CN115611302A - Preparation process of nano basic copper carbonate and nano basic copper carbonate - Google Patents

Preparation process of nano basic copper carbonate and nano basic copper carbonate Download PDF

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CN115611302A
CN115611302A CN202211297658.4A CN202211297658A CN115611302A CN 115611302 A CN115611302 A CN 115611302A CN 202211297658 A CN202211297658 A CN 202211297658A CN 115611302 A CN115611302 A CN 115611302A
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copper carbonate
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胡志程
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Hangzhou Fuyang Hongyuan Renewable Resources Utilization Co ltd
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    • C01G3/00—Compounds of copper
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    • C—CHEMISTRY; METALLURGY
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    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract

The application relates to the technical field of preparation of inorganic metal compound materials, and particularly discloses a preparation process of nano basic copper carbonate and the nano basic copper carbonate. A preparation process of nanometer basic copper carbonate comprises the following steps: preparing a sodium carbonate solution, preparing an additive solution, carrying out a precipitation reaction, filtering and drying, wherein the precipitation reaction comprises the following steps: dripping sodium carbonate solution and additive solution into the acidic etching solution at the same time at the temperature of 25-35 ℃ for precipitation reaction, wherein the pH value of the reaction end point is 5.5-9.5; the quality of the acid etching solution is Cu 2+ The mass ratio of the acid etching solution to the sodium carbonate is (0.45-1.35) to 1; the mass ratio of the acidic etching solution to the additive is 1: (5.5-16.5). The preparation process of the nanometer alkaline copper carbonate effectively utilizes the etching waste liquid, is simple in generation process, and is high in purity and small in particle size.

Description

Preparation process of nano basic copper carbonate and nano basic copper carbonate
Technical Field
The application relates to the technical field of preparation of inorganic metal compound materials, in particular to a preparation process of nano basic copper carbonate and the nano basic copper carbonate.
Background
The basic copper carbonate has wide application, and can be used for manufacturing signal bombs, fireworks, paints, bactericides, wood preservatives, feed additives and the like. After the superfine copper carbonate is superfine, the application performance of the basic copper carbonate can be greatly improved, and the nano materials with different particle sizes have different optical, electric and magnetic effects.
At present, the commonly used preparation methods of basic copper carbonate comprise an ammonia method, a copper nitrate method and a copper sulfate method, the copper sulfate method is mostly researched at home and abroad, but the production cost is higher. In recent years, some people produce alkaline copper carbonate by using acidic etching solution waste liquid, and can effectively recycle the acidic etching solution waste liquid. The process for producing the alkaline copper carbonate by using the acidic etching solution waste liquid generally comprises the following steps: firstly, copper oxide is prepared from copper-containing etching waste liquid, and then basic copper carbonate is prepared through the working procedures of dissolving copper in ammonia carbon solution, evaporating ammonia, depositing copper and the like.
In view of the above-mentioned related technologies, the applicant believes that the process of ammonia distillation and copper deposition consumes much energy, and the whole synthesis process needs to be carried out in three steps, which is cumbersome.
Disclosure of Invention
In order to simplify the production steps and improve the product quality, the application provides a preparation process of nano basic copper carbonate and the nano basic copper carbonate.
In a first aspect, the application provides a preparation process of nano basic copper carbonate, which adopts the following technical scheme:
a preparation process of nanometer basic copper carbonate comprises the following steps: preparing sodium carbonate solution, preparing additive solution, precipitating, filtering, drying,
the precipitation reaction is as follows: simultaneously dripping a sodium carbonate solution and an additive solution into the acidic etching solution at the temperature of between 25 and 35 ℃ to perform precipitation reaction, wherein the pH value of the reaction end point is between 5.5 and 9.5;
the quality of the acid etching solution is Cu 2+ The mass ratio of the acid etching solution to the sodium carbonate is (0.45-1.35) to 1; the mass ratio of the acidic etching solution to the additive is 1: (5.5-16.5).
By adopting the technical scheme, the acidic etching solution is acidic copper chloride etching waste liquid which contains a large amount of copper ions and chloride ions, a sodium carbonate solution and an additive are simultaneously added into the acidic etching solution, and the sodium carbonate and the copper ions are subjected to precipitation reaction to generate copper carbonate; the additive can disperse and shape the generated copper carbonate particles, and the additive is added along with the sodium carbonate, so that the copper carbonate can be dispersed and shaped just before the copper carbonate is generated, the copper carbonate generated in advance can not influence the copper carbonate generated in the following, the agglomeration among the copper carbonate particles is reduced, and the quality of the generated alkaline copper carbonate is improved. The preparation process is simple and easy to operate, and the generated alkaline copper carbonate has high quality.
Preferably, the mass ratio of the acidic etching solution to the additive is 1: (9-13).
By adopting the technical scheme, the proportion of the additive to the acidic etching solution is further optimized, the dispersing and shaping effects of the additive on the generated basic copper carbonate particles are improved, and the quality of the generated basic copper carbonate is further improved.
Preferably, the additive is one or more of sodium dodecyl sulfate and polyvinylpyrrolidone.
By adopting the technical scheme, the sodium dodecyl sulfate is an anionic surfactant, can be matched with sodium carbonate, can influence the balance of van der Waals force and electrostatic repulsion force among particles, and prevents the particles from growing and enlarging; the polyvinyl pyrrolidone as a high molecular surfactant can be used as a dispersant, a granularity regulator, an anti-redeposition agent and a cosolvent in different dispersion systems, fully plays the dispersing and sizing roles and improves the quality of the generated basic copper carbonate.
Preferably, the additive comprises the following components in a mass ratio of (2-3): 1 sodium dodecyl sulfate and polyvinylpyrrolidone.
The concentration of hydrogen ions in the acidic copper chloride etching solution is high, when the acidic copper chloride etching solution reacts with a sodium carbonate alkali solution, the pH value of the solution is reduced quickly, the alkalinity of sodium carbonate is too strong, hydroxide radicals are too much left after the reaction is finished, and copper hydroxide generated by the reaction of copper ions and hydroxide radicals is easily decomposed into copper oxide, so that the preparation of basic copper carbonate is not facilitated. By adopting the technical scheme, the sodium dodecyl sulfate is alkaline in water, can reduce initial p H of reaction after being mixed with sodium carbonate, can also enable p H in the reaction process to change slowly, keeps p H value in the p H range of saturated basic copper carbonate solution in the reaction process, and is beneficial to the formation of basic copper carbonate sediment. Within the range of the mixture ratio of the sodium dodecyl sulfate to the polyvinylpyrrolidone defined by the application, the purity of the generated basic copper carbonate is higher.
Preferably, the polyvinylpyrrolidone has an average molecular weight of 45000-58000.
Preferably, the mass percentage concentration of the sodium carbonate solution is 5-20%.
Preferably, the acidic etching solution is diluted by water by a factor of 2-3.
By adopting the technical scheme, the acidic etching solution is diluted, the content of chloride ions in the generated product can be reduced, but the dilution times are too high, the content of the chloride ions can be increased instead, the dilution times are limited to be 2-3 times, and the alkaline copper carbonate product with higher purity can be obtained. In addition, the particle size of the basic copper carbonate increases with the concentration of the reactant, and the basic copper carbonate product with smaller particle size can be obtained after dilution.
Preferably, the acidic etching solution is diluted by a mixed solution of water and ethanol, and the mass ratio of the water to the ethanol is (5-7): 1.
by adopting the technical scheme, when ethanol is not added and water is used as a solvent, particles generated by hydrolysis easily grow and agglomerate, and the particles become large. When ethanol is added as a solvent, copper chloride in the etching solution is dissolved in absolute ethanol in a molecular form, and when hydrolysis reaction occurs, ethanol exists on the surface of the generated particles, so that the surface tension of the particles is small, and the particles are not easy to agglomerate and grow. In addition, the surfactant can be adsorbed on the surface of the particles to form steric hindrance, so that a good dispersing effect is achieved, and the agglomeration of the particles is hindered.
In a second aspect, the present application provides a nano basic copper carbonate prepared by any one of the above-described preparation processes of nano basic copper carbonate.
In summary, the present application has the following beneficial effects:
1. according to the method, the sodium carbonate solution and the additive are added into the acidic etching solution at the same time, the sodium carbonate and the copper ions are subjected to precipitation reaction to generate the nano-alkaline copper carbonate, the production process is simple, the operation is easy, and the obtained Cu of the nano-alkaline copper carbonate 2+ The mass percentage content can reach 55.52-56.25 percent, and Cl - The mass percentage content can reach 0.001-0.0005%, the product is in a regular microspherical shape, and the grain diameter can reach 2.0-3.5 mu m.
Drawings
FIG. 1 is a scanning electron micrograph of basic copper carbonate obtained in example 1 at a resolution of 200 nm;
FIG. 2 is a scanning electron micrograph of basic copper carbonate obtained in example 1 at a resolution of 500 nm;
FIG. 3 is a scanning electron micrograph of basic copper carbonate obtained in example 1 at a resolution of 2 μm;
FIG. 4 is a scanning electron micrograph of basic copper carbonate obtained in example 1 at a resolution of 5 μm;
figure 5 is an XRD pattern of basic copper carbonate obtained in example 1.
Detailed Description
The present application will be described in further detail with reference to examples.
Raw materials
The raw materials of the embodiment of the application can be obtained by market:
acid etching solution: density 1.30 g/mL; cu 2+ Mass concentration 118.6 g/L, H + Concentration 1.88 mol/L, cl - The mass concentration is 274.74 g/L.
Examples
Example 1
A preparation process of nano basic copper carbonate comprises the following steps:
s1, preparing sodium carbonate solution
Adding 1kg of sodium carbonate solid into 19kg of water, stirring and dissolving to prepare a sodium carbonate solution with the mass percentage concentration of 5% for later use;
s2, preparing additive solution
Adding 900kg of polyvinylpyrrolidone into 3kg of water, performing ultrasonic dispersion at 25 ℃ for 30min, cooling to room temperature, adding 7kg of water to prepare a polyvinylpyrrolidone aqueous solution with the concentration of 2mol/L, shaking up, and standing for 30min for later use;
s3, precipitation reaction
Simultaneously dropwise adding the sodium carbonate solution obtained by 20kgS and the additive solution obtained by S2 into 5kg of acidic etching solution at 30 ℃ to perform precipitation reaction, wherein the reaction end point is a PH value of 5.5, so as to obtain a mixed solution; the mass of the acidic etching solution is Cu 2+ The mass ratio of the acidic etching solution to the sodium carbonate is 0.45; the mass ratio of the acidic etching solution to the additive is 1:5.5;
s4, filtering
Filtering the mixed solution obtained in the step S3, and reserving solid substances;
s5, drying
And (4) drying the solid substance obtained in the step (S4) at the temperature of 80 ℃ to obtain the nano basic copper carbonate.
Example 2
Different from the embodiment 1, in the step S3 in the embodiment 2, the sodium carbonate solution obtained from 20kgS and the additive solution obtained from S2 are simultaneously added dropwise into 11kg of the acidic etching solution, so as to perform a precipitation reaction, wherein the reaction end point is PH 5.5, and a mixed solution is obtained; the mass of the acidic etching solution is Cu 2+ The mass ratio of the acid etching solution to the sodium carbonate is 1.1; the mass ratio of the acidic etching solution to the additive is 1:5.5.
example 3
Different from the embodiment 1, in the step S3 in the embodiment 2, the sodium carbonate solution obtained from 20kgS and the additive solution obtained from S2 are simultaneously added dropwise into 15kg of the acidic etching solution for precipitation reaction, and the reaction end point is PH 5.5 to obtain a mixed solution; the mass of the acidic etching solution is Cu 2+ The mass ratio of the acidic etching solution to the sodium carbonate is 1.35; the mass ratio of the acidic etching solution to the additive is 1:5.5.
example 4
Different from the embodiment 1, in the step S3 in the embodiment 4, the sodium carbonate solution obtained from 20kgS and the additive solution obtained from S2 are simultaneously added dropwise into 11kg of the acidic etching solution, so as to perform a precipitation reaction, wherein the reaction end point is PH 5.5, and a mixed solution is obtained; the mass of the acidic etching solution is Cu 2+ The mass ratio of the acid etching solution to the sodium carbonate is 1:1; the mass ratio of the acidic etching solution to the additive is 1:9.
example 5
Different from the embodiment 1, in the step S3 in the embodiment 5, the sodium carbonate solution obtained from 20kgS and the additive solution obtained from S2 are simultaneously added dropwise into 11kg of the acidic etching solution, so as to perform a precipitation reaction, wherein the reaction end point is PH 5.5, and a mixed solution is obtained; the mass of the acidic etching solution is Cu 2+ Mass meter, acidThe mass ratio of the etching solution to the sodium carbonate is 1:1; the mass ratio of the acidic etching solution to the additive is 1:11.
example 6
Different from the embodiment 1, in the step S3 in the embodiment 6, the sodium carbonate solution obtained from 20kgS and 13.1kg of the additive solution obtained from S2 are simultaneously added dropwise into 11kg of the acidic etching solution, so as to perform a precipitation reaction, wherein the reaction end point is PH 5.5, so as to obtain a mixed solution; the mass of the acidic etching solution is Cu 2+ The mass ratio of the acid etching solution to the sodium carbonate is 1:1; the mass ratio of the acidic etching solution to the additive is 1:13.
example 7
Different from the embodiment 1, in the step S3 in the embodiment 7, the sodium carbonate solution obtained from 20kgS and the additive solution obtained from S2 are simultaneously added dropwise into 11kg of the acidic etching solution, so as to perform a precipitation reaction, wherein the reaction end point is PH 5.5, and a mixed solution is obtained; the mass of the acidic etching solution is Cu 2+ The mass ratio of the acid etching solution to the sodium carbonate is 1:1; the mass ratio of the acidic etching solution to the additive is 1:16.5.
example 8
Unlike example 5, the end point of the reaction in example 8 was pH 7.
Example 9
Unlike example 5, the reaction end point in example 9 was at a pH of 9.5.
Example 10
Different from the embodiment 8, in the S2 in the embodiment 10, 5.44kg of sodium dodecyl sulfate is dissolved in 10kg of water to prepare a sodium dodecyl sulfate water solution with the concentration of 2mol/L, shaken up and kept stand for 30min for standby;
the amount of additive solution added in S3 was 31kg.
Example 11
Unlike example 10, the additive solution in S3 in example 11 comprised 21.1kg of a 2mol/L solution of sodium dodecylsulfonate and 3.6kg of a 2mol/L solution of polyvinylpyrrolidone, the mass ratio of sodium dialkylsulfonate to polyvinylpyrrolidone being 2:1.
Example 12
Unlike example 10, the additive solution in S3 in example 12 comprised 23.6kg of a 2mol/L solution of sodium dodecyl sulfonate and 2.8kg of a 2mol/L solution of polyvinylpyrrolidone, with the mass ratio of sodium dialkyl sulfonate to polyvinylpyrrolidone being 3:1.
Example 13
Unlike example 10, the additive solution in S3 in example 13 comprised 15.7kg of a 2mol/L solution of sodium dodecyl sulfonate and 5.6kg of a 2mol/L solution of polyvinylpyrrolidone, the mass ratio of sodium dialkyl sulfonate to polyvinylpyrrolidone being 1:1.
Example 14
Different from the embodiment 12, in the embodiment 14, 1kg of sodium carbonate solid is added into 4kg of water in the S1, stirred and dissolved, and prepared into a sodium carbonate solution with the mass percentage concentration of 20% for standby;
the amount of the sodium carbonate solution used in S3 was 5kg.
Examples 15 to 17
In examples 15 to 17, the acidic etching solution was diluted with water in a dilution ratio of 2 times, 3 times, and 4 times, respectively, unlike in example 12.
Example 18
Different from example 16, in example 18, the mixture of water and ethanol with the mass ratio of 6:1 was used for dilution.
Comparative example
Comparative example 1
Different from the embodiment 1, the mass ratio of the acid etching solution to the sodium carbonate in the embodiment 1 is 2:1.
Comparative example 2
Different from the example 1, the mass ratio of the acidic etching solution to the sodium carbonate in the comparative example 2 is 0.2.
Comparative example 3
Different from the embodiment 1, the mass ratio of the acid etching solution to the sodium carbonate in the comparative example 3 is 1:3.
Comparative example 4
Different from the example 1, the mass ratio of the acidic etching solution to the sodium carbonate in the comparative example 4 is 1.
Performance test
Detection method/test method
The following property tests were performed on the nano basic copper carbonate prepared in examples 1 to 18 and comparative examples 1 to 4:
for the basic copper carbonates in examples 1-18 and comparative examples 1-4, the copper content of the product is determined by an indirect iodometry method according to industrial basic copper carbonate HG/T4825-2015, and the chlorine content of the product is analyzed by a visual turbidimetry method; the morphology of the product was analyzed by SEM and the phase composition was analyzed by XRD and recorded, the results are shown in table 1 and figures 1-5.
As can be seen from fig. 1 to 4, the basic copper carbonate product prepared in example 1 is small-particle basic copper carbonate, has an irregular spherical shape and is dispersed locally and uniformly; in addition, many small particles are tightly agglomerated to form large particles with irregular shapes of Jiang Kuaizhuang, and the gaps formed by the agglomeration among the particles are easy to be mixed with chloride ions, which is one of the possible reasons for not completely removing the chloride ions in the product.
As can be seen from fig. 5, the diffraction peak of the basic copper carbonate product obtained in example 1 is consistent with the PDF standard card of basic copper carbonate (JCPDS-41-1390), which indicates that there is no impurity peak other than the diffraction peak of basic copper carbonate, indicating that the basic copper carbonate product obtained in the present application has high purity.
TABLE 1 Performance test results
Figure RE-5317DEST_PATH_IMAGE001
It can be seen by combining examples 1-18 and comparative examples 1-4 and table 1 that the nano basic copper carbonate products prepared in examples 1-18 meet the requirements of industrial basic copper carbonate HG/T4825-2015, and the copper content of the nano basic copper carbonate prepared in examples 1-18 is higher than that of comparative examples 1-4, the chlorine content is lower than that of comparative examples 1-4, and the particle size of the product is also lower than that of comparative examples 1-4, which indicates that the nano basic copper carbonate prepared by the preparation process of the application has higher purity, smaller particle size and better overall quality.
By combining examples 1-7 with comparative examples 1-4 and table 1, it can be seen that the ratio of sodium carbonate to the etching solution and the ratio of the additive to the etching solution can affect the quality of the nano alkaline copper carbonate, and the nano alkaline copper carbonate prepared by the method has high purity and fine particle size in the ratio of sodium carbonate to the etching solution and the ratio of the additive to the etching solution defined in the application; this is probably because, within the limits defined in the present application, the additives can sufficiently disperse and shape the resulting copper carbonate particles, reduce agglomeration among the copper carbonate particles, and improve the quality of the resulting basic copper carbonate.
In combination with examples 10-14 and table 1, it can be seen that the copper content of the nano basic copper carbonate prepared in examples 11-14 is higher than that of example 10, the chlorine content is lower than that of example 10, and the particle size of the product is substantially the same, which indicates that the purity of the nano copper carbonate prepared by using the sodium dodecyl sulfate solution compounded with polyvinylpyrrolidone as an additive is higher, and the effect is better within the range of the ratio of the sodium dodecyl sulfate solution to the polyvinylpyrrolidone defined in the present application, probably because the sodium dodecyl sulfate affects the balance between van der waals force and electrostatic repulsion force between particles, preventing the particles from growing larger; the polyvinyl pyrrolidone as a high molecular surfactant can be used as a dispersant, a granularity regulator, an anti-redeposition agent and a cosolvent in different dispersion systems, is matched with sodium dodecyl sulfate, fully plays the dispersing and shaping functions of the polyvinyl pyrrolidone, and improves the quality of the generated alkaline copper carbonate. The sodium dodecyl sulfate and sodium carbonate can reduce initial p H of reaction, and can also make p H change slowly in the reaction process, and can keep p H value in the range of p H of saturated basic copper carbonate solution in the reaction process, so that it is favourable for forming basic copper carbonate precipitate.
By combining the example 12 with the examples 15 to 18 and combining the table 1, it can be seen that the copper content of the nano basic copper carbonate prepared in the examples 15 to 18 is higher than that of the example 12, the chlorine content is lower than that of the example 12, and the particle size of the product is also lower than that of the example 12, which shows that the purity of the nano basic copper carbonate product can be improved and the particle size of the product can be refined by diluting the etching solution and then reacting with sodium carbonate; wherein, the effect is better when the ethanol and water are used for compounding and mixing liquid for dilution. This is probably because when ethanol is added as a solvent, copper chloride in the etching solution is dissolved in absolute ethanol in a molecular form, and when a hydrolysis reaction occurs, the surface of the generated particles has ethanol, the surface tension thereof is small, and the particles are not easy to aggregate and grow. In addition, the surfactant can be adsorbed on the surface of the particles to form steric hindrance, so that a good dispersing effect is achieved, and the agglomeration of the particles is hindered.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.

Claims (9)

1. A preparation process of nanometer basic copper carbonate comprises the following steps: sodium carbonate solution preparation, additive solution preparation, precipitation reaction, filtration and drying, which is characterized in that,
the precipitation reaction is as follows: dripping sodium carbonate solution and additive solution into the acidic etching solution at the same time at the temperature of 25-35 ℃ for precipitation reaction, wherein the pH value of the reaction end point is 5.5-9.5;
the quality of the acid etching solution is Cu 2+ The mass ratio of the acid etching solution to the sodium carbonate is (0.45-1.35): 1; the mass ratio of the acidic etching solution to the additive is 1: (5.5-16.5).
2. The process of claim 1, wherein the nano basic copper carbonate is prepared by the following steps: the mass ratio of the acidic etching solution to the additive is 1: (9-13).
3. The process of claim 1, wherein the nano basic copper carbonate is prepared by the following steps: the additive is one or more of sodium dodecyl sulfate and polyvinylpyrrolidone.
4. The process of claim 3, wherein the step of preparing the nano basic copper carbonate comprises the following steps: the additive comprises sodium dodecyl sulfate and polyvinylpyrrolidone in a mass ratio of (2-3) to 1.
5. The process of claim 3, wherein the step of preparing the nano basic copper carbonate comprises the following steps: the average molecular weight of the polyvinylpyrrolidone is 45000-58000.
6. The process of claim 1, wherein the nano basic copper carbonate is prepared by the following steps: the mass percentage concentration of the sodium carbonate solution is 5-20%.
7. The process of claim 1, wherein the nano basic copper carbonate is prepared by the following steps: and diluting the acidic etching solution by using water, wherein the dilution times are 2-3 times.
8. The process of claim 7, wherein the step of preparing the nano basic copper carbonate comprises the following steps: diluting the acidic etching solution by using a mixed solution of water and ethanol, wherein the mass ratio of the water to the ethanol is (5-7): 1.
9. a nano basic copper carbonate produced by the process for producing nano basic copper carbonate according to any one of claims 1 to 8.
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CN109455753A (en) * 2018-10-26 2019-03-12 深圳骏泽环保有限公司 Etching solution recycles technique
CN111333099A (en) * 2020-03-06 2020-06-26 合肥工业大学 Method for preparing nano copper hydroxide from acidic copper chloride etching waste liquid

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