A method for producing electrolytic copper powder

Abstract

The application belongs to the field of powder metallurgy manufacturing, and particularly discloses a production method of electrolytic copper powder, which is characterized by adopting a new wet oxidation prevention technology for the electrolytic copper powder, is simple in operation, short in technological process, and good in oxidation prevention effect; and a low-temperature nitrogen drying technology is adopted for the drying technology of the product in the later period, so that the method for reducing hydrogen gas by ammonia decomposition is not needed, the powder body cannot be caused to be aggregated and the dendrite shrinks due to high-temperature sintering, the internal dendrite morphology structure of the copper powder is well preserved, the quality is high, the copper powder is applied to the fields of powder metallurgy parts, diamond products, electrocarbon products, electronic materials and chemical catalysts, and the quality and stability of the products of downstream customers are ensured.

Description

TECHNICAL FIELD

[0001] The application belongs to the field of powder metallurgy manufacturing, and particularly relates to a production method of electrolytic copper powder. BACKGROUND

[0002] The main anti-oxidation technical means of electrolytic copper powder is hydrogen reduction method. The electrolytic copper powder produced by the method has the defects of poor dendritic morphology structure, poor formability, serious agglomeration and the like. The electrolytic copper powder product has poor quality and cannot be used in the electric carbon manufacturing industry on a large scale. In order to make up for the deficiency, the low-temperature drying technology and the wet anti-oxidation technology are mainly adopted to produce the electrolytic copper powder. SUMMARY

[0003] The application aims to provide a production method of electrolytic copper powder, which improves the internal morphology structure of the electrolytic copper powder and improves the process technical index of the electrolytic copper powder product by adopting new anti-oxidation and drying means.

[0004] In order to achieve the above-mentioned purpose, the technical scheme adopted by the application is as follows:

[0005] A production method of electrolytic copper powder, characterized in that the method comprises the following steps:

[0006] First step: using an electrolytic copper plate as an anode, using a copper sulfate solution as an electrolyte, and adopting an electrolysis method to prepare electrolytic copper powder;

[0007] Second step: performing a wet anti-oxidation process, using TTA as a wet anti-oxidation agent, using alcohol as a solvent to dissolve the TTA, and then adding pure water to prepare an anti-oxidation agent solution, the mass ratio of which is controlled to be between 0.35% and 0.45%, and the electrolytic copper powder is soaked in the prepared anti-oxidation agent solution for 15-17 min after being washed;

[0008] Third step: performing a powder washing process, using pure water to wash the electrolytic copper powder, and performing the second step of the wet anti-oxidation process after the second powder washing operation and after the last powder washing operation;

[0009] Fourth step: drying, using a drying box to dry the material, and the drying temperature is 50-60 DEG C;

[0010] Fifth step: screening and batching, screening the dried material through a screening machine and batching.

[0011] Preferably, TTA is used as the main wet anti-oxidation agent in the second step, and the use method is to use alcohol as a solvent to dissolve the TTA, and the mass ratio of TTA to alcohol is 3:5 to ensure that the anti-oxidation agent TTA is completely dissolved into a transparent liquid.

[0012] Preferably, the wet anti-oxidation electrolytic copper powder in the fourth step is dried, and the low-temperature nitrogen drying technology is used for drying treatment of the electrolytic copper powder, nitrogen gas is filled in the drying box as a protective gas to prevent the powder from being oxidized during the drying process, and the drying temperature is controlled within 50-60 DEG C.

[0013] The beneficial effects of the present application are:

[0014] The wet anti-oxidation technology of the production method of the electrolytic copper powder of the present application not only saves manpower and cost, but also greatly improves the production efficiency, and the anti-oxidation effect is also simple and convenient to operate compared with the traditional method. The low-temperature nitrogen drying technology not only saves production and labor cost, but also effectively ensures that the electrolytic copper powder dendrite structure is well preserved and not agglomerated. The electrolytic copper powder prepared by the above method has greatly improved process technical index and increased use field range. BRIEF DESCRIPTION OF DRAWINGS

[0015] Figure 1 It is an electron microscope picture of the electrolytic copper powder sample of Example 1;

[0016] Figure 2 It is a scanning electron microscope picture of the electrolytic copper powder of Example 2;

[0017] Figure 3 It is a scanning electron microscope picture of the electrolytic copper powder of Example 3. DETAILED DESCRIPTION

[0018] The specific steps of the present application are as follows:

[0019] 1. Electrolytic powder preparation: using electrolytic copper plate as anode, electrolytic copper powder is prepared by using soluble anode electrolysis method;

[0020] 2. Powder washing: the electrolytic copper powder is washed with pure water until the SO4 2- and the like in the electrolytic copper powder meet the relevant process standards, and the powder washing operation is completed;

[0021] 3. Wet anti-oxidation: TTA is used as a wet anti-oxidant, and alcohol is used as a solvent to dissolve TTA; the mass ratio of TTA to alcohol is 3:5, pure water is added after TTA is completely dissolved, an anti-oxidant solution is prepared, and finally the mass ratio of TTA to solution is ensured to be between 0.35%-0.45%. After the third and last washing process of the powder washing of operation 2, the prepared anti-oxidant solution is added to the electrolytic copper powder for wet anti-oxidation, and each operation is static immersion for 15-16 min;

[0022] 4. Drying: the material is dried by using a drying box, the drying temperature is set within 50-60 DEG C, and nitrogen gas is filled in the drying box as a protective gas to prevent the powder from being oxidized during the drying process;

[0023] 5. Screening and batching: the dried material is screened by a screening machine and batched, and a -200 mesh screen aperture is selected for screening.

[0024] The performance of the electrolytic copper powder prepared by the above steps is shown in Table 1 below:

[0025] Table 1 Main technical indicators of electrolytic copper powder

[0026]

[0027] The application will be further described below in combination with specific examples:

[0028] Example 1

[0029] 1. Using an electrolytic copper plate as an anode, electrolytic copper powder is prepared by a soluble anode electrolysis method;

[0030] 2. The electrolytic copper powder is washed with pure water until the SO4 2- and other substances in the electrolytic copper powder meet the relevant process standards, and the powder washing operation is completed;

[0031] 3. TTA is used as a wet oxidation inhibitor, alcohol is used as a solvent to dissolve TTA, and the mass ratio of TTA to alcohol is 3:5. After TTA is completely dissolved, pure water is added to prepare an oxidation inhibitor solution, and finally the mass ratio of added TTA to the solution is 0.4%. After the third and last washing of the powder in operation 2, the prepared oxidation inhibitor solution is added to the electrolytic copper powder for wet oxidation, and each operation is static immersion for 16 minutes;

[0032] 4. The material is dried in a drying oven, and the drying temperature is set to be within 50°C. Nitrogen gas is introduced into the drying oven as a protective gas to prevent the powder from being oxidized during the drying process;

[0033] 5. The dried material is screened by a screening machine and batched, and a -200 mesh screen aperture is selected for screening.

[0034] The process technical parameter results of the electrolytic copper powder prepared by the above method are shown in Table 2 below:

[0035] Table 2 Process technical data of electrolytic copper powder

[0036]

[0037] The attached Figure 1 are electron microscope photos of the relevant electrolytic copper powder samples.

[0038] The electrolytic copper powder prepared by the above method has advanced technical indicators and meets the relevant process technical standards, and can be applied to industrial fields such as the electric carbon industry.

[0039] Example 2

[0040] 1. Using electrolytic copper plate as anode, electrolytic copper powder is prepared by soluble anode electrolysis method;

[0041] 2. The electrolytic copper powder is washed with pure water until the SO4 2- and the like in the electrolytic copper powder meet the relevant process standards, and the powder washing operation is completed;

[0042] 3. TTA is used as a wet oxidation inhibitor, and alcohol is used as a solvent to dissolve TTA. The mass ratio of TTA to alcohol is 3:5. After TTA is completely dissolved, pure water is added to prepare an oxidation inhibitor solution. The final mass ratio of TTA to solution is 0.45%. After the third and last washing of the electrolytic copper powder in operation 2, the prepared oxidation inhibitor solution is added to the electrolytic copper powder for wet oxidation, and each operation is static immersion for 15 min;

[0043] 4. The material is dried in a drying oven, and the drying temperature is set to 55°C. Nitrogen gas is introduced into the drying oven as a protective gas to prevent the powder from being oxidized during the drying process;

[0044] 5. The dried material is sieved by a screening machine and batched, and a -200 mesh sieve with a mesh size of 200 is selected for sieving.

[0045] The electrolytic copper powder prepared by the above method has the following process technical parameter results as shown in Table 3

[0046] Table 3 Process technical data of electrolytic copper powder

[0047]

[0048] The attached Figure 2 are electron microscope photos of the relevant electrolytic copper powder samples:

[0049] The electrolytic copper powder prepared by the above method has advanced technical indicators and meets the relevant process technical standards, and can be applied to industrial fields such as the electric carbon industry.

[0050] Example 3

[0051] 1. Using electrolytic copper plate as anode, electrolytic copper powder is prepared by soluble anode electrolysis method;

[0052] 2. The electrolytic copper powder is washed with pure water until the SO4 2- and the like in the electrolytic copper powder meet the relevant process standards, and the powder washing operation is completed;

[0053] 3. Adopt TTA as wet anti-oxidant, and adopt alcohol as solvent to dissolve TTA. The mass ratio of TTA and alcohol is 3:5. After TTA is completely dissolved, add pure water to prepare anti-oxidant solution. Finally, add TTA with mass ratio of 0.35% to the prepared anti-oxidant solution, and then add the solution to the electrolytic copper powder to carry out wet anti-oxidation after the third and the last washing process of the powder in operation 2, and the static immersion time is 16 min each time;

[0054] 4. Dry the material in a drying oven, and set the drying temperature within 60℃. During the drying process, introduce nitrogen gas into the drying oven as protective gas to prevent the powder from being oxidized;

[0055] 5. Screen the dried material through a screening machine, and then batch the screened material. The screen mesh with a mesh size of-200 is used for screening.

[0056] The electrolytic copper powder prepared by the above method has the following process technical parameter results shown in Table 4

[0057] Table 4 Process technical data of electrolytic copper powder

[0058]

[0059] The attached Figure 3 are electron microscope photos of the electrolytic copper powder samples:

[0060] The electrolytic copper powder prepared by the above method has advanced technical indexes, and meets the relevant process technical standards, and can be applied to the industrial field of electric carbon industry and the like.

Claims

1. A method for producing electrolytic copper powder, characterized by: The method comprises the following steps: First step: using electrolytic copper plate as anode, using copper sulfate solution as electrolyte, electrolytic copper powder is prepared by electrolysis method; Second step: wet anti-oxidation process is carried out, TTA is used as wet anti-oxidant, alcohol is used as solvent to dissolve TTA, pure water is added to prepare anti-oxidant solution, the mass ratio of TTA to anti-oxidant solution is controlled between 0.35%-0.45%, the electrolytic copper powder is soaked in the prepared anti-oxidant solution for 15-17 minutes after washing; Third step: powder washing process is carried out, pure water is used to wash the electrolytic copper powder, and the second wet anti-oxidation process is carried out after the second powder washing operation and after the last powder washing operation; Fourth step: drying, the material is dried in a drying box, the drying temperature is 50-60℃; Fifth step: screening and batching, the dried material is screened and batched by a screening machine.

2. A process for the production of electrolytic copper powder according to claim 1, characterized in that: In the second step, TTA is used as the main wet anti-oxidant, and the method is to dissolve TTA with alcohol as solvent, the mass ratio of TTA to alcohol is 3:5, and the anti-oxidant TTA is completely dissolved into transparent liquid.

3. A process for the production of electrolytic copper powder as claimed in claim 1, wherein: In the fourth step, the electrolytic copper powder after wet anti-oxidation is dried, low-temperature nitrogen drying technology is used for drying treatment of the electrolytic copper powder, nitrogen gas is filled into the drying box as protective gas during the drying process to prevent the powder from being oxidized, and the drying temperature is controlled within 50-60℃.

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