CN105036158A - Method for preparing sodium nitrate through solvent extraction - Google Patents
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Abstract
The invention provides a method for preparing sodium nitrate through solvent extraction. The method includes the following steps that step1, a potassium chloride saturated solution with the temperature of 50 DEG C-70 DEG C is prepared, nitric acid is added to react with the potassium chloride saturated solution at the temperature of 50 DEG C-70 DEG C, cooling crystallization and solid-liquid separation are performed, and an obtained solid phase is washed with water and dried to obtain a potassium nitrate product; step2, an extraction agent is added into a liquid phase obtained in solid-liquid separation in the step1, and a raffinate water phase is returned into a reaction vessel in the step1; 3, an organic phase obtained in extraction in the step2 is mixed with water or a second mother solution, ammonia gas is led into the mixture for reverse extraction, and a reverse extraction organic phase is returned to the step2; 4, condensation crystallization and solid-liquid separation are performed on a reverse extraction water phase in the step3 to obtain ammonium chloride and a first mother solution, potassium chloride is added into the first mother solution and reacts with the first mother solution at the temperature of 60 DEG C-80 DEG C, cooling crystallization and solid-liquid separation are performed to obtain a solid phase and the second mother solution, the obtained solid phase is washed and dried to obtain a potassium nitrate product, and the second mother solution is returned to the step3.
Description
Technical field
The invention belongs to agricultural fertilizer material production field, particularly the method for saltpetre is prepared in a kind of solvent extraction.
Background technology
Saltpetre is a kind of not chloride higher-grade nitrogen, potassium two-nutrient compound fertilizer, its total nutritive ingredient is up to 60wt%, general applicability is strong, non-volatility, can be absorbed by plants and soil completely after using, can not chemical residual be brought into, effectively can improve the quality and yield of plant, be called as " real green fertilizer ".The production method of saltpetre is numerous, and the method for current industrial main employing has: SODIUMNITRATE-Repone K conversion method, ammonium nitrate-Repone K double decomposition, ion exchange method, nitric acid and Repone K preparation method.
Wang Guiyun etc. report a kind of method that solvent extration prepares Agricultural Potassium Nitrate, and Repone K, nitric acid and circulating mother liquor add in reactor and react in about 5 DEG C by the method, filter, by gained filter cake washing, dry after obtain potassium nitrate product; With being dissolved with HNO
3primary isoamyl alcohol extraction filtrate, make the HCl in filtrate and the unreacted HNO of part
3enter in primary isoamyl alcohol, extracting phase returns recycle; Use rare HNO
3extraction is washed and is dissolved with HCl and HNO
3primary isoamyl alcohol, extraction wash after containing HNO
3primary isoamyl alcohol recycle, extraction wash after aqueous phase be HCl and HNO
3nitration mixture; The HNO in described nitration mixture is extracted with tributyl phosphate (TBP)
3, obtain dilute hydrochloric acid and contain HNO
3tBP, with water back extraction containing HNO
3tBP, by rare for gained HNO
3wash for extraction and be dissolved with HCl and HNO
3primary isoamyl alcohol, gained TBP recycles.(Wang Guiyun, etc. solvent extration prepares Agricultural Potassium Nitrate [J], inorganic chemicals industry, and 1998,30 (3): 13 ~ 15.).The method has the following disadvantages: (1) energy consumption is high: temperature of reaction controlled at about 5 DEG C, needs a large amount of freezing energy consumptions, cause production cost too high in production process; (2) effectively HCl and HNO cannot be separated
3, extracting and separating complicated operation is loaded down with trivial details: due to primary isoamyl alcohol with there is certain mutual solubility between TBP and water, and thus there will be containing the phenomenon containing TBP in primary isoamyl alcohol, primary isoamyl alcohol in TBP, cause effect of extracting undesirable, sepn process is complicated, is separated HCl and HNO
3process become the main part of whole process for producing potassium nitrate, separation costs is high; (3) extraction agent consumption is large: the method adopts primary isoamyl alcohol extracting HCl, the partition ratio of HCl in isoamyl alcohol and water is about 0.058 ~ 0.57, namely when HCl concentration is higher, primary isoamyl alcohol has good selectivity to HCl, but in potassium nitrate crystal mother liquor, HCl concentration is not high usually, thus the percentage extraction of primary isoamyl alcohol to hydrochloric acid is lower, and primary isoamyl alcohol solubleness in water is larger, part primary isoamyl alcohol is soluble in the aqueous phase when extracting and causes damage, therefore, reach certain effect of extracting, the consumption of primary isoamyl alcohol is large, causes production cost high; (4) concentration of by-product hydrochloric acid is very low, is 7.5% ~ 8.5%, and containing impurity HNO
3although can obtain through further concentrated the hydrochloric acid that concentration is about 20%, the hydrochloric acid after concentrated still cannot as production marketing, and concentration operation needs to consume a large amount of energy, also there is the problem that energy consumption is too high, containing HNO in by-product hydrochloric acid
3also result in raw material NO
3 -waste.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of solvent extraction to prepare the method for saltpetre, to simplify production technique, the reduction energy consumption of saltpetre and to save production cost.
The method of saltpetre is prepared in solvent extraction of the present invention, and processing step is as follows:
(1) saturated potassium chloride solution that temperature is 50 ~ 70 DEG C is prepared, nitric acid is added in saturated potassium chloride solution, under agitation obtain reaction solution in 50 ~ 70 DEG C of reaction 30 ~ 60min, reaction solution crystallisation by cooling, solid-liquid separation are obtained solid phase and liquid phase, gained solid phase is saltpetre crude product, washed with water and be drying to obtain potassium nitrate product by described saltpetre crude product, the add-on of nitric acid should make the mol ratio of Repone K in nitric acid and saturated potassium chloride solution be 1:(1.0 ~ 1.5);
(2) in step (1) solid-liquid separation gained liquid phase, add extraction agent to extract at 20 ~ 30 DEG C, extraction gained raffinate aqueous phase is back in step (1) for preparing saturated potassium chloride solution, the volume ratio of described extraction agent and solid-liquid separation gained liquid phase is (1 ~ 3): 1, described extraction agent is made up of primary isoamyl alcohol, tributyl phosphate and trioctylamine, and the volume ratio of primary isoamyl alcohol, tributyl phosphate, trioctylamine is 1:(5 ~ 10): (20 ~ 35);
(3) step (2) is extracted the organic phase and water obtained or step (4) gained second mother liquor is mixed to get mixed solution, in this mixed solution, pass into ammonia carry out back extraction at 50 ~ 70 DEG C, stop when the pH value of mixed solution is 7 ~ 8 passing into ammonia, gained back extraction organic phase is back in step (2) and extracts;
(4) by step (3) gained strip aqueous condensing crystal and solid-liquid separation, by-product ammonium chloride and the first mother liquor is obtained; Repone K is added in the first mother liquor, under agitation obtain reaction solution in 60 ~ 80 DEG C of reaction 30 ~ 60min, by reaction solution crystallisation by cooling and solid-liquid separation obtains solid phase and the second mother liquor, gained solid phase is saltpetre crude product, described saltpetre crude product is washed with water and is drying to obtain potassium nitrate product, gained second mother liquor is back in step (3) mutually and carries out back extraction; The add-on of Repone K should make NO in the first mother liquor
3 -with K
+mol ratio be 1:(1 ~ 1.2).
In the step (2) of aforesaid method, the extraction residence time is 15 ~ 30min.
In the step (1) of aforesaid method, the terminal temperature of described crystallisation by cooling is 20 ~ 30 DEG C.
In the step (1) of aforesaid method, the concentration of described nitric acid is 65 ~ 68wt%.
In the step (4) of aforesaid method, the terminal temperature of described crystallisation by cooling is 18 ~ 22 DEG C.
In the step (4) of aforesaid method, described condensing crystal is that strip aqueous is concentrated into K in strip aqueous at 60 ~ 80 DEG C
+with NH
4 +mol ratio be (0.15 ~ 0.18): 1, Cl
-with NO
3 -mol ratio be (1.4 ~ 1.6): 1.
In aforesaid method method, the preferential water concentrated out during condensing crystal that step (4) is middle that adopts is for washing saltpetre crude product in step (1) and step (4); The rear water of washing saltpetre crude product in step (1) and step (4) returns in step (1) for preparing saturated potassium chloride solution by preferential employing.
In the step (3) of aforesaid method, at the flow startup initial stage, step (2) is extracted the organic phase obtained and water is mixed to get mixed solution, the consumption of water should make the volume ratio of described organic phase and aqueous phase for (3 ~ 7): 1; After producing the second mother liquor in the step (4), the organic phase that step (2) to be extracted and obtain and step (4) gained second mother liquor in step (3), is adopted to be mixed to get the scheme of mixed solution.
In aforesaid method, described saturated potassium chloride solution refers to Repone K saturated aqueous solution.
Compared with prior art, the present invention has following beneficial effect:
1, the invention provides a kind of novel method preparing saltpetre, production for saltpetre provides a kind of new thinking, nitric acid and Repone K preparation method and ammonium nitrate and Repone K double decomposition organically combine by the method, obtain the potassium nitrate product of two kinds of qualities, and the hydrochloric acid cannot sold with product existing technique obtained has changed into the ammonium chloride that can reach agricultural above index, target by product due to the method for the invention is ammonium chloride instead of hydrochloric acid, thus without the need to considering how to operate by extracting and separating problem hydrochloric acid and nitric acid are effectively separated, the method of the invention adopts a step extraction by hydrochloric acid and nitric acid extraction out, the hydrochloric acid of extraction and nitric acid can be converted into ammonium chloride and ammonium nitrate through a step back extraction again, compared with prior art, the method of the invention fundamentally solves the hydrochloric acid and nitric acid separation difficulty that exist in existing technique, lock out operation complexity is loaded down with trivial details, problem containing impurity nitric acid in the low and hydrochloric acid of concentration of hydrochloric acid, enormously simplify extraction and back-extraction operation, not only be conducive to enhancing productivity, effectively can also reduce the cost of extraction and back-extraction operation.
2, the extraction agent adopted due to the method for the invention forms by primary isoamyl alcohol, tributyl phosphate and trioctylamine are composite, and because the extracting power of trioctylamine to acid is high, simultaneously primary isoamyl alcohol, tributyl phosphate good to the effect of extracting of HCl is to HNO
3effect of extracting good, and the reasonable ratio of three, described extraction agent simultaneously can extract hydrochloric acid and nitric acid efficiently, and thus the method for the invention has that Solvent quantity is few, extraction time is short, back extraction is simple, and extraction and back-extraction operation is easy to the advantage of control.The method of the invention is when extracting, the water that raw material nitric acid can be brought into system by extraction agent is all taken away, when back extraction, the water extracted in extraction agent all can be transferred to aqueous phase from organic phase again, therefore in the circulation of the raffinate aqueous phase of step (2) and the back extraction organic phase circulation time of step (3) all without the need to concentration operation, there is the advantage that energy consumption is low.
3, due in the step (1) of the method for the invention, nitric acid and Repone K produce saltpetre 50 ~ 70 DEG C of reactions, maintain the heating less energy consumption needed for this temperature of reaction, and whole step of reaction is all without the need to refrigeration operation, therefore the energy consumption of the method for the invention is low, the reaction carrying out nitric acid and Repone K at 50 ~ 70 DEG C also has following advantage: higher temperature of reaction is conducive to the solubleness increasing Repone K, improve the output of saltpetre, rate of mass transfer and speed of reaction can also be increased, shorten the process time.
4, the utilization ratio of the method for the invention to raw material nitric acid and Repone K is very high, the circulation of raffinate aqueous phase ensure that the utilization completely of Repone K, and the circulation of raffinate aqueous phase can not introduce impurity in reaction system, and in step (4), if the process parameter control of condensing crystal and crystallisation by cooling is proper, the ammonium nitrate be transformed by unreacted nitric acid all can be converted into saltpetre, realize the utilization completely of nitric acid, if ignore the loss that technological operation causes, the utilization ratio of raw material nitric acid and Repone K can reach 100%.Simultaneously, water after washing saltpetre crude product in step (1) (4) is back to step (1) for preparing saturated potassium chloride solution, in whole technique except outwardly output potassium nitrate product and ammonium chloride byproduct, can not to output pollutent or waste in environment, technique environmental protection.
5, the method for the invention obtains the potassium nitrate product of two kinds of different qualities, step (1) gained potassium nitrate product meets GB/T20784-2006 " agricultural saltpetre " premium grads or acceptable end product index, step (4) gained potassium nitrate product meets GB/T20784-2006 " agricultural saltpetre " acceptable end product or salable product index, and, purity >=95% of the byproduct ammonium chloride that the method for the invention obtains, this purity meets agricultural ammonium chloride standard, can be used as and makes nitrogen application.
6, owing to adopting existing conventional full scale plant can realize producing in the technical process of the method for the invention, equipment investment is low, and technique is simple, and whole technical process is atmospheric operation, thus easily realizes industry and amplifies, be conducive to applying.
Accompanying drawing explanation
Fig. 1 is a kind of process flow sheet of the method for the invention.
Embodiment
The method of the invention is described further by example below in conjunction with accompanying drawing.Data in following each embodiment are system and reach the data after stablizing.In following each embodiment, purity >=99.0% of Repone K, primary isoamyl alcohol, TBP and trioctylamine massfraction are all >=98.5%; The content of each ion and material is mass percent.
Embodiment 1
As shown in Figure 1, step is as follows in the technical process of the present embodiment:
(1) by Repone K 100g, water 233g and raffinate aqueous phase (flow startup initial stage, raffinate aqueous phase is water) add in reaction vessel, preparation temperature is the saturated potassium chloride solution of 50 DEG C, the nitric acid 103g that concentration is 68wt% is added in reaction vessel, in 50 DEG C of reaction 60min under normal pressure, stirring, gained reaction solution is naturally cooled to 25 DEG C, filters, gained filter cake 20g water washing is also dried and obtained 1
#potassium nitrate product 63g, productive rate is 56%;
(2) step (1) is filtered and is obtained filtrate 364g, in this filtrate, and H
+content is 0.30wt%, Cl
-content is 12.89wt%, NO
3 -content is 8.75wt%, extraction agent is added in this filtrate, the volume ratio of extraction agent and filtrate is 1.5:1, extract at 25 DEG C, the extraction residence time is 15min, extraction gained raffinate aqueous phase is back to for preparing saturated potassium chloride solution in the reaction vessel of step (1), in this raffinate aqueous phase, H
+content is 0wt%, Cl
-content is 9.02wt%, NO
3 -content is 0.61wt%;
Described extraction agent is the mixed solution of primary isoamyl alcohol, tributyl phosphate (TBP) and trioctylamine, and the volume ratio of primary isoamyl alcohol, TBP, trioctylamine is 1:6.5:30.
(3) by step (2) extraction gained organic phase and step (4) gained second mother liquor (flow startup initial stage, using water as the second mother liquor, the volume ratio that the consumption of water should make step (2) extract organic phase and the aqueous phase obtained is 5:1) be mixed to get mixed solution, in this mixed solution, pass into ammonia carry out back extraction at 70 DEG C, stop when the pH value of mixed solution is 7 passing into ammonia, by gained back extraction organic phase (in back extraction organic phase, H
+, Cl
-and NO
3 -content be 0) be back in step (1) and recycle;
(4) step (3) gained strip aqueous is carried out condensing crystal at 60 DEG C, be concentrated into K in strip aqueous
+with NH
4 +mol ratio be 0.16:1, Cl
-with NO
3 -mol ratio be 1.5:1, filter obtain filter cake and the first mother liquor, filter cake is dried and obtains by-product ammonium chloride 58g; In the first mother liquor, add Repone K 38g, at 60 DEG C of stirring reaction 30min, gained reaction solution is naturally cooled to 20 DEG C, filter and obtain filter cake and the second mother liquor, gained filter cake 15g water washing is also dried and obtained 2
#potassium nitrate product 46g, productive rate is 93%, is back in step (3) by gained second mother liquor and recycles.
The present embodiment prepare 1
#potassium nitrate product, 2
#potassium nitrate product composition is as shown in table 1, and the index of GB/T20784-2006 " Agricultural Potassium Nitrate " premium grads, acceptable end product and salable product is as shown in table 2.
Table 1 obtain 1
#potassium nitrate product, 2
#potassium nitrate product
| Product | w(K 2O),％ | W (total N), % | w(Cl -),％ | w(H +),％ | W (free-water), % |
| 1 #Saltpetre | 46.11 | 13.62 | 0.28 | 0.01 | 0.36 |
| 2 #Saltpetre | 45.85 | 13.53 | 0.68 | 0.01 | 1.04 |
Table 2GB/T20784-2006 " Agricultural Potassium Nitrate " quality parameter
From table 1 and table 2, the present embodiment prepare 1
#potassium nitrate product and 2
#potassium nitrate product all meets the requirement of the acceptable end product in GB/T20784-2006 " agricultural saltpetre ".In the present embodiment, saltpetre overall yield is 97%.
Embodiment 2
As shown in Figure 1, step is as follows in the technical process of the present embodiment:
(1) by Repone K 100g, water 218g and raffinate aqueous phase (flow startup initial stage, raffinate aqueous phase is water) add in reaction vessel, preparation temperature is the saturated potassium chloride solution of 60 DEG C, the nitric acid 83g that concentration is 68wt% is added in reaction vessel, in 60 DEG C of reaction 45min under normal pressure, stirring, gained reaction solution is naturally cooled to 30 DEG C, filters, gained filter cake 25g water washing is also dried and obtained 1
#potassium nitrate product 49g, productive rate is 54%;
(2) step (1) is filtered and is obtained filtrate 341g, in this filtrate, and H
+content is 0.26wt%, Cl
-content is 13.54wt%, NO
3 -content is 7.79wt%, extraction agent is added in this filtrate, the volume ratio of extraction agent and filtrate is 1:1, extract at 30 DEG C, the extraction residence time is 20min, extraction gained raffinate aqueous phase is back to for preparing saturated potassium chloride solution in the reaction vessel of step (1), in this raffinate aqueous phase, H
+content is 0wt%, Cl
-content is 10.93wt%, NO
3 -content is 0.56wt%;
Described extraction agent is the mixed solution of primary isoamyl alcohol, TBP and trioctylamine, and the volume ratio of primary isoamyl alcohol, TBP, trioctylamine is 1:5.5:20.
(3) by step (2) extraction gained organic phase and step (4) gained second mother liquor (flow startup initial stage, using water as the second mother liquor, the volume ratio that the consumption of water should make step (2) extract organic phase and the aqueous phase obtained is 3:1) be mixed to get mixed solution, in this mixed solution, pass into ammonia carry out back extraction at 60 DEG C, stop when the pH value of mixed solution is 7.4 passing into ammonia, by gained back extraction organic phase (in back extraction organic phase, H
+, Cl
-and NO
3 -content be 0) be back in step (1) and recycle;
(4) step (3) gained strip aqueous is carried out condensing crystal at 70 DEG C, be concentrated into K in strip aqueous
+with NH
4 +mol ratio be 0.15:1, Cl
-with NO
3 -mol ratio be 1.6:1, filter obtain filter cake and the first mother liquor, filter cake is dried and obtains by-product ammonium chloride 46g; In the first mother liquor, add Repone K 30g, at 70 DEG C of stirring reaction 50min, gained reaction solution is naturally cooled to 18 DEG C, filter and obtain filter cake and the second mother liquor, gained filter cake 10g water washing is also dried and obtained 2
#potassium nitrate product 37g, productive rate is 95%, is back in step (3) by gained second mother liquor and recycles.
The present embodiment prepare 1
#potassium nitrate product, 2
#potassium nitrate product composition is as shown in table 3.
Table 31
#potassium nitrate product, 2
#potassium nitrate product composition
| Product | w(K 2O),％ | W (total N), % | w(Cl -),％ | w(H +),％ | W (free-water), % |
| 1 #Saltpetre | 46.11 | 13.60 | 0.42 | 0.01 | 0.33 |
| 2 #Saltpetre | 44.95 | 13.52 | 0.84 | 0.01 | 1.21 |
From table 3 and table 2, the present embodiment prepare 1
#potassium nitrate product and 2
#potassium nitrate product all meets the requirement of the acceptable end product in GB/T20784-2006 " agricultural saltpetre ".In the present embodiment, saltpetre overall yield is 95%.
Embodiment 3
As shown in Figure 1, step is as follows in the technical process of the present embodiment:
(1) by Repone K 100g, water 208g and raffinate aqueous phase (flow startup initial stage, raffinate aqueous phase is water) add in reaction vessel, preparation temperature is the saturated potassium chloride solution of 70 DEG C, the nitric acid 130g that concentration is 65wt% is added in reaction vessel, at normal pressure, 70 DEG C of stirring reaction 30min, gained reaction solution is naturally cooled to 20 DEG C, filters, gained filter cake 15g water washing is also dried and obtained 1
#potassium nitrate product 72g, productive rate is 53%;
(2) step (1) is filtered and is obtained filtrate 361g, in this filtrate, and H
+content is 0.37wt%, Cl
-content is 13.22wt%, NO
3 -content is 11.21wt%, extraction agent is added in this filtrate, the volume ratio of extraction agent and filtrate is 3:1, extract at 20 DEG C, the extraction residence time is 30min, extraction gained raffinate aqueous phase is back to for preparing saturated potassium chloride solution in the reaction vessel of step (1), in this raffinate aqueous phase, H
+content is 0wt%, Cl
-content is 9.41wt%, NO
3 -content is 0.76wt%;
Described extraction agent is the mixed solution of primary isoamyl alcohol, TBP and trioctylamine, and the volume ratio of primary isoamyl alcohol, TBP, trioctylamine is 1:10:35.
(3) by step (2) extraction gained organic phase and step (4) gained second mother liquor (flow startup initial stage, using water as the second mother liquor, the volume ratio that the consumption of water should make step (2) extract organic phase and the aqueous phase obtained is 7:1) be mixed to get mixed solution, in this mixed solution, pass into ammonia carry out back extraction at 50 DEG C, stop when the pH value of mixed solution is 8 passing into ammonia, by gained back extraction organic phase (in back extraction organic phase, H
+, Cl
-and NO
3 -content be 0) be back in step (1) and recycle;
(4) step (3) gained strip aqueous is carried out condensing crystal at 80 DEG C, be concentrated into K in strip aqueous
+with NH
4 +mol ratio be 0.18:1, Cl
-with NO
3 -mol ratio be 1.4:1, filter obtain filter cake and the first mother liquor, filter cake is dried and obtains by-product ammonium chloride 67g; In the first mother liquor, add Repone K 45g, at 80 DEG C of stirring reaction 60min, gained reaction solution is naturally cooled to 22 DEG C, filter and obtain filter cake and the second mother liquor, gained filter cake 20g water washing is also dried and obtained 2
#potassium nitrate product 54g, productive rate is 89%, is back in step (3) by gained second mother liquor and recycles.
The present embodiment prepare 1
#potassium nitrate product, 2
#potassium nitrate product composition is as shown in table 4.
Table 41
#potassium nitrate product, 2
#potassium nitrate product composition
| Product | w(K 2O),％ | W (total N), % | w(Cl -),％ | w(H +),％ | W (free-water), % |
| 1 #Saltpetre | 46.34 | 13.68 | 0.18 | 0.01 | 0.39 |
| 2 #Saltpetre | 44.18 | 13.52 | 1.23 | 0.01 | 1.16 |
As shown in Table 4,1
#potassium nitrate product meets the requirement of premium grads in GB/T20784-2006 " agricultural saltpetre ", and 2
#potassium nitrate product meets the requirement of salable product in GB/T20784-2006 " agricultural saltpetre ".In the present embodiment, saltpetre overall yield is 93%.
Claims (10)
1. a method for saltpetre is prepared in solvent extraction, it is characterized in that processing step is as follows:
(1) saturated potassium chloride solution that temperature is 50 ~ 70 DEG C is prepared, nitric acid is added in saturated potassium chloride solution, under agitation obtain reaction solution in 50 ~ 70 DEG C of reaction 30 ~ 60min, reaction solution crystallisation by cooling, solid-liquid separation are obtained solid phase and liquid phase, gained solid phase is saltpetre crude product, washed with water and be drying to obtain potassium nitrate product by described saltpetre crude product, the add-on of nitric acid should make the mol ratio of Repone K in nitric acid and saturated potassium chloride solution be 1:(1.0 ~ 1.5);
(2) in step (1) solid-liquid separation gained liquid phase, add extraction agent to extract at 20 ~ 30 DEG C, extraction gained raffinate aqueous phase is back in step (1) for preparing saturated potassium chloride solution, the volume ratio of described extraction agent and solid-liquid separation gained liquid phase is (1 ~ 3): 1, described extraction agent is made up of primary isoamyl alcohol, tributyl phosphate and trioctylamine, and the volume ratio of primary isoamyl alcohol, tributyl phosphate, trioctylamine is 1:(5 ~ 10): (20 ~ 35);
(3) step (2) is extracted the organic phase and water obtained or step (4) gained second mother liquor is mixed to get mixed solution, in this mixed solution, pass into ammonia carry out back extraction at 50 ~ 70 DEG C, stop when the pH value of mixed solution is 7 ~ 8 passing into ammonia, gained back extraction organic phase is back in step (2) and extracts;
(4) by step (3) gained strip aqueous condensing crystal and solid-liquid separation, by-product ammonium chloride and the first mother liquor is obtained; Repone K is added in the first mother liquor, under agitation obtain reaction solution in 60 ~ 80 DEG C of reaction 30 ~ 60min, by reaction solution crystallisation by cooling and solid-liquid separation obtains solid phase and the second mother liquor, gained solid phase is saltpetre crude product, described saltpetre crude product is washed with water and is drying to obtain potassium nitrate product, gained second mother liquor is back in step (3) mutually and carries out back extraction; The add-on of Repone K should make NO in the first mother liquor
3 -with K
+mol ratio be 1:(1 ~ 1.2).
2. the method for saltpetre is prepared in solvent extraction according to claim 1, it is characterized in that the extraction residence time in step (2) is 15 ~ 30min.
3. according to claim 1 or 2, the method for saltpetre is prepared in solvent extraction, it is characterized in that the terminal temperature of crystallisation by cooling described in step (1) is 20 ~ 30 DEG C.
4. according to claim 1 or 2, the method for saltpetre is prepared in solvent extraction, it is characterized in that the concentration of step (1) described nitric acid is 65 ~ 68wt%.
5. according to claim 1 or 2, the method for saltpetre is prepared in solvent extraction, it is characterized in that the terminal temperature of step (4) described crystallisation by cooling is 18 ~ 22 DEG C.
6. according to claim 1 or 2, the method for saltpetre is prepared in solvent extraction, it is characterized in that step (4) described condensing crystal is that strip aqueous is concentrated into K in strip aqueous at 60 ~ 80 DEG C
+with NH
4 +mol ratio be (0.15 ~ 0.18): 1, Cl
-with NO
3 -mol ratio be (1.4 ~ 1.6): 1.
7. according to claim 1 or 2, the method for saltpetre is prepared in solvent extraction, it is characterized in that the water concentrated out during condensing crystal in step (4) for washing saltpetre crude product in step (1) and step (4).
8. according to claim 1 or 2, the method for saltpetre is prepared in solvent extraction, it is characterized in that the rear water of washing saltpetre crude product in step (1) and step (4) to return in step (1) for preparing saturated potassium chloride solution.
9. the method for saltpetre is prepared in solvent extraction according to claim 3, it is characterized in that the rear water of washing saltpetre crude product in step (1) and step (4) to return in step (1) for preparing saturated potassium chloride solution.
10. the method for saltpetre is prepared in solvent extraction according to claim 8, it is characterized in that the rear water of washing saltpetre crude product in step (1) and step (4) to return in step (1) for preparing saturated potassium chloride solution.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107651698A (en) * | 2017-10-25 | 2018-02-02 | 安徽胜达化工科技有限公司 | A kind of production method of potassium nitrate crystals |
| CN107651697A (en) * | 2017-10-25 | 2018-02-02 | 安徽胜达化工科技有限公司 | A kind of preparation method of potassium nitrate |
| CN107840354A (en) * | 2017-10-25 | 2018-03-27 | 安徽胜达化工科技有限公司 | A kind of extractant that potassium nitrate is prepared for nitric acid potassium chloride extraction |
| CN108439521A (en) * | 2018-04-16 | 2018-08-24 | 北京石油化工学院 | A kind of regeneration method of the extractant of naphthalene sulfonic waste water |
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| CN103112876A (en) * | 2013-01-14 | 2013-05-22 | 青海盐湖工业股份有限公司 | Method for preparing potassium nitrate by utilizing nitric acid and potassium chloride |
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| US4378342A (en) * | 1980-04-20 | 1983-03-29 | Haifa Chemicals Ltd. | Process for the manufacture of potassium nitrate |
| US4364914A (en) * | 1980-04-30 | 1982-12-21 | Haifa Chemicals Ltd. | Process for the manufacture of potassium nitrate with co-production of hydrochloric acid |
| US4668495A (en) * | 1984-07-30 | 1987-05-26 | Union Explosivos Rio Tinto, S.A. | Process for obtaining potassium nitrate from potassium chloride and nitric acid |
| CN101182014A (en) * | 2007-12-15 | 2008-05-21 | 文水县振兴化肥有限公司 | Preparation technique of potassium nitrate |
| CN101734690A (en) * | 2008-11-13 | 2010-06-16 | 常福松 | Method for preparing potassium nitrate by solvent extraction method |
| CN101759205A (en) * | 2008-11-19 | 2010-06-30 | 陶伟平 | Method for preparing potassium nitrate by extracting n-butyl alcohol |
| CN102267706A (en) * | 2011-07-14 | 2011-12-07 | 中蓝连海设计研究院 | Method for preparing potassium nitrate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107651698A (en) * | 2017-10-25 | 2018-02-02 | 安徽胜达化工科技有限公司 | A kind of production method of potassium nitrate crystals |
| CN107651697A (en) * | 2017-10-25 | 2018-02-02 | 安徽胜达化工科技有限公司 | A kind of preparation method of potassium nitrate |
| CN107840354A (en) * | 2017-10-25 | 2018-03-27 | 安徽胜达化工科技有限公司 | A kind of extractant that potassium nitrate is prepared for nitric acid potassium chloride extraction |
| CN108439521A (en) * | 2018-04-16 | 2018-08-24 | 北京石油化工学院 | A kind of regeneration method of the extractant of naphthalene sulfonic waste water |
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