CN109095495A - The method of anhydrous zinc chloride is prepared from material containing zinc - Google Patents
The method of anhydrous zinc chloride is prepared from material containing zinc Download PDFInfo
- Publication number
- CN109095495A CN109095495A CN201811068499.4A CN201811068499A CN109095495A CN 109095495 A CN109095495 A CN 109095495A CN 201811068499 A CN201811068499 A CN 201811068499A CN 109095495 A CN109095495 A CN 109095495A
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- CN
- China
- Prior art keywords
- zinc
- chloride
- dichloro diamino
- material containing
- dichloro
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/04—Halides
Abstract
The present invention discloses a kind of method that anhydrous zinc chloride is prepared from material containing zinc, it is cumbersome to solve existing zinc chloride production, energy consumption is high, the big problem of water consumption, method includes a) using material containing zinc leached, filtered containing ammonium chloride or hydrochloric acid-ammonium chloride mixed system leaching agent, obtains the leachate containing zinc chloride and dichloro diamino zinc；B) leachate is used after adjusting pH value of solution progress ammino reaction containing the adjusting liquid of liquefied ammonia or ammonium hydroxide, obtains the solution precipitated containing dichloro diamino zinc；C) solution precipitated containing dichloro diamino zinc is filtered, obtains dichloro diamino zinc precipitating, and dichloro diamino zinc precipitating is subjected to impurity washing using ammonium chloride solution；D) the dichloro diamino zinc precipitating after washing dried, calcined, control 350~450 degree of calcination temperature, 30~60min of heating-up time, 30~60min of soaking time, cooling after the completion of heat preservation, cooling obtains anhydrous zinc chloride.The present invention has the characteristics that adaptability to raw material is strong, the short economy of process is high and small investment.
Description
Technical field
The method that the present invention relates to a kind of to prepare anhydrous zinc chloride from material containing zinc.
Background technique
Zinc chloride is generally raw material using zinc oxide and cadmia, carries out dissolution leaching using hydrochloric acid during production
Zinc obtains liquor zinci chloridi and passes through except the processes such as iron, displacement, evaporation to zinc chloride, and preparing anhydrous zinc chloride by this method needs
To pass through high temperature evaporation, dehydration, it is higher to the energy consumption of evaporation process, and technical process is relatively cumbersome, and energy consumption is high, uses water
Amount is big.Therefore traditional handicraft method prepares zinc chloride although technics comparing is mature, but there are problems.
Summary of the invention
In view of the deficiencies of the prior art, the method that the present invention provides a kind of to prepare anhydrous zinc chloride from material containing zinc,
This method has the characteristics that adaptability to raw material is strong, the short economy of process is high and small investment.
To achieve the above object, the present invention provides the following technical scheme that
A method of preparing anhydrous zinc chloride from material containing zinc, which comprises
Step a), which uses material containing zinc, to be leached containing ammonium chloride or hydrochloric acid-ammonium chloride mixed system leaching agent, is filtered,
Obtain the leachate containing zinc chloride and dichloro diamino zinc；
Leachate is used and carries out pH adjusting containing the adjusting liquid of liquefied ammonia or ammonium hydroxide by step b), and the zinc chloride in leachate is whole
Ammino reaction is carried out, dichloro diamino zinc is converted into, obtains the solution precipitated containing dichloro diamino zinc；
Step c) filters the solution precipitated containing dichloro diamino zinc, obtains dichloro diamino zinc precipitating, and dichloro diamino zinc is sunk
It forms sediment and impurity washing is carried out using ammonium chloride solution；
Step d) is sent into calcining furnace after the dichloro diamino zinc precipitating after washing is dried, and controls calcination temperature 350~450
Degree, 30~60min of heating-up time, 30~60min of soaking time carry out cooling, cool down, obtain anhydrous chlorination after the completion of heat preservation
Zinc.
Preferably, in 15~50g/L, the concentration of ammonium chloride is controlled in 2~6mol/ for the concentration control of zinc ion in step a)
L。
Preferably, leachate uses and carries out pH adjusting, reaction time containing the adjusting liquid of liquefied ammonia or ammonium hydroxide in step b)
It controls for 30~90min, pH 6.3~6.7.
Preferably, the mother liquor after the precipitation dichloro diamino zinc that step b) obtains is by extraction process to gold remaining in mother liquor
Belong to and carry out extraction and separation, the solution return step a) obtained after extraction is continued to use.
Preferably, the concentration of ammonium chloride solution is 2~6 mol/L in step c).
Preferably, dichloro diamino zinc can generate ammonia in calcination process in step d), after the ammonia is by collecting, absorbing
Return step b) is used.
Advantages of the present invention are as follows: the characteristics of adaptability to raw material is strong, the short economy of process is high and small investment.
Detailed description of the invention
Fig. 1 is the process flow chart that material containing zinc provided by the present embodiment prepares zinc chloride.
Specific embodiment
It is described further in conjunction with the method that 1 couple of present invention of attached drawing prepares anhydrous zinc chloride from material containing zinc.
A method of preparing anhydrous zinc chloride from material containing zinc, which comprises
Step a), which uses material containing zinc, to be leached containing ammonium chloride or hydrochloric acid-ammonium chloride mixed system leaching agent, is filtered,
Obtain the leachate containing zinc chloride and dichloro diamino zinc, wherein the concentration control of zinc ion is in 15~50g/L, ammonium chloride it is dense
Degree control is in 2~6mol/L.
Step b) by leachate use containing the adjusting liquid of liquefied ammonia or ammonium hydroxide carry out pH adjusting, control the reaction time be 30~
90min controls pH 6.4~6.6, so that ammonium ion and zinc ion form zinc ammonia complex dichloro diamino zinc in the solution, it is molten
After dichloro diamino zinc in liquid reaches saturation, dichloro diamino zinc precipitating is constantly formed, to obtain precipitating containing dichloro diamino zinc
Solution.
Step c) filters the solution precipitated containing dichloro diamino zinc, obtains dichloro diamino zinc precipitating, and by dichloro diamino
Zinc precipitating carries out impurity washing using 2~6 mol/L ammonium chloride solutions.
Step d) is sent into calcining furnace after the dichloro diamino zinc precipitating after washing is dried, and controls calcination temperature 350
~450 degree, 30~60min of heating-up time, 30~60min of soaking time, cooling is carried out after the completion of heat preservation, is cooled down, is obtained anhydrous
Zinc chloride；In the step, dichloro diamino zinc can generate ammonia in calcination process, and the ammonia is by collecting, absorbing return step
B) it continues to use.
The present embodiment is further arranged to: the mother liquor after the precipitation dichloro diamino zinc that step b) obtains passes through extraction process pair
The residual metallic leached in mother liquor is such as: after copper, cadmium, lead, cobalt, nickel carry out extraction and separation, i.e. slective extraction according to actual needs
Technique, such as zinc extraction, cadmium extraction, copper extraction, lead extraction, cobalt extraction, nickel extraction, by copper, cadmium, lead, cobalt, the nickel etc. in mother liquor
After metal ion carries out separating-purifying, the solution return step a) obtained after extraction is continued to use.
In the present embodiment, the material containing zinc in step a) is complicated from Pb-Zn deposits, zinc oxide ore, soot containing zinc, low taste
Residues containing zinc, zinc-containing sludge, one or more of containing zinc slag containing chlorine.
The following are concrete operations examples:
Being leached by ammonium chloride containing zinc material containing chlorine containing zinc 25%, obtains zinc chloride, dichloro diamino zinc of the zinc concentration in 30g/l
Mixed solution.At normal temperature, which adjusts liquid using ammonium hydroxide and adjusts pH value of solution, control solution terminal pH 6.4~4.6, it is anti-
30min between seasonable constantly forms dichloro diamino zinc white precipitate in solution.After filtering, obtained dichloro diamino zinc is used
The ammonium chloride solution of 3mol/L is washed, and the foreign metal ion of entrainment is washed away.Dichloro diamino zinc after washing, is dried
Afterwards, it is sent into calcined by rotary kiln system, calcination temperature rises at 370~400 DEG C in 60min, later soaking time 30min, protects
Cool down after the completion of temperature, obtains anhydrous zinc chloride.The another kind products gaseous ammonia obtained in calcination process passes through negative pressure absorbing
It is recycled, return system is reused.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (6)
1. a kind of method that anhydrous zinc chloride is prepared from material containing zinc, it is characterized in that: the described method includes:
Step a), which uses material containing zinc, to be leached containing ammonium chloride or hydrochloric acid-ammonium chloride mixed system leaching agent, is filtered,
Obtain the leachate containing zinc chloride and dichloro diamino zinc；
Leachate is used and carries out pH adjusting containing the adjusting liquid of liquefied ammonia or ammonium hydroxide by step b), and the zinc chloride in leachate is whole
Ammino reaction is carried out, dichloro diamino zinc is converted into, obtains the solution precipitated containing dichloro diamino zinc；
Step c) filters the solution precipitated containing dichloro diamino zinc, obtains dichloro diamino zinc precipitating, and dichloro diamino zinc is sunk
It forms sediment and impurity washing is carried out using ammonium chloride solution；
Step d) is sent into calcining furnace after the dichloro diamino zinc precipitating after washing is dried, and controls calcination temperature 350~450
Degree, 30~60min of heating-up time, 30~60min of soaking time carry out cooling, cool down, obtain anhydrous chlorination after the completion of heat preservation
Zinc.
2. the method according to claim 1 for preparing anhydrous zinc chloride from material containing zinc, it is characterized in that: zinc in step a)
The concentration control of ion is controlled in 15~50g/L, the concentration of ammonium chloride in 2~6mol/L.
3. the method according to claim 1 for preparing anhydrous zinc chloride from material containing zinc, it is characterized in that: being soaked in step b)
Liquid, which is used, out carries out pH adjusting containing the adjusting liquid of liquefied ammonia or ammonium hydroxide, and the reaction time is 30~90min, pH control 6.3~
6.7。
4. the method according to claim 1 for preparing anhydrous zinc chloride from material containing zinc, it is characterized in that: step b) obtains
Be precipitated dichloro diamino zinc after mother liquor by extraction process to metal remaining in mother liquor carry out extraction and separation, obtained after extraction
Solution return step a) continue to use.
5. the method according to claim 1 for preparing anhydrous zinc chloride from material containing zinc, it is characterized in that: chlorine in step c)
The concentration for changing ammonium salt solution is 2~6 mol/L.
6. the method according to claim 1 for preparing anhydrous zinc chloride from material containing zinc, it is characterized in that: two in step d)
Chlorine diamino zinc can generate ammonia in calcination process, which is used by return step b) after collecting, absorbing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811068499.4A CN109095495A (en) | 2018-09-13 | 2018-09-13 | The method of anhydrous zinc chloride is prepared from material containing zinc |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811068499.4A CN109095495A (en) | 2018-09-13 | 2018-09-13 | The method of anhydrous zinc chloride is prepared from material containing zinc |
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| Publication Number | Publication Date |
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| CN109095495A true CN109095495A (en) | 2018-12-28 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201811068499.4A Pending CN109095495A (en) | 2018-09-13 | 2018-09-13 | The method of anhydrous zinc chloride is prepared from material containing zinc |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115927873A (en) * | 2022-11-24 | 2023-04-07 | 东北大学 | Method for preparing zinc oxide by wet processing of secondary zinc oxide smoke dust |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093418A (en) * | 1993-04-09 | 1994-10-12 | 广州市新技术应用研究所 | Complex compound electrolysis system zinc |
| CN102212700A (en) * | 2011-05-31 | 2011-10-12 | 新干县金山化工厂 | Production method of high-purity anhydrous zinc chloride |
| CN104276595A (en) * | 2014-10-28 | 2015-01-14 | 东江环保股份有限公司 | Preparation method of basic zinc chloride |
| CN107857291A (en) * | 2017-12-01 | 2018-03-30 | 广州科城环保科技有限公司 | A kind of basic zinc chloride particulate matter and preparation method thereof |
| CN108300855A (en) * | 2018-02-05 | 2018-07-20 | 彭勃 | A kind of process of the joint of double-flow containing zinc oxide leaching and mixed liquid electrolytic zinc |
-
2018
- 2018-09-13 CN CN201811068499.4A patent/CN109095495A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093418A (en) * | 1993-04-09 | 1994-10-12 | 广州市新技术应用研究所 | Complex compound electrolysis system zinc |
| CN102212700A (en) * | 2011-05-31 | 2011-10-12 | 新干县金山化工厂 | Production method of high-purity anhydrous zinc chloride |
| CN104276595A (en) * | 2014-10-28 | 2015-01-14 | 东江环保股份有限公司 | Preparation method of basic zinc chloride |
| CN107857291A (en) * | 2017-12-01 | 2018-03-30 | 广州科城环保科技有限公司 | A kind of basic zinc chloride particulate matter and preparation method thereof |
| CN108300855A (en) * | 2018-02-05 | 2018-07-20 | 彭勃 | A kind of process of the joint of double-flow containing zinc oxide leaching and mixed liquid electrolytic zinc |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115927873A (en) * | 2022-11-24 | 2023-04-07 | 东北大学 | Method for preparing zinc oxide by wet processing of secondary zinc oxide smoke dust |
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Application publication date: 20181228 |