Extracting agent as well as preparation method and application thereof

Abstract

The invention discloses an extracting agent and a preparation method and application thereof, and belongs to the technical field of chemical engineering. The extraction agent is prepared from bis (2-ethylhexyl) phosphate and 2-hydroxy-3-naphthalene mehydroxamic acid. In addition, the invention further provides a preparation method of the extraction agent, and the preparation method comprises the step of mixing the di (2-ethylhexyl) phosphate and the 2-hydroxy-3-naphthohydroxamic acid to obtain the extraction agent. In addition, the invention also provides an application of the extraction agent or the extraction agent prepared by the preparation method in extraction of tin ions. The extraction rate of the extraction agent provided by the invention on tin ions is as high as 98.8%.

Description

Technical Field

[0001] The invention relates to the technical field of chemical industry, and in particular to an extractant and a preparation method and application thereof. Background Art

[0002] Tin-plated parts cleaning liquid, also known as tin stripping waste liquid, is wastewater generated by electronic component companies during the production of printed circuit boards (PCBs). Tin-plated parts cleaning liquid mainly contains valuable metals such as tin (Sn), copper (Cu) and methanesulfonic acid. With the continuous development of the tin industry, tin has gradually become an indispensable key rare metal in modern industry and has a wide range of industrial uses, the most important of which is in the tin-plating industry.

[0003] Common recycling treatment methods for tin-plated parts cleaning liquid include distillation recovery method, acid precipitation method, diffusion dialysis-electrodeposition method, electrolysis-precipitation method, membrane treatment method, etc. These methods have achieved the recycling of tin to a certain extent, but the distillation recovery method has high energy consumption and narrow industrial application; the acid precipitation method requires the formation of a continuous and specialized production line, which makes the initial investment large; the diffusion dialysis-electrodeposition method has high cost and poor repeatability; the electrolysis-precipitation method requires the consumption of a large amount of chemical agents to complete the extraction and precipitation process, and the treatment process is relatively complicated; the membrane treatment method requires additional processes and agents to solve the problem of ultrafiltration membrane pollution. In addition, the existing extractants are difficult to achieve a good separation effect on the tin ions in the tin-plated parts cleaning liquid, which limits the recycling of the tin-plated parts cleaning liquid to a certain extent, and the extraction rate of tin ions is not high. Summary of the invention

[0004] The purpose of the present invention is to overcome the above technical deficiencies, provide an extractant and a preparation method and application thereof, and solve the technical problem of how to improve the recovery rate of tin ions in the prior art.

[0005] In order to achieve the above technical purpose, the technical solution of the present invention provides an extractant, including di(2-ethylhexyl)phosphate and 2-hydroxy-3-naphthohydroxamic acid.

[0006] In any embodiment, the mass ratio of the di(2-ethylhexyl)phosphate to the 2-hydroxy-3-naphthohydroxamic acid is (1-6):1.

[0007] In any embodiment, a solvent is further included, and the material ratio of the total amount of the di(2-ethylhexyl)phosphate and the 2-hydroxy-3-naphthohydroxamic acid to the solvent is (30-200) g:1L.

[0008] In any embodiment, the solvent is ethyl acetate.

[0009] In addition, the present invention also provides a method for preparing the extractant, comprising: mixing di(2-ethylhexyl)phosphate and 2-hydroxy-3-naphthohydroxamic acid.

[0010] In addition, the present invention also provides a use of the extractant or the extractant prepared by the preparation method in extracting tin ions.

[0011] In any embodiment, the extractant is used to extract tin ions in the tin-plated parts cleaning solution.

[0012] In any embodiment, the above application includes the following steps:

[0013] The pH of the tin-plated parts cleaning solution is adjusted to 2-3, and then an extractant is added to extract the tin ions into the organic phase.

[0014] In any embodiment, the extractant is added according to a volume ratio of the extractant to the tin-plated parts cleaning solution of 1:(1-1.5).

[0015] In any embodiment, the process further comprises adding a sulfuric acid solution to the organic phase for stripping to obtain an acid solution containing tin ions.

[0016] Compared with the prior art, the beneficial effects of the present invention include: the extractant proposed by the present invention includes di(2-ethylhexyl) phosphate and 2-hydroxy-3-naphthohydroxamic acid, and under the cooperation of these two compounds, the extraction rate of tin ions is as high as 98.8%. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a schematic diagram of the overall process of preparing an extractant and using the extractant to extract tin ions in Example 1 of the present invention.

[0018] Figure 2 This is a photograph of step (1) of extracting tin ions in Example 1 of the present invention, wherein the mixture is stirred at room temperature and allowed to stand for decomposition. DETAILED DESCRIPTION

[0019] The "range" disclosed in the present application is defined in the form of a lower limit and an upper limit, and a given range is defined by selecting a lower limit and an upper limit, and the selected lower limit and upper limit define the boundaries of the particular range. The range defined in this way can be inclusive or exclusive of the end values, and can be arbitrarily combined, that is, any lower limit can be combined with any upper limit to form a range. For example, if a range of 60 to 120 and 80 to 110 is listed for a particular parameter, it is understood that a range of 60 to 110 and 80 to 120 is also expected. In addition, if the minimum range values ​​1 and 2 are listed, and if the maximum range values ​​3, 4 and 5 are listed, the following ranges can all be expected: 1 to 3, 1 to 4, 1 to 5, 2 to 3, 2 to 4 and 2 to 5. In the present application, unless otherwise specified, the numerical range "a to b" represents an abbreviation of any real number combination between a and b, where a and b are both real numbers. For example, the numerical range "0-5" means that all real numbers between "0-5" are listed in this document, and "0-5" is just an abbreviation of these numerical combinations. In addition, when a parameter is expressed as an integer ≥ 2, it is equivalent to disclosing that the parameter is, for example, an integer of 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc.

[0020] If there is no special explanation, the "include" and "comprising" mentioned in this application are open-ended or closed-ended. For example, the "include" and "comprising" may mean that other components not listed may also be included or only the listed components may be included or only the listed components may be included.

[0021] If not specifically stated, in this application, the term "or" is inclusive. For example, the phrase "A or B" means "A, B, or both A and B". More specifically, any of the following conditions satisfies the condition "A or B": A is true (or exists) and B is false (or does not exist); A is false (or does not exist) and B is true (or exists); or both A and B are true (or exist).

[0022] This specific embodiment provides an extractant, including di(2-ethylhexyl)phosphate and 2-hydroxy-3-naphthohydroxamic acid; the mass ratio of the di(2-ethylhexyl)phosphate to the 2-hydroxy-3-naphthohydroxamic acid is (1-6):1.

[0023] In some embodiments, the extractant further comprises a solvent, and the material ratio of the total amount of the di(2-ethylhexyl)phosphate and the 2-hydroxy-3-naphthohydroxamic acid to the solvent is (30-200) g:1L; and the solvent is ethyl acetate.

[0024] In addition, this specific embodiment also provides a method for preparing an extractant, comprising: mixing di(2-ethylhexyl)phosphate and 2-hydroxy-3-naphthohydroxamic acid.

[0025] In addition, this specific embodiment also proposes a use of the above-mentioned extractant or the extractant prepared by the above-mentioned preparation method in extracting tin ions, comprising the following steps:

[0026] Adjust the pH of the tin-plated cleaning solution to 2-3, then add an extractant to extract the tin ions into the organic phase;

[0027] A sulfuric acid solution is added to the organic phase for stripping to obtain an acid solution containing tin ions.

[0028] In some embodiments, the extractant is used to extract tin ions in the tin-plated parts cleaning solution, and the amount of the extractant added per liter of the tin-plated parts cleaning solution is 5-20 g.

[0029] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0030] In the present invention, reference is made to “some embodiments”, “this embodiment”, examples, etc., which describe a subset of all possible embodiments, but it can be understood that “some embodiments” may be the same subset or different subsets of all possible embodiments and may be combined with each other without conflict.

[0031] If similar descriptions of "first / second" appear in the application documents, the following instructions are added. In the following description, the terms "first\second\third" involved are merely used to distinguish similar objects and do not represent a specific ordering of the objects. It can be understood that "first\second\third" can be interchanged in a specific order or sequence where permitted, so that the embodiments described herein can be implemented in an order other than that illustrated or described herein.

[0032] In this embodiment, the term "and / or" is merely a description of the association relationship between associated objects, indicating that three relationships may exist. For example, object A and / or object B may represent three situations: object A exists alone, object A and object B exist at the same time, and object B exists alone.

[0033] Hereinafter, the embodiments of the present application will be described. The embodiments described below are exemplary and are only used to explain the present application, and should not be construed as limiting the present application. If no specific techniques or conditions are indicated in the embodiments, the techniques or conditions described in the literature in this area or the product specifications are used. If the manufacturer is not indicated in the reagents or instruments used, they are all conventional products that can be obtained commercially.

[0034] In the following embodiments or comparative examples, the tin-plated parts cleaning liquid from a chemical park in Hubei Province is used as the extraction object, wherein the tin ion content is w0=11.00wt%.

[0035] Example 1

[0036] Combination Figure 1 , this embodiment provides an extractant, which is prepared by the following steps:

[0037] To a beaker containing 37.5 g of di(2-ethylhexyl) phosphate (i.e., P204) and 12.5 g of 2-hydroxy-3-naphthohydroxamic acid (i.e., H205), 1000 mL of ethyl acetate was added and stirred evenly to obtain a 50 g / L extractant mixture (the mass ratio of P204 to H205 was 3:1).

[0038] This embodiment also proposes the use of the extractant in this embodiment in extracting tin ions, as follows:

[0039] (1) Measure 100 mL of tin-plated cleaning liquid and place it in a 500 mL beaker. After adjusting the pH to 2 with hydrochloric acid, add 100 mL of the extractant, the phase ratio (oil phase / water phase) is 1, and the extraction level is 1. After stirring at room temperature for 10 minutes, pour it into a separatory funnel, let it stand and separate the layers, and separate the organic phase and the aqueous phase. Figure 2 It can be seen that obvious stratification occurred during the standing process. By detecting the tin ion content of the aqueous phase, the extraction rate was found to be 98.5%.

[0040] (2) Add 2.5 mol / L sulfuric acid solution to the organic phase in step (1), stir at room temperature for 10 min, pour into a separatory funnel, let stand to separate the layers, and separate the layers to obtain an acid solution containing tin ions. The stripping rate was 93.8% by detecting the tin ion content of the aqueous phase.

[0041] (3) The organic phase in step (2) is washed with water and reused as an extractant.

[0042] Example 2

[0043] This embodiment provides an extractant, which is prepared by the following steps:

[0044] To a beaker containing 37.5 g of di(2-ethylhexyl) phosphate (ie, P204) and 12.5 g of 2-hydroxy-3-naphthohydroxamic acid (ie, H205), 1670 mL of ethyl acetate was added and stirred evenly to obtain a 30 g / L extractant mixture.

[0045] This embodiment also proposes the use of the extractant in this embodiment in extracting tin ions, which is as follows:

[0046] (1) Measure 100 mL of tin-plated cleaning liquid and place it in a 500 mL beaker. After adjusting the pH to 2 with hydrochloric acid, add 100 mL of the extractant, the phase ratio (oil phase / water phase) is 1, and the extraction level is 1. After stirring at room temperature for 10 minutes, pour it into a separatory funnel, let it stand and separate the layers, and separate the organic phase and the aqueous phase. It was determined that the extraction rate of tin ions in the organic phase was 89.2%.

[0047] (2) Add 2.5 mol / L sulfuric acid solution to the organic phase in step (1), stir at room temperature for 10 min, pour into a separating funnel, let stand to separate the layers, and separate the layers to obtain an acid solution containing tin ions. The stripping rate was determined to be 92.5%.

[0048] (3) The organic phase in step (2) is washed with water and reused as an extractant.

[0049] Example 3

[0050] This embodiment provides an extractant, which is prepared by the following steps:

[0051] To a beaker containing 37.5 g of di(2-ethylhexyl)phosphate (ie, P204) and 12.5 g of 2-hydroxy-3-naphthohydroxamic acid (ie, H205) was added 500 mL of ethyl acetate and stirred evenly to obtain a 100 g / L extractant mixture.

[0052] This embodiment also proposes the use of the extractant in this embodiment in extracting tin ions from the tin-plated parts cleaning solution. The specific steps are the same as those in Example 1. Finally, the extraction rate of tin ions is 98.6%, and the stripping rate is 93.8%.

[0053] Example 4

[0054] This embodiment provides an extractant, which is prepared by the following steps:

[0055] To a beaker containing 37.5 g of di(2-ethylhexyl)phosphate (ie, P204) and 12.5 g of 2-hydroxy-3-naphthohydroxamic acid (ie, H205) was added 250 mL of ethyl acetate and stirred evenly to obtain a 200 g / L extractant mixture.

[0056] This embodiment also proposes the use of the extractant in this embodiment in extracting tin ions from the tin-plated parts cleaning solution. The specific steps are the same as those in Example 1. Finally, the extraction rate of tin ions is 98.8%, and the stripping rate is 93.7%.

[0057] Example 5

[0058] This embodiment provides an extractant, which is prepared by the following steps:

[0059] To a beaker containing 12.5 g of di(2-ethylhexyl) phosphate (i.e., P204) and 12.5 g of 2-hydroxy-3-naphthohydroxamic acid (i.e., H205), add 250 mL of ethyl acetate and stir evenly to obtain a 100 g / L extractant mixture (the mass ratio of P204 to H205 is 1:1).

[0060] This embodiment also proposes the use of the extractant in this embodiment in extracting tin ions from the tin-plated parts cleaning solution. The specific steps are the same as those in Example 1. Finally, the extraction rate of tin ions is 85.6%, and the stripping rate is 92.2%.

[0061] Example 6

[0062] This embodiment provides an extractant, which is prepared by the following steps:

[0063] To a beaker containing 25.0 g of di(2-ethylhexyl) phosphate (i.e., P204) and 12.5 g of 2-hydroxy-3-naphthohydroxamic acid (i.e., H205), 375 mL of ethyl acetate was added and stirred evenly to obtain a 100 g / L extractant mixture (the mass ratio of P204 to H205 was 2:1).

[0064] This embodiment also proposes the use of the extractant in this embodiment in extracting tin ions from the tin-plated parts cleaning solution. The specific steps are the same as those in Example 1. Finally, the extraction rate of tin ions is 95.2%, and the stripping rate is 92.3%.

[0065] Example 7

[0066] This embodiment provides an extractant, which is prepared by the following steps:

[0067] To a beaker containing 50.0 g of di(2-ethylhexyl) phosphate (i.e., P204) and 12.5 g of 2-hydroxy-3-naphthohydroxamic acid (i.e., H205), 625 mL of ethyl acetate was added and stirred evenly to obtain a 100 g / L extractant mixture (the mass ratio of P204 to H205 was 4:1).

[0068] This embodiment also proposes the use of the extractant in this embodiment in extracting tin ions from the tin-plated parts cleaning solution. The specific steps are the same as those in Example 1. Finally, the extraction rate of tin ions is 98.4%, and the stripping rate is 93.7%.

[0069] Example 8

[0070] This embodiment provides an extractant, which is prepared by the following steps:

[0071] To a beaker containing 62.5 g of di(2-ethylhexyl) phosphate (i.e., P204) and 12.5 g of 2-hydroxy-3-naphthohydroxamic acid (i.e., H205), add 750 mL of ethyl acetate and stir evenly to obtain a 100 g / L extractant mixture (the mass ratio of P204 to H205 is 5:1).

[0072] This embodiment also proposes the use of the extractant in this embodiment in extracting tin ions from the tin-plated parts cleaning solution. The specific steps are the same as those in Example 1. Finally, the extraction rate of tin ions is 93.3% and the stripping rate is 92.9%.

[0073] Example 9

[0074] This embodiment provides an extractant, which is prepared by the following steps:

[0075] To a beaker containing 75.0 g of di(2-ethylhexyl) phosphate (i.e., P204) and 12.5 g of 2-hydroxy-3-naphthohydroxamic acid (i.e., H205), add 875 mL of ethyl acetate and stir evenly to obtain a 100 g / L extractant mixture (the mass ratio of P204 to H205 is 6:1).

[0076] This embodiment also proposes the use of the extractant in this embodiment in extracting tin ions from the tin-plated parts cleaning solution. The specific steps are the same as those in Example 1. Finally, the extraction rate of tin ions is 84.7% and the stripping rate is 92.1%.

[0077] Comparative Example 1

[0078] To a beaker containing 50 g of di(2-ethylhexyl) phosphate (ie, P204), 1000 mL of ethyl acetate was added and stirred evenly to obtain 50 g / L of an extractant.

[0079] This comparative example also proposes the use of the extractant in the comparative example in extracting tin ions from the tin-plated parts cleaning solution. The specific steps are the same as those in Example 1. The extractant is added to the tin-plated parts cleaning solution, and the final tin ion extraction rate is 76.9% and the back extraction rate is 91.8%.

[0080] Comparative Example 2:

[0081] To a beaker containing 50 g of 2-hydroxy-3-naphthohydroxamic acid (i.e., H205), add 1000 mL of ethyl acetate and stir evenly to obtain 50 g / L of an extractant.

[0082] This comparative example also proposes the use of the extractant in the comparative example in extracting tin ions from the tin-plated parts cleaning solution. The specific steps are the same as those in Example 1. The extractant is added to the tin-plated parts cleaning solution, and the final tin ion extraction rate is 48.8% and the back-extraction rate is 91.5%.

[0083] Table 1 Flotation results of Examples 1-9 and Comparative Examples 1-2

[0084] serial number Extraction rate of tin ions / % Stripping rate of tin ions / % Example 1 98.5 93.8 Example 2 89.2 92.5 Example 3 98.6 93.8 Example 4 98.8 93.7 Example 5 85.6 92.2 Example 6 95.2 92.3 Example 7 98.4 93.7 Example 8 93.3 92.9 Example 9 84.7 92.1 Comparative Example 1 76.9 91.8 Comparative Example 2 48.8 91.5

[0085] It can be seen from Table 1 that the extraction efficiency of using a mixture of di(2-ethylhexyl) phosphate and 2-hydroxy-3-naphthohydroxamic acid is significantly improved compared with using a single extraction agent, and the extraction rate can be as high as 98.8%, and the stripping rate can be as high as 93.8%.

[0086] The specific implementation of the present invention described above does not constitute a limitation on the protection scope of the present invention. Any other corresponding changes and modifications made based on the technical concept of the present invention should be included in the protection scope of the claims of the present invention.

Claims

1. An extractant, characterized in that These include di(2-ethylhexyl)phosphate and 2-hydroxy-3-naphthohydroxamic acid.

2. The extractant according to claim 1, characterized in that The mass ratio of the di(2-ethylhexyl)phosphate to the 2-hydroxy-3-naphthohydroxamic acid is (1-6):

1.

3. The extractant according to claim 1 or 2, characterized in that The invention also comprises a solvent, and the material ratio of the total amount of the di(2-ethylhexyl)phosphate and the 2-hydroxy-3-naphthohydroxamic acid to the solvent is (30-200) g:1L.

4. The extractant according to claim 3, characterized in that The solvent is ethyl acetate.

5. A method for preparing the extractant according to any one of claims 1 to 4, characterized in that: include: The product is obtained by mixing di(2-ethylhexyl)phosphate and 2-hydroxy-3-naphthohydroxamic acid.

6. Use of the extractant according to any one of claims 1 to 4 or the extractant prepared by the preparation method according to claim 5 in extracting tin ions.

7. The use according to claim 6, characterized in that: The extractant is used for extracting tin ions in the tin-plated parts cleaning solution.

8. The use according to claim 6, characterized in that: The following steps are involved: The pH of the tin-plated parts cleaning solution is adjusted to 2-3, and then an extractant is added to extract the tin ions into the organic phase.

9. The use according to claim 8, characterized in that: The extractant is added according to a volume ratio of the extractant to the tin-plated parts cleaning solution of 1:(1-1.5).

10. The use according to claim 8, characterized in that: The method also includes adding a sulfuric acid solution to the organic phase for stripping to obtain an acid solution containing tin ions.

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