Non-silicon defoamer, synthetic method and application in extraction of rhenium field

Abstract

The application discloses a synthetic method of a non-silicon type defoaming agent and application of the defoaming agent in the field of hydrometallurgical extraction of scandium, and the defoaming agent is synthesized through two-step reactions of three components of A component, B component and C component; the specific synthesis steps are as follows: 1) esterification reaction of amino acid substances A and fatty alcohol substances B to generate amino ester substances D; 2) substitution reaction of the amino ester substances D and triazine compounds C to obtain the non-silicon type defoaming agent. The defoaming agent disclosed by the application has a wide application range, can be applied to a hydrometallurgical front-end scandium extraction method of laterite nickel ore and an MHP hydrometallurgical open circuit scandium impurity process and the like, is added as an auxiliary agent in an extraction process, is used for reducing liquid surface tension, preventing formation and enrichment of a third phase material, reducing occurrence of emulsification, improving process stability and output quality, and has important industrial application value.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of hydrometallurgy, and particularly relates to a non-silicon type defoaming agent, a synthesis method and application in the field of extraction of scandium. BACKGROUND

[0002] Defoaming agents have wide applications in chemical industry and industrial production, and their main function is to inhibit the formation and stabilization of foam in liquid. In the process of extraction of scandium, a large amount of surfactants or other organic substances often exist in the liquid phase, which are prone to form foam, affecting the progress of the reaction and the purity of the product. Therefore, an effective defoaming agent is particularly important in these processes. Traditional defoaming agents are mostly based on silicon compounds, such as silicone oil, silane derivatives, etc. However, silicon-based defoaming agents may have toxicity or poor biodegradability under certain conditions, which limits their development in environmentally friendly applications. Therefore, it is of great scientific significance and application value to develop a non-silicon type and environmentally friendly defoaming agent.

[0003] Most of the currently reported non-silicon type defoaming agents are based on polymers or small organic molecule compounds, but their application research in the process of extraction of metals such as scandium is still relatively limited. Although the existing defoaming agents show good defoaming effect in some fields, there may be certain challenges in terms of stability, selectivity and compatibility with the reaction system in specific extraction of scandium process.

[0004] Therefore, it is urgent to develop a new type of non-silicon defoaming agent with the following characteristics: (1) high defoaming performance, which can effectively inhibit the formation and stabilization of foam in liquid; (2) good environmental friendliness and biodegradability, reducing the negative impact on the environment.

[0005] The present application aims to provide a new synthesis method of non-silicon type defoaming agent and its application in the field of extraction of scandium, in order to solve the limitations of the prior art and meet the urgent needs of high-efficiency and environmentally friendly defoaming agents in industrial production. SUMMARY

[0006] In view of the above problems, the present application discloses a synthesis method of non-silicon type defoaming agent, which can be applied in the field of extraction of scandium as an extractant aid to inhibit the generation of third phase in the extraction process and improve the process stability.

[0007] To achieve the above objectives, the present application adopts the following technical solutions:

[0008] A synthesis method of non-silicon type defoaming agent, which is synthesized by two-step reaction of three components A, B and C;

[0009] The specific synthesis steps are as follows:

[0010] 1) esterification reaction of amino acid substance A and fatty alcohol substance B to generate amino ester substance D;

[0011] 2) substitution reaction of amino ester substance D and triazine compound C to obtain non-silicon type defoamer.

[0012] Preferably, the A component is an amino acid substance, such as one or more of 5-aminopentanoic acid (CAS: 660-88-8), 4-aminobutyric acid (CAS: 56-12-2), 3-aminopropanoic acid (CAS: 107-95-9), 6-aminohexanoic acid (CAS: 60-32-2).

[0013] Preferably, the B component is a fatty alcohol substance, such as one or more of methanol (CAS: 67-56-1), ethanol (CAS: 64-17-5), propanol (CAS: 71-23-8).

[0014] Preferably, the C component is an organic heterocyclic compound, preferably a triazine compound, such as one of 2-chloro-4.6-diamino-1.3.5-triazine (CAS: 3397-62-4), 2-hydroxy-4.6-diamino-1.3.5-triazine (CAS: 108-78-1).

[0015] As a preferred scheme of the process of the present application, the specific process of esterification reaction in step 1) is as follows:

[0016] 1) adding amino acid substance A to the suspension containing fatty alcohol substance B and catalyst to obtain a mixture for reaction;

[0017] 2) after the reaction is completed, continue to heat and reflux; after the heating and reflux is completed, perform post-treatment to obtain amino ester substance D.

[0018] The post-treatment comprises the steps of cooling, removing solvent under reduced pressure, filtering, and drying.

[0019] Preferably, the temperature of the mixture in step 1) is 0-5℃, the amount of amino acid substance D is 0.1-1 mol, the amount of fatty alcohol substance B is 0.5-2 mol, the catalyst is selected from one of SOCl2 (CAS: 7791-09-7), PCl3 (CAS: 7719-12-2), the amount of catalyst is 0.1-2 mol, and the reaction time is 1-5 h.

[0020] Preferably, the heating and reflux temperature in step 2) is 40-80℃, and the reflux time is 1-3 h.

[0021] Preferably, the cooling temperature is 20-35℃, and the pressure is 1-10 kPa.

[0022] Preferably, the filtration is carried out in a non-polar solvent, the residue is suspended in a non-polar solvent for filtration, the non-polar solvent is one or more of hexane, n-pentane (CAS: 109-66-0), cyclohexane (CAS: 110-82-7), dichloromethane (CAS: 75-09-2), and the amount of non-polar solvent is 50-500 ml.

[0023] Preferably, the drying is vacuum drying, the vacuum degree is in the range of 10-100 mmHg, the drying temperature is 30-50℃, and the drying time is 16-28h.

[0024] As a preferred scheme of the process of the present application, the specific process of the substitution reaction in step 2) is as follows:

[0025] 1) Dissolve the triazine compound C in a solvent, and add the amino ester compound D obtained in step 1);

[0026] 2) Heat the obtained mixture for reaction, and after the reaction is completed, carry out post-treatment to obtain the non-silicon type defoamer.

[0027] In the present application, the post-treatment comprises the steps of filtration, concentration, washing, and drying.

[0028] Preferably, the amount of triazine compound C is 0.01-0.2 mol, the amount of water is 50-300 ml, and the amount of amino ester compound D is 1-1.5 times the amount of triazine compound C.

[0029] Preferably, the reaction temperature is 80-130℃, and the reaction time is 12-18h.

[0030] Preferably, after the reaction is completed, a cooling step is further included, the cooling temperature is 0-5℃, and the cooling time is 1-6h.

[0031] Preferably, the filtrate after filtration is subjected to vacuum concentration, and the vacuum concentration conditions are as follows: temperature 30-60℃, vacuum degree in the range of 1-10 kPa, and time 3-5h.

[0032] Preferably, the oil-like mixture obtained after vacuum concentration is washed with ethanol, and the number of washing times is not limited, and is preferably 1-10 times.

[0033] Preferably, the drying is preferably carried out in vacuum, the drying temperature is 30-60℃, the vacuum degree is 1-10 kPa, and the time is 10-25h.

[0034] In another aspect, the present application provides a non-silicon type defoamer prepared by the above method.

[0035] Finally, the application also provides a non-silicon defoamer in the field of extraction of scandium, and the non-silicon defoamer is mixed with an extractant solution and a scandium-containing sulfate solution to perform multi-stage countercurrent extraction.

[0036] Preferably, the total amount of the non-silicon defoamer added is 0.01-0.1 times the volume of the extractant solution;

[0037] The extractant solution is a mixture of an extractant and solvent oil, wherein the volume content of the extractant is 15-25%;

[0038] Preferably, the extractant is one or more of P204 and P507;

[0039] Preferably, the solvent oil is one or more of light white oil and kerosene;

[0040] Preferably, the conditions of the multi-stage countercurrent extraction are as follows: the extraction stage number is 3-5, the temperature is 35-55°C, and the extraction phase ratio is O:A=(1-4):1;

[0041] As a preferred scheme of the process of the application, the metal components of the scandium-containing sulfate solution are as follows in terms of the concentration of metal ions: Ni 75-100 g / L, Co 3-15 g / L, Mn 0.5-10 g / L, Sc 0.5-1.5 g / L, Mg 0.5-5 g / L, Cu 0.3-5 g / L, Zn 0-5 g / L, Fe 0-1 g / L, and Cr 0-0.5 g / L.

[0042] The application has the following beneficial effects:

[0043] The application uses a non-silicon defoamer as an additive, which contains a melamine group and has certain chemical stability and thermal stability due to its high nitrogen content, and has better environmental compatibility and good stability compared with some traditional defoamers, can effectively inhibit the generation and enrichment of the third phase in the extraction of scandium, reduce the generation of phenomena such as miscibility and emulsification, and achieve the effects of maintaining the stability of the process and improving the purity and quality of the product. DETAILED DESCRIPTION

[0044] The application will be further described in detail below in combination with examples, but the following examples are only simple examples of the application and do not represent or limit the protection scope of the application, and the protection scope of the application is subject to the claims.

[0045] Raw materials and sources:

[0046] The raw materials of the application are amino acid substance A, fatty alcohol substance B, and triazine compound C;

[0047] Wherein the amino acid A is 5-aminovaleric acid (CAS: 660-88-8, purchased from Zhengzhou Huiju Chemical Co., Ltd., purity 97%, specification 500g / bottle) or 3-aminopropanoic acid (CAS: 107-95-9, purchased from Inokai, purity 99%, specification 500g / bottle);

[0048] The fatty alcohol B is methanol (CAS: 67-56-1, purchased from Beijing Zepin Science and Technology Co., Ltd., purity 99.9%, specification 500ml / bottle) or ethanol (CAS: 64-17-5, purchased from Aldrich, purity ≥99.7%, specification 500ml / bottle);

[0049] The triazine compound C is 2-hydroxy-4.6-diamino-1.3.5-triazine (CAS: 645-92-1, purchased from Alfa Aesar (China) Chemical Co., Ltd., purity 90%, specification 1g / package) or 2-chloro-4.6-diamino-1.3.5-triazine (CAS: 3397-62-4, purchased from Shanghai Yuan Ye Biological Technology Co., Ltd., purity 95%, specification 100g / bottle).

[0050] Test method:

[0051] The structure characteristics of the synthesized defoaming agent are characterized by nuclear magnetic resonance spectroscopy, instrument model Bruker Avance III HD 600MHz nuclear magnetic resonance spectrometer, Bruker Company.

[0052] Example 1

[0053] A synthesis method of a non-silicon type defoaming agent, which is synthesized by two-step reaction of three components A, B and C:

[0054] 5-aminovaleric acid (CAS: 660-88-8) is selected as component A, purchased from Zhengzhou Huiju Chemical Co., Ltd., purity 97%, specification 500g / bottle, methanol (CAS: 67-56-1) is selected as component B, purchased from Beijing Zepin Science and Technology Co., Ltd., purity 99.9%, specification 500ml / bottle, and 2-hydroxy-4.6-diamino-1.3.5-triazine (CAS: 645-92-1) is selected as component C, purchased from Alfa Aesar (China) Chemical Co., Ltd., purity 90%, specification 1g / package.

[0055] Esterification reaction: 0.1mol 5-aminovaleric acid is added to the suspension of 0.5mol methanol and 0.1mol SOCl2 in a 0℃ water bath. After 1h of reaction, the mixture becomes a clear solution, heated to reflux at 40℃ for 1h. The mixture is cooled to 20℃, and reduced to 1kPa. The residue is suspended in 50ml n-pentane, vacuum filtered and dried at 30℃ for 16h to obtain 5-amino-1-pentanoic acid methyl ester.

[0056] Substitution reaction: 0.01 mol 2-hydroxy-4.6-diamino-1.3.5-triazine was dissolved in 50 ml water, 0.01 mol 5-amino-1-pentanoic acid methyl ester was added; the resulting mixture was heated to 80°C and refluxed for 12 h, cooled in a 0°C water bath for 1 h, then the mixture was filtered, the filtrate was concentrated under vacuum at 30°C and 1 kPa for 3 h to obtain an oily mixture, which was washed with 300 ml ethanol, and residual ethanol was removed under vacuum at 30°C and 1 kPa for 10 h to obtain a non-silicon type defoamer solid, the structure of which is shown in detail in formula 1,

[0057]

[0058] Structure of non-silicon type defoamer of formula 1 (Example 1)

[0059] The structure characteristics of the synthesized non-silicon type defoamer were characterized by nuclear magnetic resonance spectroscopy, instrument model Bruker Avance III HD 600MHz nuclear magnetic resonance spectrometer, Bruker Corporation;

[0060] NMR data: 1H NMR (500 MHz, DMSO-d6) δ 7.14 (t, J = 3.8 Hz, 1H), 6.35 (d, J = 6.1 Hz, 2H), 6.24 (d, J = 6.1 Hz, 2H), 3.63 (s, 3H), 3.42 (td, J = 6.3, 3.7 Hz, 2H), 2.33 (t, J = 7.1 Hz, 1H), 1.74 - 1.55 (m, 4H).

[0061]

Example 2

[0062] A method for synthesizing a non-silicon type defoamer, which is synthesized by two-step reaction of three components A, B and C:

[0063] 3-Aminopropanoic acid (CAS: 107-95-9) was selected as component A, purchased from Inokai, purity 99%, specification 500 g / bottle, methanol (CAS: 67-56-1) was selected as component B, purchased from Beijing Zeping Science and Technology Co., Ltd., purity 99.9%, specification 500 ml / bottle, and 2-chloro-4.6-diamino-1.3.5-triazine (CAS: 3397-62-4) was selected as component C, purchased from Shanghai Yuanye Biotechnology Co., Ltd., purity 95%, specification 100 g / bottle.

[0064] Esterification reaction: To a suspension of 2 mol of methanol and 2 mol of PCl3, 1 mol of 3-aminopropanoic acid was added in a 5 °C water bath. After 5 h of reaction, the mixture became a clear solution, and heating at 80 °C under reflux was performed for 3 h. The mixture was cooled to 35 °C, and reduced to 10 kPa. The residue was suspended in 500 ml of dichloromethane, and vacuum filtered at 100 mmHg, 50 °C for 28 h to obtain 3-amino-1-propanoic acid methyl ester.

[0065] Substitution reaction: 0.2 mol of 2-chloro-4,6-diamino-1,3,5-triazine was dissolved in 300 ml of water, and 0.3 mol of 5-amino-1-pentanoic acid methyl ester was added; the resulting mixture was heated to 130 °C under reflux for 18 h, and cooled to 5 °C in a water bath for 6 h. The mixture was then filtered, and the filtrate was concentrated at 60 °C under vacuum at 10 kPa for 5 h to obtain an oily mixture, which was washed with 1000 ml of ethanol, and residual ethanol was removed at 60 °C under vacuum at 10 kPa for 25 h to obtain a non-silicon type defoamer solid, the structure of which is shown in formula 2.

[0066]

[0067] Structure of non-silicon type defoamer of formula 2 (Example 2)

[0068] The structure of the synthesized non-silicon type defoamer was characterized using nuclear magnetic resonance spectroscopy, instrument model Bruker Avance III HD 600MHz nuclear magnetic resonance spectrometer, Bruker Corporation;

[0069] NMR data:1H NMR (500 MHz, DMSO-d6) δ 7.19 (t, J = 3.7 Hz, 1H), 6.38 (d, J = 6.1 Hz, 2H), 6.29 (d, J = 6.1 Hz, 2H), 3.86 (td, J = 6.3, 3.7 Hz, 2H), 3.63 (s, 3H), 2.67 (t, J = 6.2 Hz, 2H).

[0070]

Example 3

[0071] A method for synthesizing a non-silicon type defoamer, which is synthesized by two-step reaction of three components A, B and C:

[0072] 5-aminovaleric acid (CAS: 660-88-8) was selected as component A, purchased from Zhengzhou Huiju Chemical Co., Ltd., purity 97%, specification 500 g / bottle, ethanol (CAS: 64-17-5) was selected as component B, purchased from Aldrich, purity ≥ 99.7%, specification 500 ml / bottle, 2-chloro-4.6-diamino-1.3.5-triazine (CAS: 3397-62-4) was selected as component C, purchased from Shanghai Yuanye Bio-Technology Co., Ltd., purity 95%, specification 100 g / bottle.

[0073] Esterification reaction: 0.5 mol of 5-amino-1-pentanoic acid was added to a suspension of 1 mol of ethanol and 50 ml of SOCl2 in a 2 °C water bath. After 3 h of reaction, the mixture became a clear solution, and heating was carried out at 70 °C for 2 h. The mixture was cooled to 30 °C, and reduced to 2 kPa. The residue was suspended in 100 ml of cyclohexane, and vacuum filtered and dried at 40 °C for 26 h to obtain 5-amino-1-pentanoic acid ethyl ester.

[0074] Substitution reaction: 0.1 mol of 2-chloro-4.6-diamino-1.3.5-triazine was dissolved in 100 ml of water, and 0.12 mol of 5-amino-1-pentanoic acid methyl ester was added. The resulting mixture was heated to 95 °C and refluxed for 15 h, and then cooled in a 2 °C water bath for 5 h. The mixture was filtered, and the filtrate was concentrated at 40 °C under a vacuum of 1.5 kPa for 4 h to obtain an oily mixture, which was washed with 800 ml of ethanol. The residual ethanol was removed at 50 °C under a vacuum of 1.5 kPa for 15 h to obtain a non-silicon type defoamer solid, the structural formula of which is shown in formula 3.

[0075]

[0076] Formula 3 non-silicon type defoamer structural formula (Example 3)

[0077] The structure characteristics of the synthesized non-silicon type defoamer were characterized by nuclear magnetic resonance spectroscopy. The instrument model was Bruker Avance III HD 600MHz nuclear magnetic resonance spectrometer, Bruker Corporation.

[0078] NMR data:1H NMR (500 MHz, DMSO-d6) δ 7.14 (t, J = 3.7 Hz, 1H), 6.27 (s, 3H), 4.10 (q, J = 6.9 Hz, 2H), 3.46–3.35 (m, 2H), 2.33 (t, J = 7.0 Hz, 1H), 1.73–

[0079] 1.60 (m, 4H), 1.19 (t, J = 7.0 Hz, 3H).

[0080]

Example 4

[0081] Application of a non-silicon type defoaming agent in the field of extraction of scandium, comprising the following steps:

[0082] 1) Mix the extractant P204 with light white oil according to the volume ratio of 25:75 to obtain an extractant solution, divide the extractant solution into four groups of equal volume, numbered a, b, c, and d, wherein group a does not add an auxiliary, group b adds the non-silicon type defoaming agent in Example 1, group c adds the non-silicon type defoaming agent in Example 2, and group d adds the non-silicon type defoaming agent in Example 3, the addition ratio is 0.05 times the volume of the extractant solution, to obtain an extraction organic phase;

[0083] 2) Take four portions of the same volume of scandium-containing sulfate solution and perform one-stage multi-stage countercurrent extraction with the four groups of extraction organic phases in 1), the one-stage multi-stage countercurrent extraction conditions are: extraction stages 3, temperature 40℃, extraction phase ratio O:A = 1:1, to obtain a raffinate aqueous phase and an organic phase loaded with scandium and other metals, wherein group a has obvious third phase generation during extraction, phase separation is difficult, and the scandium extraction rate is only 80%, group b does not produce a third phase during extraction, the scandium extraction rate is 99.97%, group c does not produce a third phase during extraction, the scandium extraction rate is 99.95%, and group d also does not produce a third phase during extraction, the scandium extraction rate is 99.98%.

[0084] 3) Take the organic and aqueous phases at the phase interface during the extraction process of groups a, b, c, and d and place them in a separatory funnel, perform a shake flask experiment using a shaker, the shaker parameters are: shaking frequency 300 rpm, shaking time 5 min, and the phase separation time is recorded using a stopwatch, as shown in Table 1, the phase separation time with the addition of the defoaming agent is significantly shorter than the phase separation time without the addition of the defoaming agent.

[0085] Table 1 Evaluation of the phase separation time of the non-silicon type defoaming agent

[0086]

[0087]

[0088]

Example 5

[0089] Application of a non-silicon type defoaming agent in the field of extraction of scandium, comprising the following steps:

[0090] 1) Mix the extractant P507 with light white oil according to the volume ratio of 15:85 to obtain an extractant solution, divide the extractant solution into four groups of equal volume, numbered a, b, c, and d, wherein group a does not add an auxiliary, group b adds the non-silicon type defoaming agent in Example 1, group c adds the non-silicon type defoaming agent in Example 2, and group d adds the non-silicon type defoaming agent in Example 3, the addition ratio is 0.01 times the volume of the extractant solution, to obtain an extraction organic phase;

[0091] 2) Take four equal volumes of scandium-containing sulfate solution, respectively with the four groups of extraction organic phase in 1) to carry out one-stage multistage countercurrent extraction, one-stage multistage countercurrent extraction conditions: extraction series 5, temperature 35℃, extraction phase ratio O:A = 4:1, get raffinate water phase and organic phase loaded with scandium and other metals, wherein a group of extraction process has obvious third phase, difficult to separate, scandium extraction rate is only 75%, b group extraction process does not produce third phase, scandium extraction rate 99.96%, c group extraction process does not produce third phase, scandium extraction rate 99.92%, d group extraction process also does not produce third phase, scandium extraction rate 99.93%.

[0092] 3) Take a, b, c, d four groups of extraction process at the interface of organic and aqueous phase in separatory funnel, using shaker bottle experiment, shaker parameters: oscillation frequency 300 rpm, oscillation time 5 min, use stopwatch to record the phase separation time, see table 2, adding defoaming agent phase separation time is significantly shorter than that without adding defoaming agent.

[0093] Table 2 non-silicon type defoaming agent phase separation time evaluation

[0094] Sample Phase separation time / s No additive 129 Addition of Example 1 non-silicon type defoamer 31 Addition of Example 2 non-silicon type defoamer 33 Addition of Example 3 non-silicon type defoamer 32

[0095]

Example 6

[0096] A non-silicon type defoaming agent is applied in the field of extraction of scandium, including the following steps:

[0097] 1) Mix the extractant P204 with light white oil according to the volume ratio of 25:75 to obtain an extractant solution, and divide the extractant solution into four groups with equal volume, numbered a, b, c, d, wherein a group does not add auxiliary agent, b group adds non-silicon type defoaming agent in example 1, c group adds non-silicon type defoaming agent in example 2, d group adds non-silicon type defoaming agent in example 3, the addition ratio is 0.1 times of the volume of the extractant solution, to obtain the extraction organic phase;

[0098] 2) Take four equal volumes of scandium-containing sulfate solution, respectively with the four groups of extraction organic phase in 1) to carry out one-stage multistage countercurrent extraction, one-stage multistage countercurrent extraction conditions: extraction series 4, temperature 55℃, extraction phase ratio O:A = 2:1, get raffinate water phase and organic phase loaded with scandium and other metals, wherein a group of extraction process has obvious third phase, difficult to separate, scandium extraction rate is only 78%, b group extraction process does not produce third phase, scandium extraction rate 99.97%, c group extraction process does not produce third phase, scandium extraction rate 99.95%, d group extraction process also does not produce third phase, scandium extraction rate 99.94%.

[0099] 3) Take the organic and aqueous phases at the interface in the four groups of extraction process in the separatory funnel, use the shaker to do the shake bottle experiment, the shaker parameters: oscillation frequency 300 rpm, oscillation time 5 min, use the stopwatch to record the phase separation time, see Table 3 for details, the phase separation time with defoamer is significantly shorter than that without defoamer.

[0100] Table 3 Evaluation of phase separation time of non-silicon defoamer

[0101] Sample Phase separation time / s No additive 133 Addition of Example 1 non-silicon type defoamer 28 Addition of Example 2 non-silicon type defoamer 27 Addition of Example 3 non-silicon type defoamer 31

[0102]

Comparative Example

[0103] 1) Mix the extractant P204 with kerosene according to the volume ratio of 25:75 to obtain an extractant solution, divide the extractant solution into two groups with equal volume, numbered a and b, wherein group a adds the non-silicon defoamer in Example 1, and group b adds N-oleoyl sarcosine sodium (a common non-silicon defoamer), the addition ratio is 0.05 times the volume of the extractant solution, to obtain an extraction organic phase;

[0104] 2) Take two portions of the same volume of scandium-containing sulfate solution, and carry out one-stage multi-stage countercurrent extraction with the four groups of extraction organic phases in 1), the one-stage multi-stage countercurrent extraction conditions are: extraction stages 3, temperature 45℃, extraction phase ratio O:A = 3:1, to obtain raffinate water phase and organic phase loaded with scandium and other metals, wherein group a does not produce a third phase during extraction, the scandium extraction rate is 99.91%, and group b produces a weakly miscible third phase during extraction, the scandium extraction rate is 96.95%;

[0105] 3) Take the organic and aqueous phases at the interface in the four groups of extraction process in the separatory funnel, use the shaker to do the shake bottle experiment, the shaker parameters: oscillation frequency 300 rpm, oscillation time 5 min, use the stopwatch to record the phase separation time, see Table 3 for details, the phase separation time with defoamer is significantly shorter than that without defoamer.

[0106] Table 4 Evaluation of phase separation time of different defoamers

[0107] Sample Phase separation time / s Addition of Example 1 non-silicon type defoamer 31 Addition of N-oleoyl sarcosine sodium 55

Claims

1. A method for synthesizing a non-silicon defoamer, which is synthesized by two-step reaction of three components A, B and C; the A component is an amino acid substance; the B component is a fatty alcohol substance, and the C component is a triazine compound; the specific synthesis steps are: 1) esterification reaction of the amino acid substance and the fatty alcohol substance to generate an amino ester substance; 2) substitution reaction of the amino ester substance and the triazine compound to obtain a non-silicon defoamer containing a melamine group. The A component is one or more of 5-amino pentanoic acid, 4-amino butyric acid, 3-amino propionic acid and 6-amino hexanoic acid; and / or, the B component is one or more of methanol, ethanol and propanol; and / or, the C component is one of 2-chloro-4.6-diamino-1.3.5-s-triazine and 2-hydroxy-4.6-diamino-1.3.5-s-triazine. The specific process of the esterification reaction in step 1) is: a, adding the amino acid substance to a suspension containing the fatty alcohol substance and a catalyst to generate a mixture for reaction; b, after the reaction is completed, heating and refluxing are continued, and after the heating and refluxing are completed, post-treatment is performed to obtain the amino ester substance. In process a, the temperature of the mixture is 0-5℃, the amount of the amino acid substance is 0.1-1 mol, the amount of the fatty alcohol substance is 0.5-2 mol, the catalyst is selected from one of SOCl2 and PCl3, the amount of the catalyst is 0.1-2 mol, and the reaction time is 1-5 h; and / or, in process b, the heating and refluxing temperature is 40-80℃, and the refluxing time is 1-3 h.

2. The method of synthesis of claim 1, wherein, The specific process of the substitution reaction in step 2) is: c, dissolving the triazine compound in a solvent and adding the amino ester substance obtained in step 1); d, heating and reacting the obtained mixture, and after the reaction is completed, post-treatment is performed to obtain the non-silicon defoamer.

3. The method of synthesis according to claim 1 or 2, wherein, In process c, the amount of the triazine compound is 0.01-0.2 mol, the amount of water is 50-300 ml, and the amount of the amino ester substance is 1-1.5 times the amount of the triazine compound; and / or, in process d, the heating and reaction temperature is 80-130℃, and the reaction time is 12-18 h.

7. The non-silicon defoamer obtained by the synthesis method according to any one of claims 1-6.

8. Application of the non-silicon defoamer according to claim 7 in the field of extraction of scandium, wherein the obtained non-silicon defoamer is mixed with an extractant solution, and multi-stage countercurrent extraction is performed with a solution containing scandium sulfate.

4. The method of synthesis of claim 3, wherein, The total amount of the non-silicon defoamer added is 0.01-0.1 times the volume of the extractant solution; and / or, the extractant solution is a mixture of an extractant and solvent oil, wherein the volume content of the extractant is 15-25%; and / or, the extractant is one or more of P204 and P507; and / or, the solvent oil is one or more of light white oil and kerosene.

5. The method of synthesis of claim 1 or 2, wherein, ​ ​ ​ 6. The method of synthesis of claim 5, wherein, ​ ​ ​ 9. Use according to claim 8, wherein the compound is ###0002### ​ 10. Use according to claim 8 or 9, characterized in that, The conditions of the multi-stage countercurrent extraction are: extraction stage number 3-5, temperature 35-55 ℃, extraction phase ratio O:A=(1-4):1; and / or, the metal components of the scandium-containing sulfate solution are, in terms of the concentration of metal ions: Ni 75-100 g / L, Co 3-15 g / L, Mn 0.5-10 g / L, Sc 0.5-1.5 g / L, Mg 0.5-5 g / L, Cu 0.3-5 g / L, Zn 0-5 g / L, Fe 0-1 g / L, Cr 0-0.5 g / L.

Images