CN102602980A - Industrial preparation method of alkali copper sulfate - Google Patents
Industrial preparation method of alkali copper sulfate Download PDFInfo
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- CN102602980A CN102602980A CN2012101235999A CN201210123599A CN102602980A CN 102602980 A CN102602980 A CN 102602980A CN 2012101235999 A CN2012101235999 A CN 2012101235999A CN 201210123599 A CN201210123599 A CN 201210123599A CN 102602980 A CN102602980 A CN 102602980A
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Abstract
The invention discloses an industrial preparation method of alkali copper sulfate. The used materials are non-toxic and harmless and can be obtained at low cost, which is good for industrial production; in the production process, citric acid root ion is used as a complexing agent so that the product grain size is increased, which is beneficial to cleaning; usually, washing just needs to be carried out twice and the production efficiency is improved; after reaction, the citric acid root ion is remained in the waste water, is non-toxic, pollution-free and degradable, and can be complex with heavy metal ions (such as arsenic and lead) possibly existing in the production system so that the heavy metal ions can be discharged out of the production system together with the waste water, thereby effectively preventing the heavy metal ions from entering the target output and further improving the purity of the product. In addition, ammonia nitrogen is not involved in the production process, thereby solving the problem of recycling of ammonia nitrogen in the traditional method. Therefore, the invention has favorable social and economical benefits.
Description
Technical field
The present invention relates to a kind of preparation method of compound of copper, be specifically related to a kind of industrial production process of Basic Chrome Sulphate.
Background technology
Basic Chrome Sulphate is the staple of inorganic copper fungicide Bordeaux mixture; The additive that can be used as trace copper is applied in the feed; Can also be widely used in the public nuisance-free agricultural chemicals as sterilant, sterilant, a kind of production efficiency is high, the preparation method of good product quality but lack on the market always.Such as; Application number is that 201010117119.9 patent has proposed to utilize the electronics waste liquid to add the method that alkali ammonia excretion legal system is equipped with Basic Chrome Sulphate; Can prepare Basic Chrome Sulphate; But have following main drawback: 1, Schweitzeros reagent forms verditer easily under alkaline condition, influences product gas purity and quality; 2, in the preparation system ammonia nitrogen is arranged, can be very not thorough and reclaim ammonia nitrogen with heating ammonia excretion method, it is very high thoroughly to reclaim the ammonia nitrogen cost, reclaims thoroughly then not pollute the environment.And for example application number is that 200810107597.4 patent has proposed in ammonium copper sulfate solution, to feed carbonic acid gas and prepares Basic Chrome Sulphate, and its main drawback is: 1, part copper can form ventilation breather with carbonic acid gas, influences product gas purity and quality; 2, carbonic acid gas is a gas phase, and solution is liquid phase, and the reaction between gas phase and the liquid phase can cause production efficiency low; And the problem that exists ammonia nitrogen to be difficult to reclaim equally in the reaction system.
Summary of the invention
For solving the deficiency of prior art; The object of the present invention is to provide a kind of industrial production process of Basic Chrome Sulphate, adopt cheap and easy to get, nontoxic raw materials for production, technological process is simple; When guaranteeing quality product, can enhance productivity, and then reduce production cost.Solved also that output receives the restriction of raw material and the ammonia nitrogen problem in the factory effluent in the prior preparation method.
In order to realize above-mentioned target, the present invention adopts following technical scheme:
A kind of industrial production process of Basic Chrome Sulphate is characterized in that, comprises the steps:
A, preparation contain the A solution of sulfate ion and cupric ion, and be for use;
B, preparation contain the B solution of hydroxide ion, and be for use;
C, introducing complexing agent: add complexing agent C at least one in above-mentioned A solution and B solution; Above-mentioned complexing agent C dissolving back forms the solution that comprises citrate ion; After carrying out this step, above-mentioned A solution and B solution respectively again note make A1 solution and B1 solution;
D, simultaneously, flow in the reaction kettle lentamente with A1 solution and B1 solution, chemical reaction takes place in both, and it is 3 ~ 9 that the flow of regulating A1 solution and B1 solution in the reaction process makes the pH value of reaction kettle for reaction liquid, produces intermediate product;
E, intermediate product is transferred in the suction filter, washs to washings and be neutral, and carry out suction filtration, produce primary product tentatively to dewater;
F, primary product is dried processing, prepare the title product Basic Chrome Sulphate.
A kind of industrial production process of aforesaid Basic Chrome Sulphate; It is characterized in that; Above-mentioned A solution directly is acid wiring board bluestone waste, perhaps is copper-bath, is perhaps made by one or more and sulfuric acid reaction in verditer, ventilation breather, the cupric oxide.
A kind of industrial production process of aforesaid Basic Chrome Sulphate is characterized in that, above-mentioned B solution is sodium hydroxide and/or potassium hydroxide solution.
A kind of industrial production process of aforesaid Basic Chrome Sulphate is characterized in that, above-mentioned complexing agent C is Hydrocerol A or solubility Citrate trianion.
A kind of industrial production process of aforesaid Basic Chrome Sulphate is characterized in that, the mass concentration of cupric ion is 2% ~ 12% in the above-mentioned A solution.
A kind of industrial production process of aforesaid Basic Chrome Sulphate is characterized in that, the mass concentration of hydroxide ion is 5% ~ 15% in the above-mentioned B solution.
A kind of industrial production process of aforesaid Basic Chrome Sulphate is characterized in that, the mol ratio of above-mentioned cupric ion and citrate ion is 1:0.01 ~ 0.8.
A kind of industrial production process of aforesaid Basic Chrome Sulphate is characterized in that, the temperature of reaction among the above-mentioned steps d is 35 ~ 75 ℃.
A kind of industrial production process of aforesaid Basic Chrome Sulphate is characterized in that, adopts pH electrode that the pH value of reaction kettle for reaction liquid is monitored among the above-mentioned steps d.
A kind of industrial production process of aforesaid Basic Chrome Sulphate is characterized in that, the pH value of reaction solution is 4 ~ 7 among the above-mentioned steps d.
Usefulness of the present invention is: a kind of industrial production process of Basic Chrome Sulphate of the present invention, and the advantages of nontoxic raw materials of employing is harmless and cheap and easy to get, helps the industriallization volume production; Adopt citrate ion as complexing agent in the production process; Make product granularity obtain growth, help cleaning, generally carry out twice washing and get final product; Can enhance productivity; Citrate ion remained in the waste water after reaction was accomplished, and nontoxic, pollution-free and easy degraded makes heavy metal ion discharge production system with waste water but also can carry out complexing with the heavy metal ion (like arsenic, lead) that possibly exist in the production system; Effectively avoid heavy metal ion to enter into title product, further improve degree of purity of production; In addition, do not relate to ammonia nitrogen in the production process, solved the problem of the ammonia nitrogen of puzzlement recovery always in the traditional method.Therefore the present invention has good society and economic benefit.
Description of drawings
Fig. 1 is the synoptic diagram of preferred embodiment of a kind of industrial production process of Basic Chrome Sulphate of the present invention.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is done concrete introduction.
With reference to Fig. 1, the industrial production process of Basic Chrome Sulphate of the present invention comprises following step:
A, preparation contain sulfate ion (SO
4 2-) and cupric ion (Cu
2+) A solution, for use;
Specifically, A solution can directly be acid wiring board bluestone waste, can directly utilize trade waste like this, reduces production costs; Also can be copper-bath, perhaps make by one or more and sulfuric acid reaction in verditer, ventilation breather, the cupric oxide.Among the present invention, the concentration of A solution there is not special requirement, as a kind of preferred, in order to take into account production cost, production efficiency and productive rate, Cu in the A solution
2+Mass concentration be 2% ~ 12%.
B, preparation contain hydroxide ion (OH
-) B solution, for use;
B solution is the solubility hydroxide solution, like industrial lye, sodium hydroxide and/or potassium hydroxide solution.As a kind of preferred, OH in the B solution
-Mass concentration be 5% ~ 15%, can take into account production cost, efficient and productive rate like this.
Need to prove that the order of step a and step b is unrestricted, that is to say that can carry out step b earlier and carry out step a again, this is clearly, does not give unnecessary details here.
Introduce complexing agent C in c, in A solution and B solution at least one, should form after the complexing agent C dissolving and comprise citrate ion (C
6H
5O
7 3-) solution, obscure for the ease of describing and being unlikely to cause, after having carried out this step, A solution and B solution are remembered again respectively and are made A1 solution and B1 solution.
That is to say, no matter A solution and B solution are only to have wherein a kind ofly to have added complexing agent C or all added complexing agent C in step c, after having carried out step c, A solution and B solution all respectively again note make A1 and B1 solution, to show difference.
Comprise C in view of forming in the water-soluble or aqueous solution of C
6H
5O
7 3-The aqueous solution, so C is Hydrocerol A or solubility Citrate trianion, like Trisodium Citrate, Tripotassium Citrate etc.
As a kind of preferred version, Cu in the production system
2+With C
6H
5O
7 3-Mol ratio be 1:0.01 ~ 0.8, preferred as further, both mol ratios are 1:0.05 ~ 0.4.
D, produce intermediate product: with A1 solution and B1 solution simultaneously, flow in the reaction kettle lentamente, make both that chemical reaction take place, it is 3 ~ 9 that the flow through adjusting A1 solution and B1 solution in the reaction process makes the pH value of reaction kettle for reaction liquid, produces intermediate product;
In step c, we are called complexing agent with the C that introduces, and briefly set forth here: in reaction process, and C
6H
5O
7 3-Serve as the role of complexing agent, detailed process is following: C
6H
5O
7 3-At first with Cu
2+Complex reaction takes place, and generates inner complex [Cu
3(C
6H
5O
7H
3)
4]
2+, then at OH
-Effect generates verditer (Cu (OH) down
2), the Cu of generation (OH)
2At C
6H
5O
7 3-Effect down with solution in copper sulfate (CuSO
4) reaction generation Basic Chrome Sulphate deposition (CuSO
43Cu (OH)
2); After reaction is accomplished, C
6H
5O
7 3-Be left in the reaction solution with ionic species, if there is heavy metal ion (like arsenic, lead) in the reaction solution, will with the heavy metal ion complexing to avoid in the heavy metal ion target approach product.
Generally speaking, reaction principle of the present invention can be expressed as follows:
Therefore, in fact said intermediate product is meant by CuSO among the present invention
43Cu (OH)
2Solidliquid mixture with reaction solution (solution that other soluble substances or ion are formed) composition.
Steps d is the core procedure of preparation Basic Chrome Sulphate, and the selection of reaction conditions and control have remarkable influence to quality, quality and the stability of product.In fact, this step does not have strict requirement, preferred 35 ~ 75 ℃ to temperature of reaction.But to the control of pH value with select most importantly, and adopted a kind of method extremely easily that the pH value is regulated, that is: the pH value of coming reaction solution in the conditioned reaction still of the flow through adjustment A1 solution and B1 solution.Specifically, we know, contain OH in the B1 solution
-If the pH value that we will control reaction solution is 3 ~ 9, in case the pH value that monitors reaction solution less than or will be less than 3, we just through reducing A1 solution or increasing the flow of B1 solution, make the increase of pH value so; And, the pH value is reduced in case the pH value that monitors reaction solution greater than perhaps being greater than 9, then increases A1 solution or reduces the flow of B1 solution.
As a kind of preferred, the pH value of reaction solution is 4 ~ 7.
For convenient, monitor pH value effectively, can monitor the pH value of reaction solution through the pH test paper, certain, in order to be convenient to suitability for industrialized production more, preferably adopt pH electrode that the reaction solution in the reaction kettle is carried out the successive real-time automatic monitoring.
E, the intermediate product that steps d is produced are transferred in the suction filter, wash to washings to be neutral, carry out suction filtration then tentatively to dewater, and produce primary product;
F, the primary product that step e is produced are dried processing, prepare the title product Basic Chrome Sulphate.
Certainly, before oven dry, can also increase a dehydrating step, thereby can dry product quickly, enhance productivity.Bake out temperature and drying time do not have strict restriction, confirm to get final product in conjunction with concrete process condition, and bake out temperature is selected between 30 ~ 180 ℃ usually.
Embodiment 1:
Copper sulfate is dissolved in a reactor drum forms Cu
2+Mass concentration is 2% A solution, and is for use; Sodium hydroxide is dissolved in No. two reactor drums forms OH
-Mass concentration is 5% B solution, and is for use; In A solution, add Hydrocerol A, make Cu
2+With C
6H
5O
7 3-Mol ratio be 1:0.01, after this, A solution and B solution respectively again note make A1 solution and B1 solution; In the reaction kettle of 2L, add 500mL water; Water temperature is 35 ℃, with A1 solution and B1 solution simultaneously, flow in the reaction kettle lentamente, adopt in the reaction process pH electrode in real time in the monitoring reaction still pH value of reaction solution and pH value situation that basis monitors determine whether to adjust the flow of two kinds of solution; Make the pH value of reaction solution be controlled at about 3 and greater than 3; Successive reaction is closed A1 solution and B1 solution after for some time, produces intermediate product; Intermediate product is transferred in the suction filter, and the water washed twice records washings and is neutral, carries out suction filtration and produces primary product tentatively to dewater; Primary product is transferred in the drying treatment device dries processing, make the title product Basic Chrome Sulphate.The mass content that records Basic Chrome Sulphate is 99.24%, and median size is 35 microns.
Embodiment 2:
In a reactor drum, put into a certain amount of acid wiring board bluestone waste, form Cu
2+Mass concentration is 7.6% A solution, and is for use; Pottasium Hydroxide is dissolved in No. two reactor drums forms OH
-Mass concentration is 8% B solution, and is for use; In A solution, add Trisodium Citrate, make Cu
2+With C
6H
5O
7 3-Mol ratio be 1:0.3, after this, A solution and B solution respectively again note make A1 solution and B1 solution; In the reaction kettle of 2L, add 500mL water; Water temperature is 50 ℃, with A1 solution and B1 solution simultaneously, flow in the reaction kettle lentamente, adopt in the reaction process pH electrode in real time in the monitoring reaction still pH value of reaction solution and pH value situation that basis monitors determine whether to adjust the flow of two kinds of solution; The pH value of reaction solution is controlled at about 5; Successive reaction is closed A1 solution and B1 solution after for some time, produces intermediate product; Intermediate product is transferred in the suction filter, and the water washed twice records washings and is neutral, carries out suction filtration and produces primary product tentatively to dewater; Be transferred in the drying treatment device after primary product dewatered and dry processing, make the title product Basic Chrome Sulphate.Heavy metal content in the title product is analyzed, and the lead ion mass concentration is 7.6ppm, and the arsonium ion mass concentration is 5.4ppm, can not constitute influence to the purity of Basic Chrome Sulphate.The mass content that records Basic Chrome Sulphate is 99.08%, and median size is 42 microns.
Embodiment 3:
Copper sulfate is dissolved in a reactor drum forms Cu
2+Mass concentration is 10% A solution, and is for use; Sodium hydroxide is dissolved in No. two reactor drums forms OH
-Mass concentration is 12% B solution, and is for use; In B solution, add Hydrocerol A, make Cu
2+With C
6H
5O
7 3-Mol ratio be 1:0.6, after this, A solution and B solution respectively again note make A1 solution and B1 solution; In the reaction kettle of 2L, add 500mL water; Water temperature is 60 ℃, with A1 solution and B1 solution simultaneously, flow in the reaction kettle lentamente, adopt in the reaction process pH electrode in real time in the monitoring reaction still pH value of reaction solution and pH value situation that basis monitors determine whether to adjust the flow of two kinds of solution; The pH value of reaction solution is controlled at about 7; Successive reaction is closed A1 solution and B1 solution after for some time, produces intermediate product; Intermediate product is transferred in the suction filter, and the water washed twice records washings and is neutral, carries out suction filtration and produces primary product tentatively to dewater; Primary product is transferred in the drying treatment device dries processing, make the title product Basic Chrome Sulphate.The mass content that records Basic Chrome Sulphate is 99.31%, and median size is 28 microns.
Embodiment 4:
In a reactor drum, put into a certain amount of acid wiring board bluestone waste, form Cu
2+Mass concentration is 12% A solution, and is for use; Pottasium Hydroxide is dissolved in No. two reactor drums forms OH
-Mass concentration is 15% B solution, and is for use; In A solution and B solution, all add Trisodium Citrate, make Cu
2+With C
6H
5O
7 3-Total mol ratio be 1:0.8, after this, A solution and B solution respectively again note make A1 solution and B1 solution; In the reaction kettle of 2L, add 500mL water; Water temperature is 75 ℃, with A1 solution and B1 solution simultaneously, flow in the reaction kettle lentamente, adopt in the reaction process pH electrode in real time in the monitoring reaction still pH value of reaction solution and pH value situation that basis monitors determine whether to adjust the flow of two kinds of solution; Make the pH value of reaction solution be controlled at about 9 and less than 9; Successive reaction is closed A1 solution and B1 solution after for some time, produces intermediate product; Intermediate product is transferred in the suction filter, and the water washed twice records washings and is neutral, carries out suction filtration and produces primary product tentatively to dewater; Be transferred in the drying treatment device after primary product dewatered and dry processing, make the title product Basic Chrome Sulphate.Heavy metal content in the title product is analyzed, and the lead ion mass concentration is 6.4ppm, and the mass concentration of arsonium ion is 3.5ppm, can not constitute influence to the purity of Basic Chrome Sulphate.The mass content that records Basic Chrome Sulphate is 99.01%, and median size is 36 microns.
More than show and described ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand, and the foregoing description does not limit the present invention in any form, and all employings are equal to the technical scheme that mode obtained of replacement or equivalent transformation, all drop in protection scope of the present invention.
Claims (10)
1. a kind of industrial production process of Basic Chrome Sulphate is characterized in that, comprises the steps:
A, preparation contain the A solution of sulfate ion and cupric ion, and be for use;
B, preparation contain the B solution of hydroxide ion, and be for use;
C, introducing complexing agent: add complexing agent C at least one in above-mentioned A solution and B solution; Above-mentioned complexing agent C dissolving back forms the solution that comprises citrate ion; After carrying out this step, above-mentioned A solution and B solution respectively again note make A1 solution and B1 solution;
D, simultaneously, flow in the reaction kettle lentamente with A1 solution and B1 solution, chemical reaction takes place in both, and it is 3 ~ 9 that the flow of regulating A1 solution and B1 solution in the reaction process makes the pH value of reaction kettle for reaction liquid, produces intermediate product;
E, intermediate product is transferred in the suction filter, washs to washings and be neutral, and carry out suction filtration, produce primary product tentatively to dewater;
F, primary product is dried processing, prepare the title product Basic Chrome Sulphate.
2. a kind of industrial production process of Basic Chrome Sulphate according to claim 1; It is characterized in that; Above-mentioned A solution is acid wiring board bluestone waste, perhaps is copper-bath, is perhaps made by one or more and sulfuric acid reaction in verditer, ventilation breather, the cupric oxide.
3. a kind of industrial production process of Basic Chrome Sulphate according to claim 1 is characterized in that, above-mentioned B solution is sodium hydroxide and/or potassium hydroxide solution.
4. a kind of industrial production process of Basic Chrome Sulphate according to claim 1 is characterized in that, above-mentioned complexing agent C is Hydrocerol A or solubility Citrate trianion.
5. a kind of industrial production process of Basic Chrome Sulphate according to claim 1 is characterized in that, the mass concentration of cupric ion is 2% ~ 12% in the above-mentioned A solution.
6. a kind of industrial production process of Basic Chrome Sulphate according to claim 1 is characterized in that, the mass concentration of hydroxide ion is 5% ~ 15% in the above-mentioned B solution.
7. a kind of industrial production process of Basic Chrome Sulphate according to claim 1 is characterized in that, the mol ratio of above-mentioned cupric ion and citrate ion is 1:0.01 ~ 0.8.
8. a kind of industrial production process of Basic Chrome Sulphate according to claim 1 is characterized in that, temperature of reaction is 35 ~ 75 ℃ among the above-mentioned steps d.
9. a kind of industrial production process of Basic Chrome Sulphate according to claim 1 is characterized in that, adopts pH electrode that the pH value of reaction kettle for reaction liquid is monitored among the above-mentioned steps d.
10. according to a kind of industrial production process of each described Basic Chrome Sulphate of claim 1 ~ 9, it is characterized in that the pH value of reaction solution is 4 ~ 7 among the above-mentioned steps d.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043769A (en) * | 2012-12-07 | 2013-04-17 | 常州大学 | Compound agent for removing lead from waste water |
| CN103145172A (en) * | 2013-04-03 | 2013-06-12 | 北京科技大学 | Method for preparing yolk/shell structured basic copper sulfate |
| CN106430282A (en) * | 2016-11-28 | 2017-02-22 | 青岛科技大学 | Preparation method of basic copper sulfate |
| CN107151028A (en) * | 2017-06-07 | 2017-09-12 | 江门市东江环保技术有限公司 | A kind of method that utilization alkaline etching liquid produces basic copper sulfate |
| CN107324373A (en) * | 2017-07-18 | 2017-11-07 | 清华大学 | The method of purification of malachite pigment |
| FR3092727A1 (en) * | 2019-02-19 | 2020-08-21 | Upl Limited | Process for preparing copper compounds |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043769A (en) * | 2012-12-07 | 2013-04-17 | 常州大学 | Compound agent for removing lead from waste water |
| CN103145172A (en) * | 2013-04-03 | 2013-06-12 | 北京科技大学 | Method for preparing yolk/shell structured basic copper sulfate |
| CN103145172B (en) * | 2013-04-03 | 2014-06-18 | 北京科技大学 | Method for preparing yolk/shell structured basic copper sulfate |
| CN106430282A (en) * | 2016-11-28 | 2017-02-22 | 青岛科技大学 | Preparation method of basic copper sulfate |
| CN106430282B (en) * | 2016-11-28 | 2018-05-25 | 青岛科技大学 | A kind of preparation method of basic copper sulfate |
| CN107151028A (en) * | 2017-06-07 | 2017-09-12 | 江门市东江环保技术有限公司 | A kind of method that utilization alkaline etching liquid produces basic copper sulfate |
| CN107324373A (en) * | 2017-07-18 | 2017-11-07 | 清华大学 | The method of purification of malachite pigment |
| CN107324373B (en) * | 2017-07-18 | 2019-05-28 | 清华大学 | The method of purification of malachite pigment |
| FR3092727A1 (en) * | 2019-02-19 | 2020-08-21 | Upl Limited | Process for preparing copper compounds |
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|---|---|
| CN102602980B (en) | 2014-05-28 |
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Effective date of registration: 20160427 Address after: 01, room 5, building 369, 215129 deer Road, hi tech Zone, Jiangsu, Suzhou Patentee after: Suzhou Long Lake nano science and Technology Co Ltd Address before: 215129 Jiangsu province Suzhou city road high tech Zone deer No. 369 Industrial Park No. 21 501-505 Patentee before: Liao Yongzhi |