CN105366706A - Preparation method of nano-sized basic zinc carbonate - Google Patents
Preparation method of nano-sized basic zinc carbonate Download PDFInfo
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- CN105366706A CN105366706A CN201410420362.6A CN201410420362A CN105366706A CN 105366706 A CN105366706 A CN 105366706A CN 201410420362 A CN201410420362 A CN 201410420362A CN 105366706 A CN105366706 A CN 105366706A
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Abstract
The invention discloses a preparation method of nano-sized basic zinc carbonate, and relates to the field of chemical industry. The preparation method comprises the technological processes of raw material preparation, a reaction under water bath condition and cleaning and drying. According to the technological method, the nano-sized basic zinc carbonate is prepared through a hydrogen sulfate-ammonium bicarbonate method, the preparation technology is simple, the raw materials are low in cost and wide in source, the method can be easily mastered and operated by a worker, and the preparation efficiency is high; a certain mass fraction of magnesium element is doped, the grain size of basic zinc carbonate powder is significantly decreased, and the larger the mass fraction of the magnesium element is, the larger the grain size of the basic zinc carbonate powder is. Therefore, according to the technological method, the addition amount of the magnesium element is strictly controlled, the grain size of the basic zinc carbonate powder can reach the optimum value; in the reaction process, by means of reasonably controlling the reaction temperature and the stirring speed, the reaction rate is increased, the reaction time is shortened, and meanwhile the grain size of the basic zinc carbonate powder is indirectly decreased.
Description
Technical field
The present invention relates to chemical field, be specifically related to a kind of preparation method of nanometer zinc subcarbonate.
Background technology
Zinc subcarbonate is a kind of white trickle amorphous powder, odorless, tasteless, water insoluble and alcohol, be slightly soluble in ammoniacal liquor, dissolve in diluted acid and sodium hydroxide, be the effect of 30% with massfraction, discharge, form superoxide, at 250 ~ 500 DEG C, heat by different time, when being cooled to room temperature, fluorescence phenomenon can be there is, it is widely used in medicine, rubber, latex product, the sweetening agent of petrochemical complex and chemical fertilizer, catalyzer and fodder additives etc., at present, what market was sold is common zinc subcarbonate, its index Zn content, loss on ignition, heavy metal Pb content, moisture vitriol amount (in), screenings (wet screening 100um), cadmium content does not all propose specific requirement to its grain fineness number, application number is that CN200510031183.4 discloses a kind of alkaline zinc carbonate nano-wire and preparation method thereof, it mainly solves technical problems such as now there is no alkaline zinc carbonate nano-wire material and preparation method, its drip irrigation device is: with zinc oxide (or zinc salt) for raw material, with ammoniacal liquor (or EDTA) for coordination agent, soluble carbonate salt is precipitation agent, reaction generates Zn complex solution, then distilled water or other solvents is added, or heat, or not only added water or other solvents but also heated, zinc subcarbonate is made to precipitate equably and generate nano thread, to be separated by filtration again and after using distilled water (or weak ammonia) washing precipitation, alkaline zinc carbonate nano-wire is obtained through super-dry, it prepares zinc subcarbonate in water solution system, technical process is simple, reaction conditions is gentle, preparation cost is very cheap, but the zinc subcarbonate grain fineness number that this kind of method is prepared is large, Zn content is low, inferior quality, be not suitable for the raw material being used as some makeup.
Summary of the invention
It is simple that problem to be solved by this invention is to provide a kind of production technique, and grain fineness number is low, the preparation method of the nanometer zinc subcarbonate that Zn content is high.
To achieve these goals, the technical scheme that the present invention takes for: the preparation method of a kind of nanometer zinc subcarbonate provided, comprises following processing step:
(1) raw material is prepared: zinc sulfate and the magnesium sulfate mixed solution system of preparing certain substance withdrawl syndrome, for subsequent use;
(2) react under water bath condition: the solution prepared in step (1) is placed in the water-bath that design temperature is 56 ~ 63 DEG C, stir, and slowly add ammonium bicarbonate soln to system, at this moment system generates zinc subcarbonate white precipitate, and releases CO
2bubble, and the pH value using PH test paper assaying reaction solution, when pH value reaches about 6.5, bubbles volume starts to reduce, and when pH value reaches 7.0, no longer includes bubble and produces, illustrate that reaction terminates, continue constant temperature 2 ~ 3h, stop heating and stir, sedimentation 30 ~ 45min;
(3) cleaning, drying: the white precipitate produced in filtration step (2), first distilled water white laundry precipitation 2 ~ 3 times are used, re-use dispersion agent white laundry precipitation 3 ~ 4 times, after washing is good, white precipitate is placed in vacuum-drying 2 ~ 3h at 110 DEG C of temperature, nanometer zinc subcarbonate powder can be obtained.
Preferably, in described step (1) zinc sulfate and magnesium sulfate mixed solution system in the amount of substance ratio of zinc sulfate and magnesium sulfate be 56:1.3.
Preferably, the equipment that in described step (2), stirring technique is used is electric blender.
Preferably, controlling stirring velocity in described step (2) is 350 ~ 400r/min.
Preferably, the dispersion agent described in described step (3) is dehydrated alcohol.
Preferably, the equipment that in described step (3), drying process is used is vacuum drying oven.
Adopt technical scheme of the present invention, hydrogen sulfate-ammonium bicarbonate method is adopted to prepare nanometer zinc subcarbonate, preparation technology is simple, raw materials cost is low, source is wide, workman easily grasps and operates, preparation efficiency is high, by mixing the magnesium elements of certain mass mark wherein, significantly reduce the grain fineness number of zinc subcarbonate powder, along with the increase of magnesium elements massfraction, the grain fineness number of zinc subcarbonate powder can become large thereupon, therefore, by the strict add-on controlling magnesium elements in this processing method, its grain fineness number is made to reach optimum value, in reaction process, by conservative control temperature of reaction and stirring velocity, improve speed of reaction, decrease the reaction times, also indirectly reduce the grain fineness number of zinc subcarbonate powder simultaneously.
Embodiment
embodiment 1:
(1) prepare raw material: zinc sulfate and the magnesium sulfate mixed solution system of preparing certain substance withdrawl syndrome, for subsequent use, wherein, the amount of substance ratio of described zinc sulfate and magnesium sulfate is 56:1.3;
(2) react under water bath condition: the solution prepared in step (1) is placed in the water-bath that design temperature is 56 DEG C, use electric blender stirs, control stirring velocity is 350r/min, and slowly add ammonium bicarbonate soln to system, at this moment system generates zinc subcarbonate white precipitate, and releases CO
2bubble, and the pH value using PH test paper assaying reaction solution, when pH value reaches about 6.5, bubbles volume starts to reduce, and when pH value reaches 7.0, no longer includes bubble and produces, illustrate that reaction terminates, continue constant temperature 2h, stop heating and stir, sedimentation 32min;
(3) cleaning, drying: the white precipitate produced in filtration step (2), first distilled water white laundry is used to precipitate 2 times, re-use dehydrated alcohol dispersion agent white laundry and precipitate 3 times, vacuum-drying 2h in the vacuum drying oven after washing is good, white precipitate being placed in 110 DEG C of temperature, can obtain nanometer zinc subcarbonate powder.
embodiment 2:all the other are identical with embodiment 1, and difference is that, in described step (2), temperature of reaction is 62 DEG C, and stirring velocity is 360r/min, and constant temperature time is 3h, and the settling time is 43min; In described step (3), use distilled water white laundry to precipitate 2 times, use dehydrated alcohol dispersion agent white laundry to precipitate 4 times, the vacuum-drying time is 3h.
embodiment 3:all the other are identical with embodiment 1, and difference is that, in described step (1), temperature of reaction is 63 DEG C, and stirring velocity is 365r/min, and constant temperature time is 3h, and the settling time is 42min; In described step (3), use distilled water white laundry to precipitate 3 times, use dehydrated alcohol dispersion agent white laundry to precipitate 4 times, the vacuum-drying time is 2.5h.
embodiment 4:all the other are identical with embodiment 1, and difference is that, in described step (1), temperature of reaction is 62 DEG C, and stirring velocity is 358r/min, and constant temperature time is 3h, and the settling time is 41min; In described step (3), use distilled water white laundry to precipitate 3 times, use dehydrated alcohol dispersion agent white laundry to precipitate 3 times, the vacuum-drying time is 2.5h.
After above processing step, take out nanometer zinc subcarbonate powder sample, to be measured:
From above data, the nanometer zinc subcarbonate powder sample grain fineness number produced is at below 10mm, and grain fineness number is low, and Zn content is more than 55%, Zn content is high, and Mg content is about 1.32%, and foreign matter content is below 1%, foreign matter content is low, and processing method is simple, easily grasps.
Obvious specific implementation of the present invention is not subject to the restrictions described above; as long as have employed the improvement of the various unsubstantialities that method of the present invention is conceived and technical scheme is carried out; or design of the present invention and technical scheme directly applied to other occasion, all within protection scope of the present invention without to improve.
Claims (6)
1. a preparation method for nanometer zinc subcarbonate, comprises following processing step:
(1) raw material is prepared: zinc sulfate and the magnesium sulfate mixed solution system of preparing certain substance withdrawl syndrome, for subsequent use;
(2) react under water bath condition: the solution prepared in step (1) is placed in the water-bath that design temperature is 56 ~ 63 DEG C, stir, and slowly add ammonium bicarbonate soln to system, at this moment system generates zinc subcarbonate white precipitate, and releases CO
2bubble, and the pH value using PH test paper assaying reaction solution, when pH value reaches about 6.5, bubbles volume starts to reduce, and when pH value reaches 7.0, no longer includes bubble and produces, illustrate that reaction terminates, continue constant temperature 2 ~ 3h, stop heating and stir, sedimentation 30 ~ 45min;
(3) cleaning, drying: the white precipitate produced in filtration step (2), first distilled water white laundry precipitation 2 ~ 3 times are used, re-use dispersion agent white laundry precipitation 3 ~ 4 times, after washing is good, white precipitate is placed in vacuum-drying 2 ~ 3h at 110 DEG C of temperature, nanometer zinc subcarbonate powder can be obtained.
2. the preparation method of a kind of nanometer zinc subcarbonate according to claim 1, is characterized in that: in the mixed solution system of the middle zinc sulfate of described step (1) and magnesium sulfate, the amount of substance ratio of zinc sulfate and magnesium sulfate is 56:1.3.
3. the preparation method of a kind of nanometer zinc subcarbonate according to claim 1, is characterized in that: the equipment that in described step (2), stirring technique is used is electric blender.
4. the preparation method of a kind of nanometer zinc subcarbonate according to claim 1, is characterized in that: controlling stirring velocity in described step (2) is 350 ~ 400r/min.
5. the preparation method of a kind of nanometer zinc subcarbonate according to claim 1, is characterized in that: the dispersion agent described in described step (3) is dehydrated alcohol.
6. the preparation method of a kind of nanometer zinc subcarbonate according to claim 1, is characterized in that: the equipment that in described step (3), drying process is used is vacuum drying oven.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410420362.6A CN105366706A (en) | 2014-08-25 | 2014-08-25 | Preparation method of nano-sized basic zinc carbonate |
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| CN201410420362.6A CN105366706A (en) | 2014-08-25 | 2014-08-25 | Preparation method of nano-sized basic zinc carbonate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023124478A1 (en) * | 2021-12-30 | 2023-07-06 | Tcl科技集团股份有限公司 | Basic zinc salt nanoparticles and preparation method therefor, and quantum dot light-emitting diode |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045956A (en) * | 1989-03-27 | 1990-10-10 | 吉林市金刚化工厂 | Produce zinc subcarbonate and active zinc flower with ammonium bicarbonate precipitation method |
| CN1053412A (en) * | 1990-01-19 | 1991-07-31 | 辛集市化工二厂 | The bicarbonate of ammonia neutralisation is produced zinc oxide |
-
2014
- 2014-08-25 CN CN201410420362.6A patent/CN105366706A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045956A (en) * | 1989-03-27 | 1990-10-10 | 吉林市金刚化工厂 | Produce zinc subcarbonate and active zinc flower with ammonium bicarbonate precipitation method |
| CN1053412A (en) * | 1990-01-19 | 1991-07-31 | 辛集市化工二厂 | The bicarbonate of ammonia neutralisation is produced zinc oxide |
Non-Patent Citations (1)
| Title |
|---|
| 侯新刚等: "碱式碳酸锌晶粒细化的工艺研究", 《无机盐工业》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023124478A1 (en) * | 2021-12-30 | 2023-07-06 | Tcl科技集团股份有限公司 | Basic zinc salt nanoparticles and preparation method therefor, and quantum dot light-emitting diode |
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