CN110371939B - Preparation method of diammonium phosphate based on phosphoric acid extraction spent acid - Google Patents
Preparation method of diammonium phosphate based on phosphoric acid extraction spent acid Download PDFInfo
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- CN110371939B CN110371939B CN201910684680.6A CN201910684680A CN110371939B CN 110371939 B CN110371939 B CN 110371939B CN 201910684680 A CN201910684680 A CN 201910684680A CN 110371939 B CN110371939 B CN 110371939B
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/234—Purification; Stabilisation; Concentration
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Abstract
The invention relates to a preparation method of diammonium phosphate based on phosphoric acid extraction spent acid. The technical scheme is as follows: adding water into the phosphoric acid raffinate according to the mass ratio of the phosphoric acid raffinate to the water of 1: 0.1-0.3, and stirring for 0.5-1 h to obtain diluted phosphoric acid raffinate; adding urea into the diluted phosphoric acid raffinate acid according to the mass ratio of (0.5-2): 1 of urea to the diluted phosphoric acid raffinate acid, stirring at 70-100 ℃ until the pH value is 6-7, and carrying out solid-liquid separation to obtain purified phosphoric acid raffinate acid and impurity-removed slag; washing the impurity-removed slag with water to obtain washed impurity-removed slag and washing water; the washing water is returned to the step I for diluting phosphoric acid raffinate; concentrating the purified phosphoric acid raffinate to P 2 O 5 The content of the diammonium phosphate is 40-50 wt%, and then the diammonium phosphate is introduced into a tubular reactor, and the neutralization degree is controlled to be 1.8-2.0, so that diammonium phosphate based on phosphoric acid raffinate acid is obtained. The invention has the characteristics of good operating environment, easy filtration, low phosphorus loss rate in the impurity removal process and no introduction of new impurities.
Description
Technical Field
The invention belongs to the technical field of phosphoric acid extraction spent acid. In particular to a preparation method of diammonium phosphate based on phosphoric acid extraction spent acid.
Background
The wet-process phosphoric acid production has low energy consumption and strong raw material adaptability, and is widely applied to the preparation of different phosphorus products. However, in the wet extraction process, a large amount of impurities such as Fe, Al, Mg and the like enter the leaching solution along with phosphorus, so that the phosphorus and the impurity ions in the subsequent process are difficult to separate. In recent years, the solvent extraction process in the wet-process production of phosphoric acid is widely applied to the preparation of high-purity phosphoric acid due to the advantages of high efficiency and good selectivity. Although the solvent extraction process has significant economic benefits, the following two main problems still exist: firstly, phosphorus is extracted and impurity ions are enriched in the extraction process, the viscosity of phosphoric acid raffinate is very high, a large amount of colloidal precipitates are generated, and the filtration is very difficult; secondly, phosphoric acid raffinate still contains phosphorus with a certain concentration, and is commonly used for producing agricultural monoammonium phosphate or diammonium phosphate, but the content of impurity ions such as Fe, Al, Mg and the like is very high, so that the purity of phosphorus products prepared by the subsequent process cannot reach the standard.
"method for preparing industrial grade monoammonium phosphate by twice-neutralization raffinate" (CN 103896232A) patent technology and kui et al adopt ammonia gas twice-neutralization method to treat phosphoric acid raffinate (kui et al. process optimization for preparing industrial grade monoammonium phosphate by raffinate [ J ], chemical and biological engineering, 2015, 32(08), 63-66), and finally adopt crystallization method to prepare industrial grade monoammonium phosphate: firstly, diluting high-viscosity raffinate acid; then, carrying out primary ammonia neutralization on the diluted phosphoric acid extraction spent acid, wherein the end point pH of the primary ammonia neutralization is 3.4-3.6, and filtering after curing; then carrying out secondary ammonia neutralization, wherein the final pH value of the secondary ammonia neutralization is 4.4-4.6, and filtering after curing; finally, the monoammonium phosphate is prepared by adopting a concentration crystallization method. The process adopts the conventional neutralizer-ammonia gas to treat phosphoric acid raffinate, has good impurity removal effect, but still has the following three problems: firstly, a large amount of colloidal precipitate generated in the impurity removal process is difficult to filter; secondly, the phosphorus loss is large and generally reaches 25-30%; thirdly, ammonia is adopted for impurity removal, the escape of ammonia from the reactor is difficult to avoid in the operation process, and the operation environment of a laboratory and an industrial field is poor.
A process for preparing industrial monoammonium phosphate and coproducing fertilizer-grade monoammonium phosphate from raffinate acid (CN 102674284A) comprises removing impurities by ammonia precipitation under the action of silicon fluoride and ammonium fluoride, and preparing monoammonium phosphate from purified raffinate acid. The process introduces fluoride as a precipitant to remove impurities, but introduces new impurity fluorine while adding fluoride ions to remove impurities. In addition, the process has the disadvantages of large phosphorus loss, poor operating environment, difficult filtration of colloidal precipitate and difficult recovery of phosphorus.
The patent of "method for producing granular monoammonium phosphate by using raffinate" (CN 101891504A) is a technology for mixing high-concentration wet-process phosphoric acid with phosphoric acid raffinate to reduce the content of impurity ions in the phosphoric acid raffinate, and finally preparing qualified monoammonium phosphate. The process has great limitation on raw materials, and when the content of impurity ions in the phosphoric acid raffinate is increased, the amount of wet-process phosphoric acid needing to be added is also increased, so that a great amount of wet-process phosphoric acid with high added value is used for preparing agricultural monoammonium phosphate, and the production cost is high.
The patent of "method for producing diammonium phosphate by using raffinate acid of purified phosphoric acid" (CN 101613094A) is characterized by that firstly, high-concentration wet-process phosphoric acid and phosphoric acid raffinate acid are mixed according to a certain proportion, and then a surfactant is added into the above-mentioned mixture so as to raise the fluidity of mixed acid and reduce viscosity. And then ammonia is used for neutralizing the complex acid according to a conventional method to prepare the diammonium phosphate. The process adds a surfactant to wet-process phosphoric acid, but the surfactant only has the effects of reducing viscosity and enabling precipitates to be filtered more easily, and impurity ions cannot be removed.
In conclusion, the existing phosphoric acid extraction spent acid treatment technology mainly has the technical defects of poor operation environment, difficult filtration of precipitates, high phosphorus loss rate, introduction of new impurities and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide a preparation method of diammonium phosphate based on phosphoric acid raffinate acid, which has the advantages of good operating environment, easy filtration of precipitate, low phosphorus loss rate and no introduction of new impurities.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following specific steps:
step one, dilution
Adding water into the phosphoric acid raffinate according to the mass ratio of 1: 0.1-0.3, and stirring for 0.5-1 h at normal temperature to obtain diluted phosphoric acid raffinate.
Step two, precipitation
Adding urea into the diluted phosphoric acid raffinate acid according to the mass ratio of urea to the diluted phosphoric acid raffinate acid of (0.5-2): 1, stirring at 70-100 ℃ until the pH value is 6-7, and carrying out solid-liquid separation to obtain purified phosphoric acid extract raffinate acid and impurity-removed slag.
Step three, washing
Washing the impurity-removed slag by water to obtain washed impurity-removed slag and washing water; and returning the washing water to the first step for diluting the phosphoric acid raffinate acid.
Step four, preparing diammonium phosphate
Concentrating the purified phosphoric acid raffinate to P 2 O 5 The content of the diammonium phosphate is 40-50 wt%, and then the diammonium phosphate is introduced into a tubular reactor, and the neutralization degree is controlled to be 1.8-2.0, so that diammonium phosphate based on phosphoric acid raffinate acid is obtained.
The phosphoric acid raffinate acid: p 2 O 5 Content (wt.)>35 wt%, MgO content of 2-8 wt%, Al 2 O 3 4-8 wt% of Fe 2 O 3 0.5-3 wt% of CaO, and<0.05wt％，K 2 content of O<0.1wt％，Na 2 Content of O<1.5 wt%, the solid content is 4-8 wt%, and the pH value is less than-0.8; the density of the phosphoric acid raffinate acid clear liquid is more than 1.6g/cm 3 。
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
(1) the urea is added at one time, so that the method has a good removing effect on various metal ions, wherein the impurity removal rate of iron and aluminum is over 98 percent, and the impurity removal rate of magnesium is over 90 percent;
(2) the urea is used as a slow-release precipitator, so that the occurrence of coprecipitation can be effectively prevented, iron ions, aluminum ions and magnesium ions in phosphoric acid raffinate are removed in a targeted manner, the inclusion of phosphorus is prevented, the generated precipitate is powdery, the generation of colloidal precipitate in the existing ammonia water purification process is avoided, and the loss rate of phosphorus can be reduced to be below 5%.
In the invention, the urea can slowly release ammonia gas when heated to above 60 ℃:
CO(NH 2 ) 2 +H 2 O→CO 2 ↑+2NH 3
NH 3 +H 2 O→NH 4 + +OH -
NH product obtained by urea hydrothermal decomposition 4 + Is a reactant for the subsequent preparation of ammonium phosphate salt products, and OH is generated by the reaction - It helps to raise the pH of the solution and eventually reaches the optimum pH range for precipitation of impurities in the phosphoric acid raffinate. In addition, the condition is controlled to slowly decompose the urea and uniformly release OH in the solution - Can prevent local pH value in the conventional ammonia water pH adjusting methodToo high results in the coiling of phosphorus due to the local strong hydrolysis of Fe and Al.
The surface morphology of the impurity-removed slag of the present invention was compared with the surface morphology of the existing ammonia impurity-removed slag, and the results are shown in fig. 1 and 2. FIG. 1 is a SEM image of the surface topography of impurity-removed slag according to the invention; FIG. 2 is a surface topography SEM image of a conventional ammonia water impurity removal product. As can be seen from figure 1, the impurity-removed product of the invention is stacked in a sheet shape, the structure is complete and consistent, and the high crystallinity of the urea precipitation product is proved; as can be seen from FIG. 2, the conventional ammonia water impurity removal product has small flake particle size and irregular shape, and is easy to form large particle agglomeration; as can be seen from the comparison between FIG. 1 and FIG. 2, the urea impurity-removed product of the present invention has a more complete and uniform morphology, a larger crystal size, and less loss of phosphorus, which is a useful element, in the process of precipitating Fe, Al, and Mg, compared to the existing ammonia water impurity-removed product.
(3) The method has the advantages that the turbid phosphoric acid raffinate is used as the treatment object, impurities in the turbid phosphoric acid raffinate are directly removed, the purification of the raffinate can be realized without filtering colloidal precipitates in the phosphoric acid raffinate, the precipitates generated on a microscopic level have high crystallinity and large grain size, particles are in a fine powder shape on a macroscopic level (impurity removal slag obtained in the conventional impurity removal mode is in a colloid shape), and the turbid matters in the phosphoric acid raffinate react with a precipitator in the impurity removal process, so that the filtration process is easier to perform, and the process flow is shortened.
(4) As described in the positive effect (2), urea slowly releases ammonia gas when heated to 60 ℃ or higher:
CO(NH 2 ) 2 +H 2 O→CO 2 ↑+2NH 3
NH 3 +H 2 O→NH 4 + +OH -
the urea is decomposed to generate ammonia and carbon dioxide, new impurities are not introduced while impurities are removed, and the prepared diammonium phosphate product meets the requirements of national standard monoammonium phosphate and diammonium phosphate (GB 10205-2009).
Therefore, the method has the advantages of good operating environment, easy filtration, low phosphorus loss rate in the impurity removal process and no introduction of new impurities.
Drawings
FIG. 1 is a surface topography SEM image of an impurity-removed slag according to the invention;
FIG. 2 is an SEM image of the surface topography of the product of ammonia water impurity removal in the prior art.
Detailed Description
The invention is further described with reference to specific embodiments, without limiting its scope.
In this embodiment:
the phosphoric acid raffinate acid: p 2 O 5 Content (wt.)>35 wt%, MgO content of 2-8 wt%, Al 2 O 3 4-8 wt% of Fe 2 O 3 0.5-3 wt% of CaO, and<0.05wt％，K 2 o content<0.1wt％，Na 2 Content of O<1.5 wt%, the solid content is 4-8 wt%, and the pH value is less than-0.8; the density of the phosphoric acid raffinate acid clear liquid is more than 1.6g/cm 3 。
The detailed description is omitted in the embodiments.
Example 1
A preparation method of diammonium phosphate based on phosphoric acid extraction spent acid. The method of the embodiment comprises the following specific steps:
step one, dilution
Adding water into the phosphoric acid raffinate according to the mass ratio of 1: 0.1-0.15, and stirring for 0.5-0.7 h at normal temperature to obtain diluted phosphoric acid raffinate.
Step two, precipitation
Adding urea into the diluted phosphoric acid raffinate acid according to the mass ratio of urea to the diluted phosphoric acid raffinate acid of (0.5-1): 1, stirring at 70-80 ℃ until the pH value is 6-6.4, and carrying out solid-liquid separation to obtain the purified phosphoric acid raffinate acid and the impurity-removed slag.
Step three, washing
Washing the impurity-removed slag by water to obtain washed impurity-removed slag and washing water; and returning the washing water to the first step for diluting the phosphoric acid raffinate acid.
Step four, preparing diammonium phosphate
Concentrating the purified phosphoric acid raffinate to P 2 O 5 The content of the diammonium phosphate is 40-44 wt%, and then the diammonium phosphate is introduced into a tubular reactor, and the neutralization degree is controlled to be 1.8-2.0, so that diammonium phosphate based on phosphoric acid raffinate acid is prepared. The prepared diammonium phosphate product based on phosphoric acid extraction spent acid meets the requirements of national standard monoammonium phosphate and diammonium phosphate (GB 10205-2009). .
Example 2
A preparation method of diammonium phosphate based on phosphoric acid extraction spent acid. The method of the embodiment comprises the following specific steps:
step one, dilution
Adding water into the phosphoric acid raffinate according to the mass ratio of 1: 0.1-0.2, and stirring for 0.6-0.8 h at normal temperature to obtain diluted phosphoric acid raffinate.
Step two, precipitation
Adding urea into the diluted phosphoric acid raffinate acid according to the mass ratio of urea to the diluted phosphoric acid raffinate acid of (1-1.5): 1, stirring at 80-90 ℃ until the pH value is 6.2-6.6, and carrying out solid-liquid separation to obtain the purified phosphoric acid raffinate acid and the impurity-removed slag.
Step three, washing
Washing the impurity-removed slag by water to obtain washed impurity-removed slag and washing water; and returning the washing water to the first step for diluting the phosphoric acid raffinate acid.
Step four, preparing diammonium phosphate
Concentrating the purified phosphoric acid raffinate to P 2 O 5 The content of the diammonium phosphate is 43-47 wt%, and then the diammonium phosphate is introduced into a tubular reactor, and the neutralization degree is controlled to be 1.8-2.0, so that diammonium phosphate based on phosphoric acid raffinate acid is prepared. The prepared diammonium phosphate product based on phosphoric acid extraction spent acid meets the requirements of national standard monoammonium phosphate and diammonium phosphate (GB 10205-2009). .
Example 3
A preparation method of diammonium phosphate based on phosphoric acid extraction spent acid. The method of the embodiment comprises the following specific steps:
step one, dilution
Adding water into the phosphoric acid raffinate acid according to the mass ratio of 1: 0.2-0.3 of the phosphoric acid raffinate acid to the water, and stirring for 0.8-1 h at normal temperature to obtain the diluted phosphoric acid raffinate acid.
Step two, precipitation
Adding urea into the diluted phosphoric acid raffinate acid according to the mass ratio of urea to the diluted phosphoric acid raffinate acid of (1.5-2): 1, stirring at 90-100 ℃ until the pH value is 6.6-7, and carrying out solid-liquid separation to obtain the purified phosphoric acid raffinate acid and the impurity-removed slag.
Step three, washing
Washing the impurity-removed slag by adopting water to obtain washed impurity-removed slag and washing water; and returning the washing water to the first step for diluting the phosphoric acid raffinate acid.
Step four, preparing diammonium phosphate
Concentrating the purified phosphoric acid raffinate to P 2 O 5 The content of the diammonium phosphate is 46-50 wt%, and then the diammonium phosphate is introduced into a tubular reactor, and the neutralization degree is controlled to be 1.8-2.0, so that diammonium phosphate based on phosphoric acid raffinate acid is prepared. The prepared diammonium phosphate product based on phosphoric acid extraction spent acid meets the requirements of national standard monoammonium phosphate and diammonium phosphate (GB 10205-2009).
Compared with the prior art, the specific implementation mode has the following positive effects:
(1) according to the specific embodiment, the urea is added at one time, so that the effect of removing various metal ions is good, wherein the impurity removal rate of iron and aluminum is more than 98%, and the impurity removal rate of magnesium is more than 90%;
(2) the urea is used as a slow-release precipitator, so that the occurrence of coprecipitation can be effectively prevented, iron ions, aluminum ions and magnesium ions in phosphoric acid raffinate are removed in a targeted manner, the inclusion of phosphorus is prevented, the generated precipitate is powdery, the generation of colloidal precipitate in the existing ammonia water purification process is avoided, and the loss rate of phosphorus can be reduced to be below 5%.
In this embodiment, the urea slowly releases ammonia when heated above 60 ℃:
CO(NH 2 ) 2 +H 2 O→CO 2 ↑+2NH 3
NH 3 +H 2 O→NH 4 + +OH -
NH product obtained by urea hydrothermal decomposition 4 + Is a reactant for the subsequent preparation of ammonium phosphate salt products, and OH is generated by the reaction - It helps to raise the pH of the solution and eventually reaches the optimum pH range for precipitation of impurities in the phosphoric acid raffinate. In addition, the condition is controlled to slowly decompose the urea and uniformly release OH in the solution - The method can prevent the coiling of phosphor caused by the local strong hydrolysis of Fe and Al due to the local over-high pH value in the conventional ammonia water pH adjusting method.
The surface morphology of the impurity-removed slag of the present embodiment is compared with the surface morphology of the impurity-removed slag of the existing ammonia water, and the results are shown in fig. 1 and 2. FIG. 1 is an SEM image of the surface topography of impurity-removed slag of example 2; FIG. 2 is a surface topography SEM image of a conventional ammonia water impurity removal product. As can be seen from FIG. 1, the impurity-removed residues are stacked in a flake shape, the structure is complete and consistent, and the high crystallinity of the urea precipitation product is proved; as can be seen from FIG. 2, the conventional ammonia water impurity removal product has small flake particle size and irregular shape, and is easy to form large particle agglomeration; as can be seen from the comparison between fig. 1 and fig. 2, the urea impurity-removed product of the present embodiment has a more complete and uniform morphology, a larger crystal size, and less loss of phosphorus, which is an active element, in the process of precipitation of Fe, Al, and Mg, compared to the existing ammonia water impurity-removed product.
(3) The treatment object of the specific embodiment is turbid phosphoric acid raffinate, the turbid phosphoric acid raffinate is directly subjected to impurity removal, the purification of raffinate can be realized without filtering colloidal precipitates in the phosphoric acid raffinate, the precipitates generated on a microscopic level have high crystallinity and large grain size, particles on a macroscopic level are in a fine powder shape (impurity removal slag obtained by the existing impurity removal mode is colloidal), and turbid matters in the phosphoric acid raffinate react with a precipitator in the impurity removal process, so that the filtration process is easier to carry out, and the process flow is shortened.
(4) As described in the positive effect (2), the urea slowly releases ammonia gas when heated to 60 ℃ or higher:
CO(NH 2 ) 2 +H 2 O→CO 2 ↑+2NH 3
NH 3 +H 2 O→NH 4 + +OH -
the urea is decomposed to generate ammonia and carbon dioxide, new impurities are not introduced while impurities are removed, and the prepared diammonium phosphate product based on phosphoric acid extraction spent acid meets the requirements of national standard monoammonium phosphate and diammonium phosphate (GB 10205-2009).
Therefore, the embodiment has the advantages of good operating environment, easy filtration, low phosphorus loss rate in the impurity removal process and no introduction of new impurities.
Claims (2)
1. A preparation method of diammonium phosphate based on phosphoric acid extraction spent acid is characterized by comprising the following specific steps:
step one, dilution
Adding water into the phosphoric acid raffinate acid according to the mass ratio of 1: 0.1-0.3, and stirring for 0.5-1 h at normal temperature to obtain diluted phosphoric acid raffinate acid;
step two, precipitation
Adding urea into the diluted phosphoric acid raffinate acid according to the mass ratio of urea to the diluted phosphoric acid raffinate acid of (0.5-2): 1, stirring at 70-100 ℃ until the pH value is 6-7, and carrying out solid-liquid separation to obtain purified phosphoric acid extract raffinate acid and impurity-removed slag;
step three, washing
Washing the impurity-removed slag by adopting water to obtain washed impurity-removed slag and washing water; the washing water is returned to the step one for diluting phosphoric acid raffinate acid;
step four, preparing diammonium phosphate
Concentrating the purified phosphoric acid raffinate acid to P 2 O 5 The content of the diammonium phosphate is 40-50 wt%, and then the diammonium phosphate is introduced into a tubular reactor, and the neutralization degree is controlled to be 1.8-2.0, so that diammonium phosphate based on phosphoric acid raffinate acid is obtained.
2. The method of claim 1, wherein the phosphoric acid raffinate acid-based diammonium phosphate is prepared byIn that the phosphoric acid raffinate acid: p 2 O 5 Content (wt.)>35 wt%, MgO content of 2-8 wt%, Al 2 O 3 4-8 wt% of Fe 2 O 3 0.5-3 wt% of CaO, and<0.05wt％，K 2 content of O<0.1wt％，Na 2 Content of O<1.5 wt%, the solid content is 4-8 wt%, and the pH value is less than-0.8; the density of the phosphoric acid raffinate acid clear liquid is more than 1.6g/cm 3 。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891504A (en) * | 2010-07-26 | 2010-11-24 | 瓮福（集团）有限责任公司 | Method for producing granular monoammonium phosphate with raffinate |
| CN102674284A (en) * | 2012-06-20 | 2012-09-19 | 瓮福（集团）有限责任公司 | Method for producing industrial monoammonium phosphate co-produced fertilizer grade monoammonium phosphate by extracted spent acid |
| CN104016322A (en) * | 2014-05-20 | 2014-09-03 | 贵阳中化开磷化肥有限公司 | Production method for diammonium hydrogen phosphate |
| CN107161967A (en) * | 2017-06-29 | 2017-09-15 | 宜都兴发化工有限公司 | It is a kind of to add the method and device that raffinate clear liquid produces high-class product diammonium phosphate product |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2432583A1 (en) * | 2002-06-20 | 2003-12-20 | Merck Patent Gesellschaft Mit Beschraenkter Haftung | Method of preparing alpha- and beta-tricalcium phosphate powders |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891504A (en) * | 2010-07-26 | 2010-11-24 | 瓮福（集团）有限责任公司 | Method for producing granular monoammonium phosphate with raffinate |
| CN102674284A (en) * | 2012-06-20 | 2012-09-19 | 瓮福（集团）有限责任公司 | Method for producing industrial monoammonium phosphate co-produced fertilizer grade monoammonium phosphate by extracted spent acid |
| CN104016322A (en) * | 2014-05-20 | 2014-09-03 | 贵阳中化开磷化肥有限公司 | Production method for diammonium hydrogen phosphate |
| CN107161967A (en) * | 2017-06-29 | 2017-09-15 | 宜都兴发化工有限公司 | It is a kind of to add the method and device that raffinate clear liquid produces high-class product diammonium phosphate product |
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