CN114057171B - Potassium phosphate salt purification process - Google Patents
Potassium phosphate salt purification process Download PDFInfo
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- CN114057171B CN114057171B CN202111438793.1A CN202111438793A CN114057171B CN 114057171 B CN114057171 B CN 114057171B CN 202111438793 A CN202111438793 A CN 202111438793A CN 114057171 B CN114057171 B CN 114057171B
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
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Abstract
The invention discloses a potassium phosphate purification process, which relates to the technical field of potassium phosphate purification, and specifically comprises the following steps: s1, weighing a proper amount of D751 resin, performing acid-base treatment to change the D751 resin into an ammonium form, and loading the D751 resin into an ion exchange column after secondary cleaning; s2, weighing a proper amount of wet-prepared K 3 PO 4 Dissolving with secondary water, pouring into an ion exchange column, controlling the flow rate to enable the solution to flow out, keeping the inflow rate consistent with the outflow rate, ensuring that the liquid level in the ion exchange column is kept unchanged, and collecting the effluent liquid by using a volumetric flask; the invention adopts D751 resin to K 3 PO 4 Purification was carried out with respect to the other strongly acidic resins, D751 resin to K 3 PO 4 The transition metal ions in the solution have stronger adsorption effect, so that the purity of the potassium phosphate salt is higher, impurities and fine particles on the surface of the D751 resin can be effectively removed, the D751 resin is prevented from being influenced in the process of purifying the potassium phosphate salt, and the purification degree of the potassium phosphate salt is further improved.
Description
Technical Field
The invention relates to the technical field of potassium phosphate purification, in particular to a potassium phosphate purification process.
Background
Potassium phosphate salt (KH) 2 PO 4 ，K 2 HPO 4 Or K 3 PO 4 ) Is an important inorganic chemical product and has wide application in various fields such as industry, agriculture, food industry and the like. At present, potassium phosphate salt produced industrially has various ways such as neutralization method, double decomposition and the like, and different production ways have advantages and disadvantages. Compared with other methods, the method has the advantages of common application, mature technology, short process flow, high product quality, less equipment investment and the like in the neutralization industry. However, some enterprises of the traditional process still adopt hot-process phosphoric acid with higher cost as a reaction raw material, and some enterprises adopt wet-process phosphoric acid, but impurities cannot be well removed in the process, so that on one hand, the purity of the generated phosphate is not high, the product is not competitive, and on the other hand, the filtrate contains a large amount of impurity components. The process is complicated due to the treatment of the filtrateThe treatment cost is high, the potassium phosphate is directly discharged into the environment to cause great pollution harm under most conditions, and a neutralization method still occupies a great amount in the production process of potassium phosphate in China, particularly K 3 PO 4 The production effect is not ideal by adopting other processes, so that the improvement and optimization of the process, the improvement of the product purity, the reduction of the energy consumption and the reduction of the emission pollution of byproducts have important significance.
Through search, chinese patent No. CN201510486383.2 discloses a method and equipment for preparing potassium phosphate by using wet-process phosphoric acid, although the potassium phosphate preparation and purification process is optimally designed, the high-quality potassium phosphate is obtained, meanwhile, impurity components are recovered to form byproducts, the process flow is simplified, the energy consumption is reduced, and the production cost is reduced. However, the existing potassium phosphate salt purification process is used for K 3 PO 4 The poor adsorption effect of the transition metal ions in the solution leads to low purity of the potassium phosphate salt, and the purification process cannot pretreat the purified substances well, which leads to the influence on the purification degree of the potassium phosphate salt. To this end, we propose a process for the purification of potassium phosphate salts.
Disclosure of Invention
The invention aims to solve the problem that the prior potassium phosphate salt purification process in the prior art is used for purifying K 3 PO 4 The method has the defects that the purity of the potassium phosphate is low due to poor adsorption effect of transition metal ions in the solution, and the purified substances cannot be well pretreated in the purification process, so that the purification degree of the potassium phosphate is influenced.
In order to achieve the purpose, the invention adopts the following technical scheme:
a potassium phosphate purification process comprises the following specific steps:
s1, weighing a proper amount of D751 resin, carrying out acid-base treatment to change the D751 resin into an ammonium form, and loading the resin into an ion exchange column after secondary cleaning;
s2, weighing a proper amount of wet-prepared K 3 PO 4 Dissolving with secondary water, pouring into ion exchange column, and controllingControlling the flow rate to enable the solution to flow out, keeping the inflow rate consistent with the outflow rate, ensuring that the liquid level in the ion exchange column is kept unchanged, and collecting the effluent liquid by using a volumetric flask;
s3, stopping passing through the column after the solution is basically collected, and fixing the volume of the solution;
s4, measuring the content of the transition metal ions in the solution by using an inductively coupled plasma emission spectrometry, judging whether the content of the transition metal ions is less than or equal to 5ppm, and if so, completing K 3 PO 4 If the concentration is more than 5ppm, performing step S5;
and S5, dissolving the solution with the constant volume in the step S4 with secondary water, purifying the solution through a D751 resin layer, recycling the effluent liquid to a volumetric flask, stopping passing through the column after the solution is basically collected, fixing the volume of the solution, synchronously measuring the content of transition metal ions in the solution in the step S4, and sequentially circulating.
As a further scheme of the invention: the column diameter of the ion exchange column in the step S1 is 4.6cm, and the column height is 1.6m; in the step S2, the flow rate is controlled to be 2-3mL/min, and the capacity of the volumetric flask is controlled to be 80-120mL.
As a further scheme of the invention: the solution in the step S3 has the constant volume for 5-8h, and the transition metal ions in the step S4 mainly comprise Fe 3+ 、Co 2+ 、Ni 2+ 、Cu 2+ With Mn 2+ 。
As a further scheme of the invention: the specific steps of the acid-base treatment of the resin D751 in the step S1 are as follows:
SS1, soaking the D751 resin in water to fully swell the resin, and removing impurities and fine particles on the surface of the D751 resin;
SS2, soaking the D751 resin for 12-16h by using 80% ethanol, and washing by using secondary water;
SS3, soaking the D751 resin by using high-purity hydrochloric acid, and washing with secondary water until the pH value is 6-7;
and SS4, finally soaking the D751 resin by using high-purity ammonia water, washing the D751 resin to be neutral by using water for the second time, and repeating the steps of SS3 and SS4 to change the D751 resin into an ammonium form.
As a further scheme of the invention: the concentration range of the high-purity hydrochloric acid in the step SS3 is 4-6mol/L, and the soaking time is 6-7h.
As a further scheme of the invention: and D751 resin is soaked in high-purity ammonia water in the step SS4 for 2-3h.
As a further scheme of the invention: k prepared by wet method in step S2 3 PO 4 The method comprises the following specific steps:
a. adding wet-process phosphoric acid into an extracting agent, mixing and oscillating, standing for layering, and separating liquid to obtain a first organic phase and a first water phase;
b. adding K into the first organic phase in the step a 2 CO 3 Powder or K 2 CO 3 Mixing and oscillating the solution, standing for layering, and separating to obtain a second organic phase and a second water phase;
c. adding K into the second aqueous phase in the step b 2 CO 3 And (3) stirring the powder, standing the powder, and filtering and drying crystals after potassium phosphate salt crystals are separated out to obtain the potassium phosphate salt.
As a further scheme of the invention: in the step a, the extracting agent is one of cyclohexylamine, 2, 4-dimethylcyclohexane and cyclohexanol.
As a further scheme of the invention: in the step a, the volume ratio of the wet-process phosphoric acid to the extracting agent is 1 to 3.5, the mixing and oscillation time is 25 to 50min, and the standing and layering time is 40 to 60min.
As a further scheme of the invention: and c, mixing and oscillating in the step b for 26-35min, and standing for 30-45min for layering.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the purification process, the content of transition metal ions in a solution is measured through an inductively coupled plasma emission spectrometry, the purification degree of potassium phosphate is judged according to the content of the transition metal ions, if the content of the potassium phosphate cannot reach the standard, the solution with constant volume is purified again through a D751 resin layer, an effluent liquid is recycled to a volumetric flask, and the process is circulated in sequence; meanwhile, the invention adopts D751 resin pair K 3 PO 4 Purification is carried out, D751 resin is opposite to K of other strong acid resins 3 PO 4 In solutionThe transition metal ions have stronger adsorption effect, so that the purity of the potassium phosphate is higher, the process flow of the invention is short, the involved reaction separation process is simple, no waste is discharged in the process flow, and the process flow is clean and pollution-free;
2. according to the method, before the potassium phosphate salt is purified, the D751 resin is soaked by water, ethanol, high-purity hydrochloric acid and high-purity ammonia water respectively, so that impurities and fine particles on the surface of the D751 resin can be effectively removed; among them, the D751 resin can be efficiently changed into an ammonium form by repeatedly immersing the D751 resin with high-purity hydrochloric acid and high-purity ammonia water, and the D751 resin can be efficiently treated to prevent the D751 resin from being affected by a process for purifying a potassium phosphate salt, thereby improving the purification degree of the potassium phosphate salt.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
Fig. 1 is a flow chart of a potassium phosphate salt purification process proposed by the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
Comparative example
Referring to fig. 1, a potassium phosphate salt purification process specifically comprises the following steps:
weighing a proper amount of D751 resin, carrying out acid-base treatment to change the D751 resin into an ammonium form, carrying out secondary cleaning, and then loading the resin into an ion exchange column;
in the present example, the column diameter of the ion exchange column was 4.6cm, and the column height was 1.6m; the flow rate is controlled to be 2-3mL/min, and the volume of the volumetric flask is controlled to be 80-120mL.
Weighing proper amount of wet-prepared K 3 PO 4 Dissolving with secondary water, pouring into an ion exchange column, controlling the flow rate to enable the solution to flow out, keeping the inflow rate consistent with the outflow rate, ensuring that the liquid level in the ion exchange column is kept unchanged, and collecting the effluent liquid by using a volumetric flask;
it needs to be further explained that the specific process of the K3PO4 prepared by the wet method is as follows: a. adding wet-process phosphoric acid into an extracting agent, mixing and oscillating, standing for layering, and separating to obtain a first organic phase and a first water phase; b. adding K2CO3 powder or K2CO3 solution into the first organic phase, mixing and oscillating, standing for layering, and separating to obtain a second organic phase and a second water phase; c. and adding K2CO3 powder into the second water phase, stirring, standing, filtering and drying crystals after potassium phosphate salt crystals are separated out, and thus obtaining the potassium phosphate salt.
Stopping passing the column after the solution is basically collected, and fixing the volume of the solution for 5-8h;
in the embodiment, the extracting agent is one of cyclohexylamine, 2, 4-dimethylcyclohexane and cyclohexanol; the volume ratio of the wet-process phosphoric acid to the extracting agent is 1-1.5, the mixing and oscillation time is 25-50min, and the standing and layering time is 40-60min;
mixing and oscillating for 26-35min, and standing for 30-45min.
Example 1
Referring to fig. 1, a process for purifying potassium phosphate salt includes the following specific steps:
weighing a proper amount of D751 resin, performing acid-base treatment to change the D751 resin into an ammonium form, and loading the D751 resin into an ion exchange column after secondary cleaning;
it should be further noted that the specific steps of the acid-base treatment of the D751 resin are as follows:
SS1, soaking the D751 resin in water to fully swell the D751 resin, and removing impurities and fine particles on the surface of the D751 resin;
SS2, soaking the D751 resin for 12-16h by using 80% ethanol, and washing by using secondary water;
SS3, soaking the D751 resin by using high-purity hydrochloric acid, and washing with secondary water until the pH value is 6-7;
and SS4, finally soaking the D751 resin by using high-purity ammonia water, washing the D751 resin to be neutral by using water for the second time, and repeating the steps of SS3 and SS4 to change the D751 resin into an ammonium form.
Specifically, before purifying the potassium phosphate salt, the D751 resin is soaked by water, ethanol, high-purity hydrochloric acid and high-purity ammonia water respectively, so that impurities and fine particles on the surface of the D751 resin can be effectively removed, wherein the D751 resin can be effectively changed into an ammonium form by repeatedly soaking the D751 resin by the high-purity hydrochloric acid and the high-purity ammonia water, the D751 resin can be effectively prevented from being influenced in the process of purifying the potassium phosphate salt by treating the D751 resin, and the purification degree of the potassium phosphate salt is further improved.
In the present example, the diameter of the ion exchange column was 4.6cm, and the height of the column was 1.6m; controlling the flow rate to be 2-3mL/min, the capacity of a volumetric flask to be 80-120mL, the concentration range of the high-purity hydrochloric acid to be 4-6mol/L, and the soaking time to be 6-7h; soaking the D751 resin in high-purity ammonia for 2-3h.
Weighing appropriate amount of wet prepared K 3 PO 4 Dissolving with secondary water, pouring into an ion exchange column, controlling the flow rate to enable the solution to flow out, keeping the inflow rate consistent with the outflow rate, ensuring that the liquid level in the ion exchange column is kept unchanged, and collecting the effluent liquid by using a volumetric flask;
it is further stated that the wet-process prepared K 3 PO 4 The specific process is as follows: a. adding wet-process phosphoric acid into an extracting agent, mixing and oscillating, standing for layering, and separating to obtain a first organic phase and a first water phase; b. adding K into the first organic phase 2 CO 3 Powder or K 2 CO 3 Mixing and oscillating the solution, standing for layering, and separating liquid to obtain a second organic phase and a second water phase; c. will be the secondAdding K into water phase 2 CO 3 And stirring and standing the powder, filtering and drying crystals after potassium phosphate salt crystals are separated out to obtain the potassium phosphate salt.
Stopping passing the column after the solution is basically collected, and fixing the volume of the solution for 5-8h;
in the embodiment, the extracting agent is one of cyclohexylamine, 2, 4-dimethylcyclohexane and cyclohexanol; the volume ratio of the wet-process phosphoric acid to the extracting agent is 1-1.5, the mixing and oscillation time is 25-50min, and the standing and layering time is 40-60min;
mixing and oscillating for 26-35min, and standing for 30-45min.
Example 2
Referring to fig. 1, a process for purifying potassium phosphate salt includes the following specific steps:
weighing a proper amount of D751 resin, carrying out acid-base treatment to change the D751 resin into an ammonium form, carrying out secondary cleaning, and then loading the resin into an ion exchange column;
in the present example, the column diameter of the ion exchange column was 4.6cm, and the column height was 1.6m; the flow rate is controlled to be 2-3mL/min, and the volume of the volumetric flask is controlled to be 80-120mL.
Weighing proper amount of wet-prepared K 3 PO 4 Dissolving with secondary water, pouring into an ion exchange column, controlling the flow rate to enable the solution to flow out, keeping the inflow rate consistent with the outflow rate, ensuring that the liquid level in the ion exchange column is kept unchanged, and collecting the effluent liquid by using a volumetric flask;
it is further stated that the wet-process prepared K 3 PO 4 The specific process is as follows: a. adding wet-process phosphoric acid into an extracting agent, mixing and oscillating, standing for layering, and separating liquid to obtain a first organic phase and a first water phase; b. adding K to the first organic phase 2 CO 3 Powder or K 2 CO 3 Mixing and oscillating the solution, standing for layering, and separating to obtain a second organic phase and a second water phase; c. adding K into the second aqueous phase 2 CO 3 And stirring and standing the powder, filtering and drying crystals after potassium phosphate salt crystals are separated out to obtain the potassium phosphate salt.
Stopping passing through the column after the solution is basically collected, and fixing the volume of the solution for 5-8h;
measuring the content of transition metal ions in the solution by inductively coupled plasma emission spectrometry, and judging whether the content of the transition metal ions is less than or equal to 5ppm, if so, completing K 3 PO 4 If the concentration is more than 5ppm, carrying out the next step;
wherein the transition metal ion mainly comprises Fe 3+ 、Co 2+ 、Ni 2+ 、Cu 2+ With Mn 2+ ；
And (3) dissolving the solution with constant volume in secondary water, purifying the solution through a D751 resin layer, recycling the effluent liquid into a volumetric flask, stopping passing through the column after the solution is basically collected, fixing the volume of the solution, measuring the content of transition metal ions in the solution, and circulating in sequence.
In the embodiment, the extracting agent is one of cyclohexylamine, 2, 4-dimethylcyclohexane and cyclohexanol; the volume ratio of the wet-process phosphoric acid to the extracting agent is 1;
mixing and oscillating for 26-35min, and standing for 30-45min.
Example 3
Referring to fig. 1, a process for purifying potassium phosphate salt includes the following specific steps:
weighing a proper amount of D751 resin, carrying out acid-base treatment to change the D751 resin into an ammonium form, carrying out secondary cleaning, and then loading the resin into an ion exchange column;
it is further illustrated that the specific steps of the acid-base treatment of the D751 resin are as follows:
SS1, soaking the D751 resin in water to fully swell the D751 resin, and removing impurities and fine particles on the surface of the D751 resin;
SS2, soaking the D751 resin for 12-16h by using 80% ethanol, and washing by using secondary water;
SS3, soaking the D751 resin with high-purity hydrochloric acid, and washing with secondary water until the pH value is 6-7;
and SS4, finally soaking the D751 resin by using high-purity ammonia water, washing the D751 resin to be neutral by using water for the second time, and repeating the steps of SS3 and SS4 to change the D751 resin into an ammonium form.
Specifically, before purifying the potassium phosphate salt, the D751 resin is soaked by water, ethanol, high-purity hydrochloric acid and high-purity ammonia water respectively, so that impurities and fine particles on the surface of the D751 resin can be effectively removed, wherein the D751 resin can be effectively changed into an ammonium form by repeatedly soaking the D751 resin by the high-purity hydrochloric acid and the high-purity ammonia water, the D751 resin can be effectively prevented from being influenced in the process of purifying the potassium phosphate salt by treating the D751 resin, and the purification degree of the potassium phosphate salt is further improved.
In the present example, the diameter of the ion exchange column was 4.6cm, and the height of the column was 1.6m; controlling the flow rate to be 2-3mL/min, the capacity of a volumetric flask to be 80-120mL, the concentration range of the high-purity hydrochloric acid to be 4-6mol/L, and the soaking time to be 6-7h; soaking the D751 resin in high-purity ammonia for 2-3h.
Weighing appropriate amount of wet prepared K 3 PO 4 Dissolving with secondary water, pouring into an ion exchange column, controlling the flow rate to enable the solution to flow out, keeping the inflow rate consistent with the outflow rate, ensuring that the liquid level in the ion exchange column is kept unchanged, and collecting the effluent liquid by using a volumetric flask;
it is further stated that the wet-process prepared K 3 PO 4 The specific process is as follows: a. adding wet-process phosphoric acid into an extracting agent, mixing and oscillating, standing for layering, and separating liquid to obtain a first organic phase and a first water phase; b. adding K to the first organic phase 2 CO 3 Powder or K 2 CO 3 Mixing and oscillating the solution, standing for layering, and separating liquid to obtain a second organic phase and a second water phase; c. adding K into the second aqueous phase 2 CO 3 And stirring and standing the powder, filtering and drying crystals after potassium phosphate salt crystals are separated out to obtain the potassium phosphate salt.
Stopping passing through the column after the solution is basically collected, and fixing the volume of the solution for 5-8h;
measuring the content of transition metal ions in the solution by inductively coupled plasma emission spectrometry, and judgingWhether the content of transition metal ions is less than or equal to 5ppm, if so, K is completed 3 PO 4 If the concentration is more than 5ppm, carrying out the next step;
wherein the transition metal ion mainly comprises Fe 3+ 、Co 2+ 、Ni 2+ 、Cu 2+ With Mn 2+ ；
And (3) dissolving the solution with constant volume by secondary water, purifying the solution in a D751 resin layer, recovering the effluent liquid to a volumetric flask, stopping passing through the column after the solution is basically collected, fixing the volume of the solution, measuring the content of transition metal ions in the solution, and circulating the solution in sequence.
In the embodiment, the extracting agent is one of cyclohexylamine, 2, 4-dimethylcyclohexane and cyclohexanol; the volume ratio of the wet-process phosphoric acid to the extracting agent is 1-1.5, the mixing and oscillation time is 25-50min, and the standing and layering time is 40-60min;
mixing and oscillating for 26-35min, and standing for 30-45min.
In summary, by comparing the comparative examples with examples 1 to 3, it can be seen that: according to the purification process, the content of transition metal ions in a solution is measured through an inductively coupled plasma emission spectrometry, the purification degree of potassium phosphate is judged according to the content of the transition metal ions, if the content of the transition metal ions does not reach the standard, the solution with constant volume is purified again through a D751 resin layer, and an effluent liquid is recovered to a volumetric flask and is sequentially circulated; meanwhile, the invention adopts D751 resin pair K 3 PO 4 Purification was carried out with respect to the other strongly acidic resins, D751 resin to K 3 PO 4 The transition metal ions in the solution have stronger adsorption effect, so that the purity of the potassium phosphate is higher, the process flow is short, the involved reaction separation process is simple, no waste is discharged in the process flow, and the process flow is clean and pollution-free; and before purifying the potassium phosphate salt, the D751 resin is respectively soaked by water, ethanol, high-purity hydrochloric acid and high-purity ammonia water, so that impurities and fine particles on the surface of the D751 resin can be effectively removed, wherein the D751 resin can be effectively changed into an ammonium form by repeatedly soaking the D751 resin by using the high-purity hydrochloric acid and the high-purity ammonia water, and the D751 resin is further subjected to the treatmentThe treatment can effectively prevent the D751 resin from influencing the process of purifying the potassium phosphate salt, thereby improving the purification degree of the potassium phosphate salt.
The process flow for purifying the potassium phosphate salt is as follows: firstly, soaking the D751 resin by water to fully swell the D751 resin, and removing impurities and fine particles on the surface of the D751 resin. The D751 resin was then soaked with 80% ethanol for 12-16h and washed with secondary water. And then soaking the D751 resin for 6-7h by using 3.5-4.5mol/L high-purity hydrochloric acid, washing the D751 resin for the second time until the pH value is 6-7, soaking the D751 resin for 2-3h by using high-purity ammonia water, washing the D751 resin for the second time until the D751 resin is neutral, and repeating the steps of SS3 and SS4 to change the D751 resin into an ammonium form, thereby completing the pretreatment of the D751 resin. And secondly, adding wet-process phosphoric acid into an extracting agent, mixing and oscillating, standing for layering, and separating to obtain a first organic phase and a first water phase. Subsequently adding K to the first organic phase 2 CO 3 Powder or K 2 CO 3 And mixing and oscillating the solution, standing for layering, and separating to obtain a second organic phase and a second water phase. Then adding K to the second aqueous phase 2 CO 3 And (3) stirring the powder, standing the powder, filtering and drying crystals after potassium phosphate crystals are separated out to obtain potassium phosphate, and finally, cleaning the pretreated D751 resin for the second time and then loading the resin into an ion exchange column. And then weighing a proper amount of potassium phosphate prepared by a wet method, dissolving the potassium phosphate with secondary water, pouring the solution into an ion exchange column, controlling the flow rate to enable the solution to flow out, keeping the inflow rate consistent with the outflow rate, ensuring that the liquid level in the ion exchange column is kept unchanged, and collecting the effluent liquid by using a volumetric flask. And stopping passing through the column after the solution is basically collected, fixing the volume of the solution, and measuring the content of the transition metal ions in the solution by using an inductively coupled plasma emission spectrometry. If the content of transition metal ions is less than or equal to 5ppm, K is completed 3 PO 4 And (4) purifying. And if the volume of the solution is more than 5ppm, dissolving the solution with constant volume by secondary water, purifying the solution by a D751 resin layer, recovering the effluent liquid to a volumetric flask, stopping passing through the column after the solution is basically collected, keeping the volume of the solution constant, and circulating the solution in sequence to finish the purification of the potassium phosphate.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The potassium phosphate purification process is characterized by comprising the following specific steps:
s1, weighing a proper amount of D751 resin, performing acid-base treatment to change the D751 resin into an ammonium form, and loading the D751 resin into an ion exchange column after secondary cleaning;
s2, weighing a proper amount of wet-prepared K 3 PO 4 Dissolving with secondary water, pouring into an ion exchange column, controlling the flow rate to enable the solution to flow out, keeping the inflow rate consistent with the outflow rate, ensuring that the liquid level in the ion exchange column is kept unchanged, and collecting the effluent liquid by using a volumetric flask;
s3, stopping column passing after the solution is basically collected, and fixing the volume of the solution;
s4, measuring the content of the transition metal ions in the solution by using an inductively coupled plasma emission spectrometry, judging whether the content of the transition metal ions is less than or equal to 5ppm, and if so, completing K 3 PO 4 If the concentration is more than 5ppm, performing step S5;
and S5, dissolving the solution with the constant volume in the step S4 with secondary water, purifying the solution through a D751 resin layer, recycling the effluent liquid to a volumetric flask, stopping passing through the column after the solution is basically collected, fixing the volume of the solution, synchronously measuring the content of transition metal ions in the solution in the step S4, and sequentially circulating.
2. The process for purifying a potassium phosphate salt according to claim 1, wherein the column diameter of the ion exchange column in step S1 is 4.6cm, and the column height is 1.6m; in the step S2, the flow rate is controlled to be 2-3mL/min, and the capacity of the volumetric flask is controlled to be 80-120mL.
3. The process of claim 1 for purifying potassium phosphate salt, wherein the potassium phosphate salt is purified by the process of claim 1The solution volume fixing time in the step S3 is 5-8h, and the transition metal ions mainly comprise Fe in the step S4 3+ 、Co 2+ 、Ni 2+ 、Cu 2+ With Mn 2+ 。
4. The purification process of potassium phosphate salt according to claim 1, characterized in that the specific steps of acid-base treatment of the resin D751 in the step S1 are as follows:
SS1, soaking the D751 resin in water to fully swell the D751 resin, and removing impurities and fine particles on the surface of the D751 resin;
SS2, soaking the D751 resin for 12-16h by using 80% ethanol, and washing by using secondary water;
SS3, soaking the D751 resin by using high-purity hydrochloric acid, and washing with secondary water until the pH value is 6-7;
and SS4, finally soaking the D751 resin by using high-purity ammonia water, washing the D751 resin to be neutral by using water for the second time, and repeating the steps of SS3 and SS4 to change the D751 resin into an ammonium form.
5. The process for purifying potassium phosphate salt according to claim 4, wherein the concentration of the high-purity hydrochloric acid in step SS3 is in the range of 4 to 6mol/L, and the soaking time is 6 to 7 hours.
6. The purification process of potassium phosphate salt according to claim 4, wherein the D751 resin is soaked in the high-purity ammonia water in the step SS4 for 2-3h.
7. The process for purifying potassium phosphate salt according to claim 1, wherein the wet-prepared K in step S2 3 PO 4 The method comprises the following specific steps:
a. adding wet-process phosphoric acid into an extracting agent, mixing and oscillating, standing for layering, and separating liquid to obtain a first organic phase and a first water phase;
b. adding K into the first organic phase in the step a 2 CO 3 Powder or K 2 CO 3 Mixing and oscillating the solution, standing for layering, and separating liquid to obtain a second organic phase and a second water phase;
c. adding K into the second water phase in the step b 2 CO 3 And (3) stirring the powder, standing the powder, and filtering and drying crystals after potassium phosphate salt crystals are separated out to obtain the potassium phosphate salt.
8. The process of claim 7, wherein the extraction agent in step a is one of cyclohexylamine, 2, 4-dimethylcyclohexane and cyclohexanol.
9. The process for purifying potassium phosphate salt according to claim 7, wherein the volume ratio of the wet-process phosphoric acid to the extracting agent in the step a is 1.
10. The process for purifying potassium phosphate salt according to claim 7, wherein the mixing and shaking time in the step b is 26-35min, and the standing and layering time is 30-45min.
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