratio mixed melting at a temperature of 200~500 DEG C realize watery fusion；Add a certain amount of zinc
Salt stirs several hours at a temperature of 200 DEG C~500 DEG C, obtains small size after drying then is cleaned multiple times in gained solid-state fused salt
Nano zine oxide.Since sylvite, lithium salts and sodium salt all have preferable solubility, advantage soluble easily in water and low-melting,
So that liquid fused salt obtained is easily uniformly mixed.Liquid fused salt can intensified response object mobility, also can be by the solid-state of generation
Fused salt separates well, to avoid reuniting.Preparation method provided by the invention can carry out under cryogenic, so that zinc salt
Nucleated directly is grown to nano zine oxide in low-temperature molten salt, without carrying out high-temperature calcination, so that it is simple process, easy to operate,
And raw material is easy to get, is low in cost, is environmental-friendly, and entire reaction process does not need special installation, is conducive to industrialized production.This hair
The nano zine oxide of bright embodiment preparation has the characteristics of crystallinity is high, size uniformity, large specific surface area, can be widely applied to
Rubber industry, cosmetic industry, chemical fibre industry, the fields such as electronics industry.
Nano zine oxide provided in an embodiment of the present invention and its low temperature preparation are illustrated With reference to embodiment
Beneficial effect caused by method.
Embodiment 1
S1,5g potassium chloride, 3g lithium nitrate are uniformly mixed with 2g sodium chloride, magnetic agitation 60 minutes is to complete at 200 DEG C
Full-fusing obtains liquid fused salt；
S2,1g zinc chloride is added in the resulting liquid fused salt of step S1, is stirred 36 hours at a temperature of 200 DEG C, to anti-
Cooling treatment is carried out after answering, and obtains solid-state fused salt；
S3, cooling gained solid-state fused salt is cleaned for 5 times using deionized water progress, it is 12 hours dry at 120 DEG C, it is natural
It is cooled to room temperature the nano zine oxide for just obtaining small size.
Fig. 2 is the X ray diffracting spectrum of small size nano zine oxide obtained by the present embodiment, as can be seen from the figure institute
The material of acquisition is pure phase, is occurred without other phases and other impurity, and the well-crystallized of nano zine oxide.
Embodiment 2
S1,6g potassium nitrate, 3g lithium chloride are uniformly mixed with 2g sodium phosphate, magnetic agitation 50 minutes is to complete at 300 DEG C
Full-fusing obtains liquid fused salt；
S2,2g zinc carbonate is added in the resulting liquid fused salt of step S1, is stirred 24 hours at a temperature of 300 DEG C, to anti-
Cooling treatment is carried out after answering, and obtains solid-state fused salt；
S3, cooling gained solid-state fused salt is cleaned for 6 times using deionized water progress, it is 36 hours dry at 80 DEG C, it is natural
It is cooled to room temperature the nano zine oxide for just obtaining small size.
Fig. 3 is the transmission electron microscope picture of small size nano zine oxide obtained by the present embodiment, it can be seen that
Gained nano zine oxide size uniformity, partial size is in 40nm or so.
Embodiment 3
S1,4g potassium bromide, 4g lithium chloride are uniformly mixed with 2g sodium sulphate, magnetic agitation 40 minutes is to complete at 400 DEG C
Full-fusing obtains liquid fused salt；
S2,3g zinc dihydrogen phosphate is added in the resulting liquid fused salt of step S1, is stirred 20 hours at a temperature of 400 DEG C,
To carry out cooling treatment after reaction, solid-state fused salt is obtained；
S3, cooling gained solid-state fused salt is cleaned for 6 times using deionized water progress, it is 24 hours dry at 100 DEG C, it is natural
It is cooled to room temperature the nano zine oxide for just obtaining small size.
Fig. 4 is nitrogen adsorption-desorption curve figure of small size nano zine oxide obtained by the present embodiment, can from figure
Out, the specific surface area of nano zine oxide is up to 59.75m2g-1。
Embodiment 4
S1,4g potassium iodide, 3g lithium sulfate are uniformly mixed with 3g sodium carbonate, magnetic agitation 30 minutes is to complete at 500 DEG C
Full-fusing obtains liquid fused salt；
S2,7g basic zinc carbonate is added in the resulting liquid fused salt of step S1, is stirred 12 hours at a temperature of 500 DEG C,
To carry out cooling treatment after reaction, solid-state fused salt is obtained；
S3, cooling gained solid-state fused salt is cleaned for 7 times using deionized water progress, it is 30 hours dry at 90 DEG C, it is natural
It is cooled to room temperature the nano zine oxide for just obtaining small size.
Embodiment 5
S1,2g potassium nitrate, 3g potassium carbonate, 2g lithium nitrate, 1g lithium chloride are uniformly mixed with 2g sodium bicarbonate, at 250 DEG C
Liquid fused salt is obtained to complete melting within lower magnetic agitation 55 minutes；
S2,6g zinc nitrate is added in the resulting liquid fused salt of step S1, is stirred 24 hours at a temperature of 300 DEG C, to anti-
Cooling treatment is carried out after answering, and obtains solid-state fused salt；
S3, cooling gained solid-state fused salt is cleaned for 5 times using deionized water progress, it is 20 hours dry at 110 DEG C, it is natural
It is cooled to room temperature the nano zine oxide for just obtaining small size.
Embodiment 6
S1,3g potassium sulfate, 3g potassium chloride, 2g lithium carbonate, 1g lithium nitrate are uniformly mixed with 2g sodium nitrate, at 400 DEG C
Liquid fused salt is obtained to complete melting within magnetic agitation 35 minutes；
S2,4g zinc sulfate is added in the resulting liquid fused salt of step S1, is stirred 36 hours at a temperature of 400 DEG C, to anti-
Cooling treatment is carried out after answering, and obtains solid-state fused salt；
S3, cooling gained solid-state fused salt is cleaned for 5 times using deionized water progress, it is 24 hours dry at 120 DEG C, it is natural
It is cooled to room temperature the nano zine oxide for just obtaining small size.
In conclusion the low temperature preparation method of the nano zine oxide provided according to embodiments of the present invention, this method pass through by
Zinc salt, which is put into liquid fused salt, to be grown, and the small and uniform nano zine oxide of available size, which can be further
Applied to semiconductor and related industrial fields.
Those skilled in the art after considering the specification and implementing the invention disclosed here, will readily occur to of the invention its
Its embodiment.This application is intended to cover any variations, uses, or adaptations of the invention, these modifications, purposes or
Person's adaptive change follows general principle of the invention and including the undocumented common knowledge in the art of the present invention
Or conventional techniques.The description and examples are only to be considered as illustrative, and true scope and spirit of the invention are by appended
Claim is pointed out.
It should be understood that the present invention is not limited to the precise structure already described above and shown in the accompanying drawings, and
And various modifications and changes may be made without departing from the scope thereof.The scope of the present invention is limited only by the attached claims.
Claims (9)
1. a kind of nano zine oxide, which is characterized in that the nano zine oxide is made of the raw material of following portions by weight:
4-6 parts of sylvite；
3-4 parts of lithium salts；
2-3 parts of sodium salt；
1-7 parts of zinc salt.
2. nano zine oxide according to claim 1, which is characterized in that the sylvite uses potassium chloride, potassium nitrate, sulfuric acid
Potassium, potassium carbonate, potassium iodide, one or more of potassium bromide.
3. nano zine oxide according to claim 1, which is characterized in that the lithium salts uses lithium chloride, lithium nitrate, sulfuric acid
Lithium, one or more of lithium carbonate.
4. nano zine oxide according to claim 1, which is characterized in that the sodium salt uses sodium chloride, sodium nitrate, sulfuric acid
Sodium, sodium carbonate, sodium bicarbonate, sodium sulfite, sodium phosphate, sodium dihydrogen phosphate, sodium iodide, one or more of sodium bromide.
5. nano zine oxide according to claim 1, which is characterized in that the zinc salt uses zinc chloride, zinc sulfate, nitric acid
Zinc, zinc carbonate, basic zinc carbonate, one or more of zinc dihydrogen phosphate.
6. a kind of low temperature preparation method of nano zine oxide, which is characterized in that the described method comprises the following steps:
4-6 parts of raw material sylvite, 3-4 parts of lithium salts and 2-3 parts of sodium salt are mixed in proportion, at a temperature of 200~500 DEG C, through magnetic force
Liquid fused salt is obtained after stir process；
1-7 parts of zinc salts are added in the liquid fused salt, at a temperature of 200 DEG C~500 DEG C, through mixing and cooling treatment
Afterwards, solid-state fused salt is obtained；
Using deionized water, the cleaning more than or equal to 5 times is carried out to the solid-state fused salt；Using drying box to consolidating after cleaning
State fused salt is dried, and cooled to room temperature obtains nano zine oxide.
7. according to the method described in claim 6, it is characterized in that, the magnetic agitation time use 30 minutes~60 minutes.
8. according to the method described in claim 6, it is characterized in that, the time of the mixing using 12 hours~48 small
When.
9. according to the method described in claim 6, it is characterized in that, the drying temperature of the drying box use 80 DEG C~120 DEG C,
Drying time uses 12 hours~36 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112939059A (en) * | 2021-03-23 | 2021-06-11 | 宁夏京成天宝饲料添加剂有限公司 | Preparation method of porous zinc oxide |
| WO2024063664A1 (en) | 2022-09-23 | 2024-03-28 | Beointech D.O.O. Beograd | Ultrasonic low temperature synthesis of an advanced multifunctional additive for application in animal feed production |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112939059A (en) * | 2021-03-23 | 2021-06-11 | 宁夏京成天宝饲料添加剂有限公司 | Preparation method of porous zinc oxide |
| WO2024063664A1 (en) | 2022-09-23 | 2024-03-28 | Beointech D.O.O. Beograd | Ultrasonic low temperature synthesis of an advanced multifunctional additive for application in animal feed production |
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