CN101823734A - Method for preparing pharmaceutical grade potassium chloride with sea salt potassium chloride - Google Patents
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Abstract
The invention relates to a method for preparing pharmaceutical grade potassium chloride with sea salt potassium chloride, which is characterized in that the sea salt potassium chloride is crushed to be loose and added into a crystallizer by a certain ratio together with circulating mother liquor and secondary washing liquid, so that materials in a crystallizer reaction area interflow; crystallizer underflow is discharged under the premise of ensuring system stability; the crystallizer underflow is centrifuged and separated to obtain a primary product and primary filtrate; and then the primary product, saturated potassium chloride solution and secondary washing liquid are added into a stirring tank by a certain ratio to be size-mixed and washed, centrifuged and separated to obtain a secondary product and secondary washing liquid; and the secondary product, the saturated potassium chloride solution and deionized water are added into the stirring tank by a certain ratio to be size mixed and washed, centrifuged and separated so as to obtain pharmaceutical grade potassium chloride and saturated potassium chloride solution.
Description
Technical field
The present invention relates to a kind of preparation method of Repone K, particularly a kind of is the method for raw material production pharmaceutical grade Repone K with potassium chloride with sea salt, belongs to the purification technique field of alkali metal halide.
Background technology
Repone K is a kind of important Inorganic Chemicals and agricultural fertilizer.Potassium ion is the essential nutrient substance of people's bulk-growth, and it accounts for 5% of human body inorganic salt, and is extremely important to the neural system and the adjusting cardiac rhythm that keep perfecting.It can prevent apoplexy, keeps normal Muscle contraction, keeps body fluid equilibrium jointly with sodium.The main production method of prior art Chinese materia medica grade potassium chloride is: it is molten to add hydro-thermal with Repone K, regulate pH value precipitation with alkali and remove elements such as calcium, magnesium, iron, adjust the pH value with hydrochloric acid again and remove elements such as iodine, bromine, after clear liquid ebuillition of heated to solution is elements such as colourless removal chlorine and carbonate, be neutral with the potassium hydroxide adjust pH at last, smart filter, evaporation-crystallisation by cooling-solid-liquid separation-dry packing get pharmaceutical grade Repone K.This method exists that ton product energy consumption is higher, water consumption is big, medical expenses are bigger, and flow process complexity, equipment erosion resistance require high, shortcoming such as facility investment is bigger.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, and a kind of production technique of the new more rational pharmaceutical grade Repone K of technology is provided, and it is workable, can effectively reduce pharmaceutical grade Repone K production cost and ton product energy consumption.
Technical problem to be solved by this invention is to realize by following technical scheme.The present invention is a kind of method with preparing pharmaceutical grade potassium chloride with sea salt potassium chloride, is characterized in that its step is as follows:
(1) potassium chloride with sea salt is crushed to loose back and joins in the crystallizer (draft tube baffle crystallizer) with circulating mother liquor, secondary washing liquid are continuous in proportion, stable, the stirring velocity of crystallization control device makes the interior material of crystallizer reaction zone be the complete mixing flow state; Reaction mass residence time in crystallizer is 0.1～10 hour; The weight proportion of potassium chloride with sea salt, circulating mother liquor, secondary washing liquid is 1: 2～20: 0.2～2;
(2) guaranteeing under the prerequisite of system stability, continuously or intermittently, the crystallizer underflow of stable emissions; The weight concentration of crystallizer underflow is 5%～35%; Crystallizer underflow gets first product and first-time filtrate through centrifugation, first-time filtrate is returned to settling vessel carried out sedimentation; The crystallizer overflow enters the settling vessel sedimentation; The settling vessel underflow gets the excessive brilliant and sedimentation filtrate of byproduct through centrifugation, and sedimentation filtrate and first-time filtrate are returned settling vessel and carried out secondary settlement; The settling vessel overflow is a circulating mother liquor, and the part circulating mother liquor enters in the step (1) and recycles, and unnecessary circulating mother liquor is discharged reactive system; The weight concentration of crystallizer overflow is 0.05%～1%;
(3) first product, saturated potassium chloride solution, secondary washing liquid are added in proportion carry out pulp washing in the steel basin, after the stirring, get second product and secondary washing liquid through centrifugation, secondary washing liquid enters the first washing lotion storage tank, part recycles in this step (3), and the crystallizer that part enters step (1) reacts; The weight proportion of first product, saturated potassium chloride solution, secondary washing liquid is 1: 0.5～10: 0.1～10;
(4) second product, saturated potassium chloride solution, deionized water are added in proportion carry out pulp washing in the steel basin, after the stirring, get three products and saturated potassium chloride solution through centrifugation, saturated potassium chloride solution enters the second washing lotion storage tank, part recycles in this step (4), and part enters the pulp washing operation of step (3); The heavy proportioning of second product, saturated potassium chloride solution, deionized water is 1: 0.5～10: 0.1～10; Three times product is pharmaceutical grade Repone K.
Use in the method for preparing pharmaceutical grade potassium chloride with sea salt potassium chloride above-described:
1, the operation of each step all can be carried out under normal temperature condition.
2, in step (1), reaction mass residence time in crystallizer is preferably 1～5 hour.
3, in the step (1), the weight proportion of potassium chloride with sea salt, circulating mother liquor, secondary washing liquid is preferably 1: 5-10: 1～1.5.
4, in the step (2), the weight concentration of crystallizer underflow is preferably 10%～30%.
5, in the step (3), the weight proportion of first product, saturated potassium chloride solution, secondary washing liquid is preferably 1: 2～and 5: 1～5.
6, in step (3) and (4), the churning time of pulp washing is preferably 2 minutes to 1 hour; More preferably 10-30 minute.
7, in the step (4), the heavy proportion optimization of second product, saturated potassium chloride solution, deionized water is 1: 2～5: 1～5.
8, technology of the present invention is cycle production process, needs to recycle circulating mother liquor, secondary washing liquid and saturated potassium chloride solution etc. in process of production.Therefore, in producing first, when the circulating mother liquor that does not have to produce in this technological process, secondary washing liquid and saturated potassium chloride solution, can prepare according to the component of above each mother liquor, so that production system can very fast steady running.
The characteristic of the crystallization of technology utilization crystallization principle of the present invention and crystallizer, purification, removal of impurities, with bittern Repone K is raw material, utilize the characteristic of crystallizer cleverly and control, bittern Repone K was finished in crystallizer intercrystalline, purification, one step of removal of impurities, exempted the production process that high energy consumption, complex process, investment are big, cost is high of traditional system pharmaceutical grade resolving process.This technology can a step make the higher first product of purity, for the final pharmaceutical grade Repone K product that obtains is laid a good foundation.The advantage of this technical process is: owing to introduce the crystalline principle cleverly in pharmaceutical grade Repone K production technique, make production at normal temperature condition and guarantee under the prerequisite of first product quality, simplify technical process, shortened production process, reduced energy consumption in production process, cost and the investment etc. of pharmaceutical grade Repone K ton product, thereby reduced the production cost of pharmaceutical grade Repone K significantly.
Description of drawings
Fig. 1 is a kind of process flow diagram of the present invention.
Embodiment
Following with reference to accompanying drawing, further describe concrete technical scheme of the present invention, so that those skilled in the art understands the present invention further, and do not constitute restriction to its right.
Embodiment 1.With reference to Fig. 1.A kind of method with preparing pharmaceutical grade potassium chloride with sea salt potassium chloride, its step is as follows:
(1) potassium chloride with sea salt is crushed to loose back and joins in the crystallizer with circulating mother liquor, secondary washing liquid are continuous in proportion, stable, the stirring velocity of crystallization control device makes the interior material of crystallizer reaction zone be the complete mixing flow state; Reaction mass residence time in crystallizer is 0.1 hour; The weight proportion of potassium chloride with sea salt, circulating mother liquor, secondary washing liquid is 1: 2: 0.2;
(2) guaranteeing under the prerequisite of system stability, continuously or intermittently, the crystallizer underflow of stable emissions; The weight concentration of crystallizer underflow is 5%; Crystallizer underflow gets first product and first-time filtrate through centrifugation, first-time filtrate is returned to settling vessel carried out sedimentation; The crystallizer overflow enters the settling vessel sedimentation; The settling vessel underflow gets the excessive brilliant and sedimentation filtrate of byproduct through centrifugation, and sedimentation filtrate and first-time filtrate are returned settling vessel and carried out secondary settlement; The settling vessel overflow is a circulating mother liquor, and the part circulating mother liquor enters in the step (1) and recycles, and unnecessary circulating mother liquor is discharged reactive system; The weight concentration of crystallizer overflow is 0.05%;
(3) first product, saturated potassium chloride solution, secondary washing liquid are added in proportion carry out pulp washing in the steel basin, after the stirring, get second product and secondary washing liquid through centrifugation, secondary washing liquid enters the first washing lotion storage tank, part recycles in this step (3), and the crystallizer that part enters step (1) reacts; The weight proportion of first product, saturated potassium chloride solution, secondary washing liquid is 1: 0.5: 0.1;
(4) second product, saturated potassium chloride solution, deionized water are added in proportion carry out pulp washing in the steel basin, after the stirring, get three products and saturated potassium chloride solution through centrifugation, saturated potassium chloride solution enters the second washing lotion storage tank, part recycles in this step (4), and part enters the pulp washing operation of step (3); The heavy proportioning of second product, saturated potassium chloride solution, deionized water is 1: 0.5: 0.1; Three times product is pharmaceutical grade Repone K.
Embodiment 2.With reference to Fig. 1.A kind of method with preparing pharmaceutical grade potassium chloride with sea salt potassium chloride, its step is as follows:
(1) potassium chloride with sea salt is crushed to loose back and joins in the crystallizer with circulating mother liquor, secondary washing liquid are continuous in proportion, stable, the stirring velocity of crystallization control device makes the interior material of crystallizer reaction zone be the complete mixing flow state; Reaction mass residence time in crystallizer is 10 hours; The weight proportion of potassium chloride with sea salt, circulating mother liquor, secondary washing liquid is 1: 20: 2;
(2) guaranteeing under the prerequisite of system stability, continuously or intermittently, the crystallizer underflow of stable emissions; The weight concentration of crystallizer underflow is 35%; Crystallizer underflow gets first product and first-time filtrate through centrifugation, first-time filtrate is returned to settling vessel carried out sedimentation; The crystallizer overflow enters the settling vessel sedimentation; The settling vessel underflow gets the excessive brilliant and sedimentation filtrate of byproduct through centrifugation, and sedimentation filtrate and first-time filtrate are returned settling vessel and carried out secondary settlement; The settling vessel overflow is a circulating mother liquor, and the part circulating mother liquor enters in the step (1) and recycles, and unnecessary circulating mother liquor is discharged reactive system; The weight concentration of crystallizer overflow is 1%;
(3) first product, saturated potassium chloride solution, secondary washing liquid are added in proportion carry out pulp washing in the steel basin, after the stirring, get second product and secondary washing liquid through centrifugation, secondary washing liquid enters the first washing lotion storage tank, part recycles in this step (3), and the crystallizer that part enters step (1) reacts; The weight proportion of first product, saturated potassium chloride solution, secondary washing liquid is 1: 10: 10;
(4) second product, saturated potassium chloride solution, deionized water are added in proportion carry out pulp washing in the steel basin, after the stirring, get three products and saturated potassium chloride solution through centrifugation, saturated potassium chloride solution enters the second washing lotion storage tank, part recycles in this step (4), and part enters the pulp washing operation of step (3); The heavy proportioning of second product, saturated potassium chloride solution, deionized water is 1: 10: 10; Three times product is pharmaceutical grade Repone K.
Embodiment 3.With reference to Fig. 1.A kind of method with preparing pharmaceutical grade potassium chloride with sea salt potassium chloride, its step is as follows:
(1) potassium chloride with sea salt is crushed to loose back and circulating mother liquor, secondary washing liquid in proportion continuously, stablize in crystallizer, the stirring velocity of crystallization control device makes that material is the complete mixing flow state in the crystallizer reaction zone; Reaction mass residence time in crystallizer is 1 hour; The weight proportion of potassium chloride with sea salt, circulating mother liquor, secondary washing liquid is 1: 5: 1;
(2) guaranteeing under the prerequisite of system stability, continuously or intermittently, the crystallizer underflow of stable emissions; The weight concentration of crystallizer underflow is 20%; Crystallizer underflow gets first product and first-time filtrate through centrifugation, first-time filtrate is returned to settling vessel carried out sedimentation; The crystallizer overflow enters the settling vessel sedimentation; The settling vessel underflow gets the excessive brilliant and sedimentation filtrate of byproduct through centrifugation, and sedimentation filtrate and first-time filtrate are returned settling vessel and carried out secondary settlement; The settling vessel overflow is a circulating mother liquor, and the part circulating mother liquor enters in the step (1) and recycles, and unnecessary circulating mother liquor is discharged reactive system; The weight concentration of crystallizer overflow is 0.1;
(3) first product, saturated potassium chloride solution, secondary washing liquid are added in proportion carry out pulp washing in the steel basin, after the stirring, get second product and secondary washing liquid through centrifugation, secondary washing liquid enters the first washing lotion storage tank, part recycles in this step (3), and the crystallizer that part enters step (1) reacts; The weight proportion of first product, saturated potassium chloride solution, secondary washing liquid is 1: 2: 5;
(4) second product, saturated potassium chloride solution, deionized water are added in proportion carry out pulp washing in the steel basin, after the stirring, get three products and saturated potassium chloride solution through centrifugation, saturated potassium chloride solution enters the second washing lotion storage tank, part recycles in this step (4), and part enters the pulp washing operation of step (3); The heavy proportioning of second product, saturated potassium chloride solution, deionized water is 1: 3: 2; Three times product is pharmaceutical grade Repone K.
Embodiment 4.With reference to Fig. 1.A kind of method with preparing pharmaceutical grade potassium chloride with sea salt potassium chloride, its step is as follows:
(1) potassium chloride with sea salt is crushed to loose back and joins in the crystallizer with circulating mother liquor, secondary washing liquid are continuous in proportion, stable, the stirring velocity of crystallization control device makes the interior material of crystallizer reaction zone be the complete mixing flow state; Reaction mass residence time in crystallizer is 5 hours; The weight proportion of potassium chloride with sea salt, circulating mother liquor, secondary washing liquid is 1: 15: 0.5;
(2) guaranteeing under the prerequisite of system stability, continuously or intermittently, the crystallizer underflow of stable emissions; The weight concentration of crystallizer underflow is 10%; Crystallizer underflow gets first product and first-time filtrate through centrifugation, first-time filtrate is returned to settling vessel carried out sedimentation; The crystallizer overflow enters the settling vessel sedimentation; The settling vessel underflow gets the excessive brilliant and sedimentation filtrate of byproduct through centrifugation, and sedimentation filtrate and first-time filtrate are returned settling vessel and carried out secondary settlement; The settling vessel overflow is a circulating mother liquor, and the part circulating mother liquor enters in the step (1) and recycles, and unnecessary circulating mother liquor is discharged reactive system; The weight concentration of crystallizer overflow is 0.5%;
(3) first product, saturated potassium chloride solution, secondary washing liquid are added in proportion carry out pulp washing in the steel basin, after the stirring, get second product and secondary washing liquid through centrifugation, secondary washing liquid enters the first washing lotion storage tank, part recycles in this step (3), and the crystallizer that part enters step (1) reacts; The weight proportion of first product, saturated potassium chloride solution, secondary washing liquid is 1: 8: 3;
(4) second product, saturated potassium chloride solution, deionized water are added in proportion carry out pulp washing in the steel basin, after the stirring, get three products and saturated potassium chloride solution through centrifugation, saturated potassium chloride solution enters the second washing lotion storage tank, part recycles in this step (4), and part enters the pulp washing operation of step (3); The heavy proportioning of second product, saturated potassium chloride solution, deionized water is 1: 6: 8; Three times product is pharmaceutical grade Repone K.
Embodiment 5.With reference to Fig. 1.A kind of method with preparing pharmaceutical grade potassium chloride with sea salt potassium chloride, its step is as follows:
(1) potassium chloride with sea salt is crushed to loose back and joins in the crystallizer with circulating mother liquor, secondary washing liquid are continuous in proportion, stable, the stirring velocity of crystallization control device makes the interior material of crystallizer reaction zone be the complete mixing flow state; Reaction mass residence time in crystallizer is 0.5 hour; The weight proportion of potassium chloride with sea salt, circulating mother liquor, secondary washing liquid is 1: 15: 1.8;
(2) guaranteeing under the prerequisite of system stability, continuously or intermittently, the crystallizer underflow of stable emissions; The weight concentration of crystallizer underflow is 30%; Crystallizer underflow gets first product and first-time filtrate through centrifugation, first-time filtrate is returned to settling vessel carried out sedimentation; The crystallizer overflow enters the settling vessel sedimentation; The settling vessel underflow gets the excessive brilliant and sedimentation filtrate of byproduct through centrifugation, and sedimentation filtrate and first-time filtrate are returned settling vessel and carried out secondary settlement; The settling vessel overflow is a circulating mother liquor, and the part circulating mother liquor enters in the step (1) and recycles, and unnecessary circulating mother liquor is discharged reactive system; The weight concentration of crystallizer overflow is 0.8%;
(3) first product, saturated potassium chloride solution, secondary washing liquid are added in proportion carry out pulp washing in the steel basin, after the stirring, get second product and secondary washing liquid through centrifugation, secondary washing liquid enters the first washing lotion storage tank, part recycles in this step (3), and the crystallizer that part enters step (1) reacts; The weight proportion of first product, saturated potassium chloride solution, secondary washing liquid is 1: 2: 0.6;
(4) second product, saturated potassium chloride solution, deionized water are added in proportion carry out pulp washing in the steel basin, after the stirring, get three products and saturated potassium chloride solution through centrifugation, saturated potassium chloride solution enters the second washing lotion storage tank, part recycles in this step (4), and part enters the pulp washing operation of step (3); The heavy proportioning of second product, saturated potassium chloride solution, deionized water is 1: 4: 2.5; Three times product is pharmaceutical grade Repone K.
Embodiment 6.Any one described using in the method for preparing pharmaceutical grade potassium chloride with sea salt potassium chloride of embodiment 1-5, the operation of each step is all carried out under normal temperature condition.
Embodiment 7.With preparing pharmaceutical grade potassium chloride with sea salt potassium chloride experiment one.
As shown in Figure 1, the potassium chloride with sea salt of caking is crushed to no obvious particulate loose condition (of surface), the potassium chloride with sea salt that fragmentation is good is with 5 kilograms/hour, the speed of 50 kilograms/hour of circulating mother liquors, 2.13 kilograms/hour of secondary washing liquid, evenly, the stable volume that joins is in 30 liters the crystallizer, the stirring velocity of crystallization control device, make that material is the complete mixing flow state in the crystallizer reaction zone, the control reaction mass in crystallizer the residence time at 1 hour.The crystallizer overflow enters the settling vessel sedimentation, and the settling vessel underflow is through centrifugation must overflow brilliant 0.25 kilogram/hour and this operation filtrate, and this filtrate and first product filtrate are returned settling vessel and carried out sedimentation again.The settling vessel overflow is that circulating mother liquor enters in the crystallizer and recycles, and unnecessary circulating mother liquor is discharged reactive system for 2.17 kilograms/hour; Emit material with 11 liters/hour speed from crystallizer bottom discharge mouth average rate.Get 4.71 kilograms of/hour first products, filtrate blowback settling vessel after filtration.Gained first product and saturated potassium chloride solution and secondary washing liquid are in first product: saturated potassium chloride solution: the ratio of secondary washing liquid=1: 0.48: 2, join steel basin, carry out pulp washing, fully stir after 15 minutes, get 4.70 kilograms/hour of second products and secondary washing liquid through centrifugation.Secondary washing liquid enters the first washing lotion storage tank, and major part recycles, and has more part and enters crystallizer and react.Gained second product and saturated potassium chloride solution and deionized water are again in second product: saturated potassium chloride solution: the ratio of deionized water=1: 4: 0.36 joins steel basin, carry out pulp washing, fully stir after 30 minutes, get 4.29 kilograms/hour of three products and saturated potassium chloride solution through centrifugation.Saturated potassium chloride solution enters the second washing lotion storage tank, and major part recycles, and has more part and enters the higher level and wash separation circuit.4.29 the kilogram/hour three product dryings pack 4.17 kilograms of/hour pharmaceutical grade Repone K products.
Embodiment 8.With preparing pharmaceutical grade potassium chloride with sea salt potassium chloride experiment two.
As shown in Figure 1, the potassium chloride with sea salt of caking is crushed to no obvious particulate loose condition (of surface), the potassium chloride with sea salt that fragmentation is good with 20 kilograms/hour, circulating mother liquor 120 kg/hour, the speed of 18.5 kilograms/hour of secondary washing liquid, it is evenly, stable that to join volume be in 80 liters of crystallizers, the stirring velocity of crystallization control device, make that material is the complete mixing flow state in the crystallizer reaction zone, the control reaction mass in crystallizer the residence time at 0.5 hour.The crystallizer overflow enters the settling vessel sedimentation, and the settling vessel underflow is through centrifugation must overflow brilliant 0.87 kilogram/hour and this operation filtrate, and this filtrate and first product filtrate are returned settling vessel and carried out sedimentation again.The settling vessel overflow is that circulating mother liquor enters in the crystallizer and recycles, and unnecessary circulating mother liquor is discharged reactive system for 18.7 kilograms/hour; Emit material with 55 liters/hour speed from crystallizer bottom discharge mouth average rate.Get 19.0 kilograms of/hour first products, filtrate blowback settling vessel after filtration.Gained first product and saturated potassium chloride solution and secondary washing liquid are in first product: saturated potassium chloride solution: the ratio of secondary washing liquid=1: 0.98: 3, join steel basin, carry out pulp washing, fully stir after 45 minutes, get 18.8 kilograms/hour of second products and secondary washing liquid through centrifugation.Secondary washing liquid enters the first washing lotion storage tank, and major part recycles, and has more part and enters crystallizer and react.Gained second product and saturated potassium chloride solution and deionized water are again in second product: saturated potassium chloride solution: the ratio of deionized water=1: 2: 0.77 joins steel basin, carry out pulp washing, fully stir after 20 minutes, get 14.9 kilograms/hour of three products and saturated potassium chloride solution through centrifugation.Saturated potassium chloride solution enters the second washing lotion storage tank, and major part recycles, and has more part and enters the higher level and wash separation circuit.14.9 the kilogram/hour three product dryings pack 14.5 kilograms of/hour pharmaceutical grade Repone K products.
Embodiment 9.With preparing pharmaceutical grade potassium chloride with sea salt potassium chloride experiment three.
As shown in Figure 1, the potassium chloride with sea salt of caking is crushed to no obvious particulate loose condition (of surface), the potassium chloride with sea salt that fragmentation is good is with 80 kilograms/hour, the speed of 400 kilograms/hour of circulating mother liquors, 121 kilograms/hour of secondary washing liquid, it is evenly, stable that to join volume be in 800 liters of crystallizers, the stirring velocity of crystallization control device, make that material is the complete mixing flow state in the crystallizer reaction zone, the control reaction mass in crystallizer the residence time at 2 hours.The crystallizer overflow enters the settling vessel sedimentation, and the settling vessel underflow is through centrifugation must overflow brilliant 2.37 kilograms/hour and this operation filtrate, and this filtrate and first product filtrate are returned settling vessel and carried out sedimentation again.The settling vessel overflow is that circulating mother liquor enters in the crystallizer and recycles, and unnecessary circulating mother liquor is discharged reactive system for 123 kilograms/hour; Emit material with 296 liters/hour speed from crystallizer bottom discharge mouth average rate.Get 75.0 kilograms of/hour first products, filtrate blowback settling vessel after filtration.Gained first product and saturated potassium chloride solution and secondary washing liquid are in first product: saturated potassium chloride solution: the ratio of secondary washing liquid=1: 1.58: 5, join steel basin, carry out pulp washing, fully stir after 60 minutes, get 72.4 kilograms/hour of second products and secondary washing liquid through centrifugation.Secondary washing liquid enters the first washing lotion storage tank, and major part recycles, and has more part and enters crystallizer and react.Gained second product and saturated potassium chloride solution and deionized water are again in second product: saturated potassium chloride solution: the ratio of deionized water=1: 2: 1.31 joins steel basin, carry out pulp washing, fully stir after 45 minutes, get 48.8 kilograms/hour of three products and saturated potassium chloride solution through centrifugation.Saturated potassium chloride solution enters the second washing lotion storage tank, and major part recycles, and has more part and enters the higher level and wash separation circuit.48.8 the kilogram/hour three product dryings pack 47.3 kilograms of/hour pharmaceutical grade Repone K products.
Claims (9)
1. the method with preparing pharmaceutical grade potassium chloride with sea salt potassium chloride is characterized in that, its step is as follows:
(1) potassium chloride with sea salt is crushed to loose back and joins in the crystallizer with circulating mother liquor, secondary washing liquid are continuous in proportion, stable, the stirring velocity of crystallization control device makes the interior material of crystallizer reaction zone be the complete mixing flow state; Reaction mass residence time in crystallizer is 0.1～10 hour; The weight proportion of potassium chloride with sea salt, circulating mother liquor, secondary washing liquid is 1: 2～20: 0.2～2;
(2) guaranteeing under the prerequisite of system stability, continuously or intermittently, the crystallizer underflow of stable emissions; The weight concentration of crystallizer underflow is 5%～35%; Crystallizer underflow gets first product and first-time filtrate through centrifugation, first-time filtrate is returned to settling vessel carried out sedimentation; The crystallizer overflow enters the settling vessel sedimentation; The settling vessel underflow gets the excessive brilliant and sedimentation filtrate of byproduct through centrifugation, and sedimentation filtrate and first-time filtrate are returned settling vessel and carried out secondary settlement; The settling vessel overflow is a circulating mother liquor, and the part circulating mother liquor enters in the step (1) and recycles, and unnecessary circulating mother liquor is discharged reactive system; The weight concentration of crystallizer overflow is 0.05%～1%;
(3) first product, saturated potassium chloride solution, secondary washing liquid are added in proportion carry out pulp washing in the steel basin, after the stirring, get second product and secondary washing liquid through centrifugation, secondary washing liquid enters the first washing lotion storage tank, part recycles in this step (3), and the crystallizer that part enters step (1) reacts; The weight proportion of first product, saturated potassium chloride solution, secondary washing liquid is 1: 0.5～10: 0.1～10;
(4) second product, saturated potassium chloride solution, deionized water are added in proportion carry out pulp washing in the steel basin, after the stirring, get three products and saturated potassium chloride solution through centrifugation, saturated potassium chloride solution enters the second washing lotion storage tank, part recycles in this step (4), and part enters the pulp washing operation of step (3); The heavy proportioning of second product, saturated potassium chloride solution, deionized water is 1: 0.5～10: 0.1～10; Three times product is pharmaceutical grade Repone K.
2. the method with preparing pharmaceutical grade potassium chloride with sea salt potassium chloride according to claim 1, it is characterized in that: the operation of each step is all carried out under normal temperature condition.
3. the method with preparing pharmaceutical grade potassium chloride with sea salt potassium chloride according to claim 1, it is characterized in that: in the step (1), reaction mass residence time in crystallizer is 1～5 hour.
4. the method with preparing pharmaceutical grade potassium chloride with sea salt potassium chloride according to claim 1, it is characterized in that: in the step (1), the weight proportion of potassium chloride with sea salt, circulating mother liquor, secondary washing liquid is 1: 5-10: 1～1.5.
5. the method with preparing pharmaceutical grade potassium chloride with sea salt potassium chloride according to claim 1 and 2, it is characterized in that: in the step (2), the weight concentration of crystallizer underflow is 10%～30%.
6. the method with preparing pharmaceutical grade potassium chloride with sea salt potassium chloride according to claim 1 and 2, it is characterized in that: in the step (3), the weight proportion of first product, saturated potassium chloride solution, secondary washing liquid is 1: 2～5: 1～5.
7. the method with preparing pharmaceutical grade potassium chloride with sea salt potassium chloride according to claim 1 and 2, it is characterized in that: in step (3) and (4), the churning time of pulp washing is 2 minutes to 1 hour.
8. the method with preparing pharmaceutical grade potassium chloride with sea salt potassium chloride according to claim 7, it is characterized in that: the churning time of pulp washing is 10-30 minute.
9. the method with preparing pharmaceutical grade potassium chloride with sea salt potassium chloride according to claim 1 and 2, it is characterized in that: in the step (4), the heavy proportioning of second product, saturated potassium chloride solution, deionized water is 1: 2～5: 1～5.
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| CN102963912A (en) * | 2012-12-25 | 2013-03-13 | 中蓝连海设计研究院 | Process for producing potassium chloride by using potassic salt ores |
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| 《盐业与化工》 20060730 袁俊生等 中国海盐苦卤综合利用技术的开发进展 第33-37页 1-9 第35卷, 第4期 2 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102963912A (en) * | 2012-12-25 | 2013-03-13 | 中蓝连海设计研究院 | Process for producing potassium chloride by using potassic salt ores |
| CN102963912B (en) * | 2012-12-25 | 2014-08-27 | 中蓝连海设计研究院 | Process for producing potassium chloride by using potassic salt ores |
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| CN101823734B (en) | 2012-02-29 |
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