Copper powder purification and iron removal control method based on multi-parameter monitoring

Abstract

The invention provides a copper powder purification and iron removal control method based on multi-parameter monitoring, and belongs to the technical field of copper powder processing. The method comprises the following steps that basic information of copper powder to be treated is obtained, and the theoretical dosage Qall of acid liquor is calculated; stirring and mixing the copper powder and pure water; setting a preset batch number n of adding the acid liquor in batches, generating an addition amount Q1 of adding the acid liquor in the first batch and an addition amount Q2 of adding the acid liquor in the second batch, and setting the interval time as t1; monitoring parameters of the mixed system are obtained, and the adding process of the acid liquor in the next batch is dynamically adjusted; and repeating until the concentration of the iron ions in the mixed system tends to be constant, thereby completing iron purification and impurity removal. Accurate iron removal through an acid leaching method can be achieved, the corrosion loss of the copper powder is reduced, and the purity and yield of the copper powder are improved; meanwhile, the addition amount of the acid liquor is accurately controlled, and the subsequent wastewater treatment cost is reduced.

Description

Technical Field

[0001] This invention relates to the field of copper powder processing technology, and in particular to a copper powder purification and iron removal control method based on multi-parameter monitoring. Background Technology

[0002] Copper powder is a crucial raw material in the production of copper-based rare earth nanocomposite catalysts. However, iron filings or powder may be present during the production process and need to be removed. A Chinese utility model patent (title: "Purification Device for Copper Powder Catalyst," announcement number: CN202290300U, announcement date: 20120704) discloses an effective method to reduce the iron impurity content in copper powder products through the adsorption of iron using a magnetic rack. To ensure the purification effect of the copper powder, the industry still requires a combination of acid leaching and magnetic separation.

[0003] However, when using acid leaching to purify and remove iron from copper powder, improper control can lead to corrosion of the copper powder by the acid, affecting the final yield. Summary of the Invention

[0004] This invention aims to provide a copper powder purification and iron removal control method based on multi-parameter monitoring, which can achieve precise iron removal by acid leaching and improve the purity of copper powder. At the same time, acid solution is added in batches and the amount of acid solution added in each batch is dynamically controlled to prevent excessive acid solution from inducing local violent reactions and causing copper powder corrosion loss, thereby improving the yield. It also allows for precise control of the amount of acid solution added, reducing the cost of subsequent wastewater treatment.

[0005] The technical solution adopted in this invention is:

[0006] A method for controlling the purification and iron removal of copper powder based on multi-parameter monitoring includes the following steps:

[0007] Step S1: Obtain basic information about the copper powder to be processed; simultaneously, calculate the theoretical amount Q of acid solution with a planned molar concentration M based on the basic information. all The basic information includes the weight W of the copper powder and the iron content C in the copper powder. Fe ;

[0008] Step S2: Mix the copper powder with pure water according to a preset solid-liquid ratio;

[0009] Step S3: Set the preset batch number n for adding the acid solution in batches; based on the theoretical dosage Q. all Given the preset batch number n, generate the amount Q1 of the first batch of acid solution added and the amount Q2 of the second batch of acid solution added, and set the interval between the first batch of acid solution added and the second batch of acid solution added as Δt1.

[0010] Step S4: Obtain the monitoring parameters of the mixing system before and after the addition of the acid solution, and compare them with the subsequent batch addition process of the acid solution after dynamic adjustment based on the monitoring parameters;

[0011] Step S5: Repeat step S4 until the concentration of iron ions in the mixed system tends to be constant, then stop adding the acid solution to complete the iron purification and impurity removal.

[0012] Further, the acid solution is acetic acid, 0.1~2 mol / L dilute hydrochloric acid, or 0.1~4 mol / L dilute sulfuric acid.

[0013] Furthermore, the solid-liquid ratio is 1:(20~50).

[0014] Furthermore, the solid-liquid ratio is 1:(30~40).

[0015] Furthermore, the stirring speed during the mixing process in step S2 is 200~500 r / min.

[0016] Furthermore, the preset batch number n ≥ 10.

[0017] Furthermore, 30 ≤ n ≤ 50.

[0018] Furthermore, the amount Q1 of the first batch of acid added and the amount Q2 of the second batch of acid added in step S3 are obtained using the following formula:

[0019] ;

[0020] ;

[0021] In the formula, Q1 is the amount of acid solution added in the first batch;

[0022] Q2 is the amount of acid solution added in the second batch;

[0023] n is the preset batch number;

[0024] k1 is a correction coefficient for the amount of acid added in the first batch, with a value ranging from 0.5 to 0.7;

[0025] k2 is a correction factor for the amount of acid added in the second addition, with a value ranging from 0.6 to 0.8.

[0026] Furthermore, in step S4, the amount Q of the acid solution added in the jth batch is... j The time interval Δt between batch j-1 and batch j j-1 The following formula is used to derive:

[0027] ;

[0028] ;

[0029] In the formula, Q1 is the amount of acid solution added in the first batch;

[0030] Q2 is the amount of acid solution added in the second batch;

[0031] Q j Let j be the amount of acid solution added in the j-th batch; where j ≥ 3;

[0032] k j The correction factor for the amount of acid added in the j-th batch is 0.5 to 1.2.

[0033] △t j-1 The time interval between batch j-1 and batch j;

[0034] L is a correction value for the preset batch number n related to the changes in the monitoring parameters after the first and second batches of acid are added, and the value is an integer from 0 to 25;

[0035] S j-1 This is a correction factor for the time interval between batch j-1 and batch j, with a value ranging from 0.5 to 1.5.

[0036] Furthermore, during each batch of adding the acid solution to the mixture, an inert gas is simultaneously introduced into the bottom of the mixture.

[0037] The beneficial effects of this invention are:

[0038] The copper powder purification and iron removal control method based on multi-parameter monitoring in this invention can achieve precise iron removal by acid leaching, thereby improving the purity of copper powder. At the same time, the acid solution is added in batches and the amount of acid solution added in each batch is dynamically controlled to prevent excessive acid solution from inducing local violent reactions and causing copper powder corrosion loss, thereby improving the yield. The precise control of the amount of acid solution added also reduces the cost of subsequent wastewater treatment. Attached Figure Description

[0039] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0040] Figure 1 This is a schematic flowchart of the copper powder purification and iron removal control method based on multi-parameter monitoring in the embodiment.

[0041] Figure 2 Example of iron ion concentration versus time curve. Detailed Implementation

[0042] The following disclosure provides many different embodiments or examples for implementing different structures of the present invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, these are merely examples and are not intended to limit the present invention.

[0043] The embodiments of the invention will now be described in detail with reference to the accompanying drawings.

[0044] This embodiment provides a copper powder purification and iron removal control method based on multi-parameter monitoring, the process of which is as follows: Figure 1 As shown in the figure. The method includes the following steps:

[0045] Step S1: Obtain basic information about the copper powder to be processed; simultaneously, calculate the theoretical amount Q of acid solution with a planned molar concentration M based on the basic information. all .

[0046] Specifically, the basic information includes the weight W of the copper powder and the iron content C in the copper powder. Fe The weight W of the copper powder can be obtained through conventional weighing methods; the iron content C in the copper powder... Fe The information can be obtained using common measurement methods such as atomic absorption spectrometry (AAS) and inductively coupled plasma optical emission spectrometry (ICP-OES). Other detection methods for obtaining basic information that are not described in this embodiment but are already publicly available can also be used in this embodiment, and will not be elaborated further. The acid solution planned to be used in this embodiment can be acetic acid, 0.1~2 mol / L dilute hydrochloric acid, or 0.1~4 mol / L dilute sulfuric acid. At room temperature, acetic acid, dilute hydrochloric acid, and dilute sulfuric acid can react smoothly with iron but not with copper, thereby achieving purification and iron removal, and improving the purity of the copper powder. Furthermore, acetic acid is a weak acid, and the molar concentrations of dilute hydrochloric acid and dilute sulfuric acid are relatively low, which helps to reduce copper powder corrosion loss. The theoretical amount of acid solution Q used in this embodiment is... all The following formula can be used to derive it:

[0047] ;

[0048] or, ;

[0049] In the formula, Q all This represents the theoretical volume of acid solution used, expressed in liters (L).

[0050] W represents the weight of the copper powder, in grams.

[0051] C Fe Iron content in copper powder, in wt%;

[0052] M is the molar concentration of the acid solution, in mol / L.

[0053] Step S2: Mix copper powder and pure water according to a preset solid-liquid ratio.

[0054] In this embodiment, copper powder and pure water are mixed at a preset solid-liquid ratio to keep the copper powder in suspension. This facilitates the contact, dissolution, and release of iron impurities by the subsequently added acid. Simultaneously, the added pure water dilutes the acid, preventing excessively high local acid concentrations that could induce copper powder corrosion and loss. Specifically, the solid-liquid ratio of copper powder to pure water can be arbitrary, but 1:(20~50) is preferred, and more preferably 1:(30~40). A suitable solid-liquid ratio helps maintain good suspension of the copper powder, thus facilitating the dissolution and release of iron impurities without significantly increasing subsequent wastewater treatment costs. In this embodiment, the stirring speed is set to 200~500 r / min, suitable for keeping the copper powder in suspension at most solid-liquid ratios.

[0055] Step S3: Preset the preset number of batches n for adding acid solution in batches; based on the theoretical dosage Q. all Given a preset batch number n, generate the amount of acid added in the first batch Q1 and the amount of acid added in the second batch Q. 2， The interval △t1 between the first batch of acid addition and the second batch of acid addition is set.

[0056] In this embodiment, the batch addition of acid can be implemented using common control methods such as peristaltic pumps, solenoid valves, and electromagnetic flowmeters. Other publicly available technologies for batch-controlled addition, not described in this embodiment, can also be used and will not be detailed here. In this embodiment, the preset batch number n is any integer greater than or equal to 1, preferably n ≥ 10, and more preferably 30 ≤ n ≤ 50. In this embodiment, the size of the preset batch number n is related to the calculation of the amount of acid added in subsequent batches; if the preset batch number n is small, the amount of acid added in each batch may be high, especially the amount Q1 of the first batch and the amount Q2 of the second batch, which is not conducive to the monitoring of purification and iron removal after the initial acid addition, and the dynamic adjustment of the subsequent acid addition process based on the initial monitoring results. It may even lead to the risk of copper powder corrosion loss due to excessive instantaneous acid volume. In this embodiment, given that subsequent adjustments are needed based on monitoring parameters after the first and second batches of acid addition, the amounts Q1 and Q2 of the first and second batches of acid addition can be obtained using the following formula:

[0057] ;

[0058] ;

[0059] In the formula, Q1 is the amount of acid solution added in the first batch, in L;

[0060] Q2 represents the amount of acid solution added in the second batch, in liters (L).

[0061] n is the preset batch number;

[0062] k1 is a correction factor for the amount of acid added in the first batch, with a value ranging from 0.5 to 0.7;

[0063] k2 is a correction factor for the amount of acid added in the second addition, with a value ranging from 0.6 to 0.8.

[0064] In this embodiment, the iron removal process of the designed mixing system is initially verified by controlling the amount of acid added in the first and second batches, providing necessary reference for subsequent dynamic adjustments.

[0065] Step S4: Obtain the monitoring parameters of the mixing system before and after the addition of acid, and compare them with the subsequent batch addition process after dynamic adjustment based on the monitoring parameters.

[0066] In this embodiment, the monitoring parameters of the mixed system include temperature and its temperature-time trend, pH value and its pH-time trend, iron ion concentration and its iron ion concentration-time trend, and copper ion concentration and its copper ion concentration-time trend. These monitoring parameters can be specifically displayed in real time using visual charts, such as... Figure 2 The iron ion concentration-time change curve shown provides a more intuitive view of the iron purification and impurity removal process and effect. In this embodiment, temperature, pH value, iron ion concentration, and copper ion concentration can be obtained using common thermometers, pH meters, and metal ion analyzers. Those skilled in the art can choose according to their needs without requiring creative effort. In this embodiment, the amount of acid added in the subsequent third batch (Q3) is dynamically adjusted based on the monitoring parameters after the first and second batches of acid addition, and the time interval between the second and third batches is Δt2. Specifically, this can be calculated using the following formula:

[0067] ;

[0068] ;

[0069] In the formula, Q3 is the amount of acid solution added in the third batch, in L;

[0070] Q1 is the amount of acid solution added in the first batch, in liters (L).

[0071] Q2 represents the amount of acid solution added in the second batch, in liters (L).

[0072] k3 is a correction factor for the amount of acid added in the third batch, ranging from 0.5 to 1.2. k3 is also a coefficient related to changes in monitored parameters. For example, if the real-time temperature is higher than the temperature monitoring threshold, k3 will approach 0.5, and vice versa; if the real-time pH is lower than the pH monitoring threshold, k3 will approach 0.5, and vice versa; if the rate of change in iron ion concentration is lower than the iron change monitoring threshold, k3 will approach 1.2, and vice versa; if the rate of change in copper ion concentration is lower than the copper change monitoring threshold, k3 will approach 1.2, and vice versa. The specific value of k3 can be chosen by considering temperature, pH, iron ion concentration changes, or copper ion concentration changes individually, or by considering a combination of factors (e.g., a weighted coefficient).

[0073] L is a preset batch number correction value, which is an integer from 0 to 25; L is a coefficient that is only related to the changes in monitoring parameters after the first and second batches of acid are added. If the changes in monitoring parameters before and after the first and second batches are large (such as large temperature fluctuations and high rate of change in iron ion concentration), it indicates that the iron impurities in the mixed system react more violently with the acid and need to be moderated and controlled. The batch number cannot be reduced too much, so the value of L will approach 0, and otherwise it will approach 25.

[0074] △t1 is the time interval between the first and second batches, in seconds;

[0075] △t2 is the time interval between the second and third batches, in seconds;

[0076] S2 is the correction factor for the time interval between the second and third batches, ranging from 0.5 to 1.5; S2 is also a coefficient related to the changes in monitoring parameters after the first and second batches of acid are added. If the changes in monitoring parameters before and after the first and second batches are large (e.g., large temperature fluctuations, high rate of change in iron ion concentration), it indicates that the iron impurities in the system react more violently with the acid, and the value of L will approach 1.5; otherwise, it will approach 0.5.

[0077] Step S5: Repeat step S4 until the concentration of iron ions in the mixed system tends to be constant. Stop adding acid solution to complete the iron purification and impurity removal, and wait for post-processing, such as water washing and drying.

[0078] In this embodiment, the repeated operation mainly involves adding Q of the acid solution in the j-th batch. j The time interval between batch j-1 and batch j is Δt j-1 The calculation involves adding acid. Specifically, the calculation can be performed using the following formula:

[0079] ;

[0080] ;

[0081] In the formula, Q1 is the amount of acid solution added in the first batch, in L;

[0082] Q2 represents the amount of acid solution added in the second batch, in liters (L).

[0083] Q j Let J be the amount of acid solution added in the j-th batch, in liters (L); where j ≥ 3.

[0084] k j This is a correction factor for the amount of acid added in the j-th batch, with a value ranging from 0.5 to 1.2.

[0085] △t j-1 The time interval between batch j-1 and batch j, in seconds;

[0086] L is a preset batch number correction value related to the changes in monitoring parameters after the first and second batches of acid are added, and the value is an integer from 0 to 25; that is, the actual batches carried out after the second batch are (nj-1-L).

[0087] S j-1 This is a correction factor for the time interval between batch j-1 and batch j, with a value ranging from 0.5 to 1.5.

[0088] If the amount added in the last batch does not apply to the formula above, use the actual total amount of acid consumed as a distance from the theoretical amount Q. all The difference is used as the amount added.

[0089] In this embodiment, the control endpoint is defined as the iron ion concentration becoming constant (e.g., the iron ion concentration no longer changes or the increase in iron ion concentration is very small). If the control endpoint is reached, regardless of whether the actual total acid consumption is less than or equal to the theoretical consumption Q, the endpoint is considered reached. all Immediately stop adding acid; if the actual total amount of acid consumed equals the theoretical amount Q, then... all If the control endpoint is not reached by then, acid solution will continue to be added based on the amount of acid added in the last batch and the interval time Δt1, until the control endpoint is reached.

[0090] The copper powder purification and iron removal control method based on multi-parameter monitoring in this embodiment can achieve precise iron removal by acid leaching, thereby improving the purity of copper powder. At the same time, the acid solution is added in batches and the amount of acid solution added in each batch is dynamically controlled to prevent excessive acid solution from inducing local violent reactions and causing copper powder corrosion and loss. The amount of acid solution added is also precisely controlled to reduce the cost of subsequent wastewater treatment.

[0091] In this embodiment, to reduce the risk of hydrogen explosion caused by hydrogen accumulation due to the acid leaching process for iron removal, an appropriate amount of inert gas, such as nitrogen, is simultaneously introduced into the bottom of the mixing system during each batch of acid addition. On the one hand, nitrogen can dilute the hydrogen; on the other hand, the release of nitrogen can also isolate oxygen, reducing copper powder oxidation.

[0092] The following is a more specific example.

[0093] A copper powder weighs 100 kg (W). The iron content (C) in the copper powder was measured. Fe The concentration is 1 wt% (approximately 1 kg). Acid leaching with 0.1 mol / L dilute sulfuric acid is planned. Calculate the theoretical acid consumption Q. all for:

[0094] L.

[0095] The initial settings are: preset batch number n=40, and interval Δt1=60s between the first batch of acid addition and the second batch of acid addition.

[0096] The initial amount of acid added, Q1, is calculated as follows:

[0097] L

[0098] The amount of acid added in the second batch, Q2, is:

[0099] L.

[0100] From the first batch to the second batch of acid added, monitoring parameters showed no significant change in the temperature of the mixed system, a moderate rate of change in iron ion concentration, and a basically constant copper ion concentration. This indicates that the aforementioned control measures were appropriate and can be continued accordingly, with the amount and interval of subsequent acid additions remaining essentially unchanged.

[0101] Therefore, the amount of acid added in the third batch is:

[0102] L;

[0103] s.

[0104] From the first batch to the second batch of acid added, if the monitoring parameters show a high rate of change in the iron ion concentration in the mixed system, it indicates that the reaction between the acid and iron in the mixed system is relatively intense, and further control is needed.

[0105] Therefore, the amount of acid added in the third batch is:

[0106] L;

[0107] s.

[0108] Continue to monitor the mixed system, and repeatedly adjust the addition of acid in subsequent batches based on the monitoring parameters until the concentration of iron ions in the mixed system tends to be constant. Stop adding acid to complete the iron purification and impurity removal process, and wait for post-processing, such as water washing and drying.

Claims

1. A method for controlling the purification and iron removal of copper powder based on multi-parameter monitoring, characterized in that, Includes the following steps: Step S1: Obtain basic information about the copper powder to be processed; simultaneously, calculate the theoretical amount Q of acid solution with a planned molar concentration M based on the basic information. all The basic information includes the weight W of the copper powder and the iron content C in the copper powder. Fe ; Step S2: Mix the copper powder with pure water according to a preset solid-liquid ratio; Step S3: Set the preset batch number n for adding the acid solution in batches; based on the theoretical dosage Q. all Given the preset batch number n, generate the amount Q1 of the first batch of acid solution added and the amount Q2 of the second batch of acid solution added, and set the interval between the first batch of acid solution added and the second batch of acid solution added as Δt1. Step S4: Obtain the monitoring parameters of the mixing system before and after the addition of the acid solution, and compare them with the subsequent batch addition process of the acid solution after dynamic adjustment based on the monitoring parameters; Step S5: Repeat step S4 until the concentration of iron ions in the mixed system tends to be constant, then stop adding the acid solution to complete the iron purification and impurity removal.

2. The copper powder purification and iron removal control method based on multi-parameter monitoring according to claim 1, characterized in that, The acid solution is acetic acid, 0.1~2 mol / L dilute hydrochloric acid, or 0.1~4 mol / L dilute sulfuric acid.

3. The copper powder purification and iron removal control method based on multi-parameter monitoring according to claim 1, characterized in that, The solid-liquid ratio is 1:(20~50).

4. The copper powder purification and iron removal control method based on multi-parameter monitoring according to claim 3, characterized in that, The solid-liquid ratio is 1:(30~40).

5. The copper powder purification and iron removal control method based on multi-parameter monitoring according to claim 1, characterized in that, The stirring speed during step S2 is 200~500 r / min.

6. The copper powder purification and iron removal control method based on multi-parameter monitoring according to any one of claims 1 to 5, characterized in that, The preset batch number n ≥ 10.

7. The copper powder purification and iron removal control method based on multi-parameter monitoring according to claim 6, characterized in that, 30≤n≤50。 8. The copper powder purification and iron removal control method based on multi-parameter monitoring according to claim 7, characterized in that, The amount of acid solution added in the first batch (Q1) and the amount of acid solution added in the second batch (Q2) in step S3 are obtained using the following formula: ； ； In the formula, Q1 is the amount of acid solution added in the first batch; Q2 is the amount of acid solution added in the second batch; n is the preset batch number; k1 is a correction coefficient for the amount of acid added in the first batch, with a value ranging from 0.5 to 0.7; k2 is a correction factor for the amount of acid added in the second addition, with a value ranging from 0.6 to 0.

8.

9. The copper powder purification and iron removal control method based on multi-parameter monitoring according to claim 8, characterized in that, In step S4, the amount Q of the acid solution added in the jth batch is... j The time interval Δt between batch j-1 and batch j j-1 The following formula is used to derive: ； ； In the formula, Q1 is the amount of acid solution added in the first batch; Q2 is the amount of acid solution added in the second batch; Q j Let j be the amount of acid solution added in the j-th batch; where j ≥ 3; k j The correction factor for the amount of acid added in the j-th batch is 0.5 to 1.

2. △t j-1 The time interval between batch j-1 and batch j; L is a correction value for the preset batch number n related to the changes in the monitoring parameters after the first and second batches of acid are added, and the value is an integer from 0 to 25; S j-1 This is a correction factor for the time interval between batch j-1 and batch j, with a value ranging from 0.5 to 1.

5.

10. The copper powder purification and iron removal control method based on multi-parameter monitoring according to any one of claims 1-5 and 7-9, characterized in that, During each batch of acid solution added to the mixture, an inert gas is simultaneously introduced into the bottom of the mixture.

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