CN105347386A - Preparation method of nano-zinc oxide - Google Patents
Preparation method of nano-zinc oxide Download PDFInfo
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- CN105347386A CN105347386A CN201510807727.5A CN201510807727A CN105347386A CN 105347386 A CN105347386 A CN 105347386A CN 201510807727 A CN201510807727 A CN 201510807727A CN 105347386 A CN105347386 A CN 105347386A
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Abstract
The invention discloses a preparation method of nano-zinc oxide and belongs to the technical field of preparation of an ultrafine inorganic material. The preparation method comprises the following steps: adding basic zinc carbonate into an ammonia solution to prepare a zinc-ammonia solution, drying the zinc-ammonia solution, crystallizing and roasting to obtain nano-zinc oxide, wherein the ammonia solution is 20-30 wt% of an ammonia-water solution, 5-15 wt% of an ammonium bicarbonate aqueous solution or a mixed solution of the ammonia-water solution and the ammonium bicarbonate aqueous solution. According to the above method, basic zinc carbonate which is used as a starting material is added into a specific solution, and then crystallization and roasting are successively carried out to obtain nano-zinc oxide; and there is no need to accurately limit raw material reaction conditions to prepare the basic zinc carbonate precursor under specific conditions, and preparation process and operating process are simplified. By roasting the basic zinc carbonate which has undergone the above treatment, the nano-zinc oxide can be obtained. Thus, efficiency is raised, and cost is reduced. The preparation method is suitable for large-scale production.
Description
Technical field
The present invention relates to inorganic materials preparing technical field, be specifically related to a kind of preparation method of nano zine oxide.
Background technology
Nano-class zinc oxide particle diameter is between 1-100nm, it is a kind of novel high function fine inorganic product, it shows much special character, as non-migratory, fluorescence, piezoelectricity, absorption and scatters ultraviolet ability etc., there is the performance of the aspects such as optical, electrical, magnetic, sensitivity, can be applicable to manufacture the various fields such as gas sensor, fluor, varistor, UV-preventing material, image recording material, piezoelectric, voltage dependent resistor, effective catalyst, magneticsubstance and plastics film.
Traditional zinc oxide is produced and is adopted calcined by rotary kiln basic carbonate zinc technology.This production method production time is long, cost is high, energy consumption is large, quality percentage is low, shopwork environment is poor, especially product granularity is thicker, activity is not high, so existing zinc subcarbonate can not be adopted directly to carry out calcining, preparation is thinner, nano level zinc subcarbonate.
Prepare the method for nano zine oxide at present, with regard to preparation process, have single stage method and two step method.Single stage method is by the direct synthesis of nano-zinc oxide of certain reaction means, as hydrothermal method and LASER HEATING method etc.; Two step method first prepares a kind of precursor, then obtains nano zine oxide by the method for thermolysis precursor, as precipitation-thermal decomposition method, sol-gel method, emulsion method etc.Zinc subcarbonate is the precursor of normal preparation.
Chinese patent literature (CN1533985A) discloses a kind of preparation method of nano-scale oxidized zinc powder, the method is for raw material with zinc solution and carbonate solution, first dispersion agent is added in zinc solution, then drip carbonate solution under high velocity agitation and carry out presoma hydrothermal synthesis reaction, obtain the suspension containing zinc carbonate, again by the suspension filtered containing zinc carbonate, calcine after filter cake washing, drying, then pulverizing obtains nanometer Zinc oxide powder.
In the above-mentioned methods, need first prepare zinc carbonate precursor, then carry out drying and calcining.The thermolysis condition of precursor and dispersiveness affect the performance of product and the investment of whole technological process and product cost.The different precursors that can obtain different sorts and character of raw material and reaction conditions, the factor such as kind, character, thermolysis environment and condition of precursor all can have a huge impact the character of final product nano zine oxide.Therefore, precursor be prepared in two step method the effect having and concern and prepare nano zine oxide success or failure, but the preparation of precursor needs accurately to control many factors, as raw material, concentration, reaction conditions etc., result in the complexity of the step of preparation technology and the loaded down with trivial details of control, improve cost, and can not produce on a large scale.
Summary of the invention
Therefore, the technical problem to be solved in the present invention to be to overcome in prior art nano zine oxide two step method step of preparation process complicated, control loaded down with trivial details, thus cause cost high, can not the defect of scale operation, and large-scale production defect can not be carried out, thus provide that a kind of technical process is simple, easy to operate, low cost, the preparation method of a kind of nano zine oxide of scale operation of can carrying out.
For this reason, technical scheme of the present invention is:
A preparation method for nano zine oxide, comprises step as follows: added by zinc subcarbonate in ammonia solution and prepare zinc ammonia solution, by zinc ammonia solution drying crystalline, roasting, obtains nano zine oxide; Described ammonia solution is the ammonia soln of 20 ~ 30wt%, the ammonium bicarbonate aqueous solution of 5 ~ 15wt% or the two mixed solution.
In the preparation method of above-mentioned nano zine oxide, in described mixed solution, the mass ratio of the ammonium bicarbonate aqueous solution of 20 ~ 30wt% ammonia soln and 5 ~ 15wt% is 1-99:99-1.
In the preparation method of above-mentioned nano zine oxide, preferably, described ammonia solution is the ammonia soln of 25wt%, the ammonium bicarbonate aqueous solution of 10wt% or the two mixed solution.
In the preparation method of above-mentioned nano zine oxide, in described zinc ammonia solution, zinc concentration is 0.5 ~ 4mol/L.
In the preparation method of above-mentioned nano zine oxide, preferably, in described zinc ammonia solution, zinc concentration is 2 ~ 3.5mol/L.
In the preparation method of above-mentioned nano zine oxide, the mass volume ratio of zinc subcarbonate and ammonia solution is 10-30g/100mL.
In the preparation method of above-mentioned nano zine oxide, the temperature of described drying is 25 ~ 140 DEG C.
In the preparation method of above-mentioned nano zine oxide, preferably, the temperature of described drying is 40 ~ 80 DEG C.
In the preparation method of above-mentioned nano zine oxide, the temperature of described roasting is 200 ~ 400 DEG C.
In the preparation method of above-mentioned nano zine oxide, preferably, the temperature of described roasting is 220 ~ 240 DEG C.Technical solution of the present invention, tool has the following advantages:
1, the preparation method of nano zine oxide provided by the invention, take zinc subcarbonate as starting raw material, by zinc subcarbonate is joined in particular solution, the ammonia soln of 20 ~ 30wt%, the ammonium bicarbonate aqueous solution of 5 ~ 15wt% or the two mixed solution, can obtain nano level zinc oxide after crystallization, roasting; Do not need the condition accurately limiting raw material reaction to prepare the zinc subcarbonate precursor of specified conditions, simplify preparation technology and operating process; And the zinc subcarbonate after above-mentioned process just can obtain nano level zinc oxide after roasting, improves efficiency, reduces cost, can produce on a large scale.
2. the preparation method of nano zine oxide provided by the invention, the Nano-class zinc oxide particle diameter of preparation is less, can reach units nano level, and median size is
active good.
Accompanying drawing explanation
Fig. 1 is the XRD figure of zinc ammonia solution roasting crystallization at 250 DEG C.
Fig. 2 is the XRD figure of zinc subcarbonate roasting at 250 DEG C.
Embodiment
Below in conjunction with specific examples and accompanying drawing, the present invention will be further described.
In following embodiment, if no special instructions, agents useful for same and equipment are commercially available.
Embodiment 1
(1) added by 10g zinc subcarbonate in the ammonia soln of 20wt% and prepare zinc ammonia solution, wherein zinc concentration is 0.5mol/L.
(2) zinc ammonia solution is dry at 25 DEG C, obtain white crystal.
(3) by white crystal roasting at 250 DEG C, Nano-class zinc oxide is obtained.
As shown in fig. 1, the analytical results wherein about Fig. 1 is as shown in table 1.
Table 1 is the XRD figure analytical results that at 250 DEG C, zinc ammonia solution roasting crystallization obtains Nano-class zinc oxide
| 2θ | D (dust) | Peak height | Area | Area % | Peak width at half height | Crystal grain (dust) |
| 31.7369(0.0191) | 2.8172(0.0027) | 699(9) | 36190(536) | 73.1 | 1.379(0.025) | 61(2) |
| 34.3487(0.0233) | 2.6087(0.0031) | 554(26) | 25529(1356) | 51.6 | 1.393(0.072) | 61(4) |
| 36.2246(0.0191) | 2.4778(0.0019) | 961(23) | 49523(1427) | 100.0 | 1.427(0.049) | 60(3) |
| 47.5185(0.0520) | 1.9119(0.0029) | 147(4) | 12091(366) | 24.4 | 2.139(0.076) | 41(2) |
| 56.5790(0.0178) | 1.6253(0.0010) | 395(9) | 20153(413) | 40.7 | 1.444(0.027) | 64(2) |
| 62.8097(0.0324) | 1.4783(0.0015) | 229(12) | 17129(922) | 34.6 | 1.940(0.121) | 49(4) |
Utilize that peak is strong, peak area and peak width at half height can calculate average grain size through Scherrer formula, as can be seen from above-mentioned Fig. 1 and table 1, Nano-class zinc oxide grain-size is not more than
Zinc subcarbonate crystal is carried out roasting at 250 DEG C, the X diffractogram of product of roasting, as shown in Figure 2, the analytical results wherein about Fig. 2 is as shown in table 2.
| 2θ | D (dust) | Peak height | Area | Area % | Peak width at half height | Crystal grain (dust) |
| 31.7821(0.0027) | 2.8133(0.0005) | 2099(23) | 45299(578) | 59.2 | 0.414(0.007) | 227(5) |
| 34.4405(0.0038) | 2.6019(0.0006) | 1543(19) | 36203(532) | 47.3 | 0.451(0.009) | 207(5) |
| 36.2723(0.0023) | 2.4746(0.0003) | 3260(27) | 76497(741) | 100 | 0.450(0.006) | 209(4) |
| 47.5597(0.0060) | 1.9103(0.0005) | 608(11) | 17046(364) | 22.3 | 0.540(0.015) | 176(6) |
| 56.5963(0.0038) | 1.6249(0.0002) | 1131(16) | 28005(457) | 36.6 | 0.476(0.010) | 211(5) |
| 62.8665(0.0059) | 1.4771(0.0002) | 777(11) | 26624(453) | 34.8 | 0.660(0.015) | 151(4) |
Utilize that peak is strong, peak area and peak width at half height can calculate average grain size through Scherrer formula, as can be seen from above-mentioned Fig. 2 and table 2, Nano-class zinc oxide grain-size is greater than
the Nano-class zinc oxide prepared with the method for embodiment 1 is fewer than the zinc subcarbonate crystal order of magnitude.
Embodiment 2
(1) added by 10g zinc subcarbonate in the ammonium bicarbonate aqueous solution of 15wt% and prepare zinc ammonia solution, wherein zinc concentration is 2mol/L.
(2) zinc ammonia solution is dry at 120 DEG C, obtain white crystal.
(3) by white crystal roasting at 220 DEG C, Nano-class zinc oxide is obtained.
The Nano-class zinc oxide average grain size obtained is
Embodiment 3
(1) added by 25g zinc subcarbonate in the mixed solution of the ammonia soln of 25wt% and the ammonium bicarbonate aqueous solution 1:1 mixing by volume of 10wt% and prepare zinc ammonia solution, wherein zinc concentration is 4mol/L.
(2) zinc ammonia solution is dry at 100 DEG C, obtain white crystal.
(3) by white crystal roasting at 240 DEG C, Nano-class zinc oxide is obtained.
The Nano-class zinc oxide average grain size obtained is
Embodiment 4
(1) added by 10g zinc subcarbonate in the ammonia soln of 30wt% and prepare zinc ammonia solution, wherein zinc concentration is 1mol/L.
(2) zinc ammonia solution is dry at 80 DEG C, obtain white crystal.
(3) by white crystal roasting at 230 DEG C, Nano-class zinc oxide is obtained.
The Nano-class zinc oxide average grain size obtained is
Embodiment 5
(1) added by 15g zinc subcarbonate in the ammonia soln of 20wt% and prepare zinc ammonia solution, wherein zinc concentration is 1mol/L.
(2) zinc ammonia solution is dry at 140 DEG C, obtain white crystal.
(3) by white crystal roasting at 220 DEG C, Nano-class zinc oxide is obtained.
The Nano-class zinc oxide average grain size obtained is
Comparative example 1
(1) added by 10g zinc subcarbonate in the ammonia soln of 10wt% and prepare zinc ammonia solution, wherein zinc concentration is 0.3mol/L.
(2) zinc ammonia solution is dry at 25 DEG C, obtain white crystal.
(3) by white crystal roasting at 250 DEG C.Obtain white powder.
The white powder obtained is zinc subcarbonate and zinc oxide mix.
Comparative example 2
(1) added by 10g zinc subcarbonate in the ammonia soln of 40wt% and prepare zinc ammonia solution, wherein zinc concentration is 0.5mol/L.
(2) zinc ammonia solution is dry at 25 DEG C, obtain white crystal.
(3) by white crystal roasting at 240 DEG C.The Nano-class zinc oxide obtained.
The Nano-class zinc oxide average grain size obtained is
Comparative example 3
(1) added by 25g zinc subcarbonate in the ammonium bicarbonate aqueous solution of 20wt% and prepare zinc ammonia solution, wherein zinc concentration is 2mol/L.
(2) zinc ammonia solution is dry at 140 DEG C, obtain white crystal.
(3) by white crystal roasting at 200 DEG C, white powder is obtained.
The white powder obtained is zinc subcarbonate and zinc oxide mix.
Obviously, above-described embodiment is only for clearly example being described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And thus the apparent change of extending out or variation be still among the protection domain of the invention.
Claims (10)
1. a preparation method for nano zine oxide, is characterized in that, comprises step as follows: added by zinc subcarbonate in ammonia solution and prepare zinc ammonia solution, by zinc ammonia solution drying crystalline, roasting, obtains nano zine oxide; Described ammonia solution is the ammonia soln of 20 ~ 30wt%, the ammonium bicarbonate aqueous solution of 5 ~ 15wt% or the two mixed solution.
2. the preparation method of nano zine oxide according to claim 1, is characterized in that, in described mixed solution, the mass ratio of the ammonium bicarbonate aqueous solution of 20 ~ 30wt% ammonia soln and 5 ~ 15wt% is 1-99:99-1.
3. the preparation method of nano zine oxide according to claim 1 and 2, is characterized in that, described ammonia solution is the ammonia soln of 25wt%, the ammonium bicarbonate aqueous solution of 10wt% or the two mixed solution.
4. the preparation method of the nano zine oxide according to any one of claim 1-3, is characterized in that, in described zinc ammonia solution, zinc concentration is 0.5 ~ 4mol/L.
5. the preparation method of nano zine oxide according to claim 4, is characterized in that, in described zinc ammonia solution, zinc concentration is 2 ~ 3.5mol/L.
6. the preparation method of the nano zine oxide according to any one of claim 1-5, is characterized in that, the mass volume ratio of zinc subcarbonate and ammonia solution is 10-30g/100mL.
7. the preparation method of the nano zine oxide according to any one of claim 1-6, is characterized in that, the temperature of described drying is 25 ~ 140 DEG C.
8. the preparation method of nano zine oxide according to claim 7, is characterized in that, the temperature of described drying is 40 ~ 80 DEG C.
9. the preparation method of the nano zine oxide according to any one of claim 1-8, is characterized in that, the temperature of described roasting is 200 ~ 400 DEG C.
10. the preparation method of nano zine oxide according to claim 9, is characterized in that, the temperature of described roasting is 220 ~ 240 DEG C.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1077753A (en) * | 1992-04-18 | 1993-10-27 | 景治熙 | Active zinc flower and high-purity zinc oxide preparation technology |
| CN1986421A (en) * | 2006-12-21 | 2007-06-27 | 天津化工研究设计院 | Preparing process of nano zinc oxide |
| JP2013001578A (en) * | 2011-06-13 | 2013-01-07 | Sakai Chem Ind Co Ltd | Zinc oxide, method for producing zinc oxide, cosmetic, coating composition, and resin composition |
| CN103395825A (en) * | 2012-08-19 | 2013-11-20 | 衡阳师范学院 | Method for producing nanometer zinc oxide by using steelmaking electric-furnace flue dust |
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- 2015-11-19 CN CN201510807727.5A patent/CN105347386A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1077753A (en) * | 1992-04-18 | 1993-10-27 | 景治熙 | Active zinc flower and high-purity zinc oxide preparation technology |
| CN1986421A (en) * | 2006-12-21 | 2007-06-27 | 天津化工研究设计院 | Preparing process of nano zinc oxide |
| JP2013001578A (en) * | 2011-06-13 | 2013-01-07 | Sakai Chem Ind Co Ltd | Zinc oxide, method for producing zinc oxide, cosmetic, coating composition, and resin composition |
| CN103395825A (en) * | 2012-08-19 | 2013-11-20 | 衡阳师范学院 | Method for producing nanometer zinc oxide by using steelmaking electric-furnace flue dust |
Non-Patent Citations (1)
| Title |
|---|
| 唐谟堂等: "《配合物冶金理论与技术》", 31 October 2011 * |
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