CN103159194B - Continuous crystallization process for monopotassium phosphate - Google Patents
Continuous crystallization process for monopotassium phosphate Download PDFInfo
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- CN103159194B CN103159194B CN201310122354.9A CN201310122354A CN103159194B CN 103159194 B CN103159194 B CN 103159194B CN 201310122354 A CN201310122354 A CN 201310122354A CN 103159194 B CN103159194 B CN 103159194B
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Abstract
The invention discloses a continuous crystallization process for monopotassium phosphate. The continuous crystallization process comprises the following specific steps of: introducing a feed liquid to be crystallized into a first-stage continuous flash crystallizer so as to be separated into a primary clear liquid, primary crystal mush and secondary steam; discharging the primary crystal mush from the first-stage continuous flash crystallizer and feeding the primary crystal mush into a second-stage continuous cooling crystallizer, wherein the second-stage continuous cooling crystallizer is composed of an Oslo crystallizer and an external cooler; separating the primary crystal mush into secondary crystal mush and a secondary clear liquid in the Oslo crystallizer; discharging the secondary crystal mush from the Oslo crystallizer, feeding the secondary crystal mush into a thickener and separating the secondary crystal mush into triple clear liquid and triple crystal mush; discharging the triple crystal mush from the thickener, feeding the triple crystal mush into a centrifugal machine, and separating the triple crystal mush into solid monopotassium phosphate and a centrifugal liquid; and discharging the solid monopotassium phosphate from the centrifugal machine. The continuous crystallization process is stable in operation, low in energy consumption and low in labor intensity; and by using the continuous crystallization process, the operation stability and the product quality are greatly improved, the on-site operation environment is improved, and the production cost of the monopotassium phosphate is reduced. A mating device for the process is small in floor area and high in capacity.
Description
Technical field
The present invention relates to the production method of potassium primary phosphate, refer in particular to a kind of crystallization processes of potassium primary phosphate.
Background technology
Potassium primary phosphate is a kind of important chemical, in industries such as agricultural, chemical industry, medicine and food, all has a wide range of applications.On chemical industry, potassium primary phosphate can be used as nutrient chemical, reinforcer, raising agent of raw material, fermentation assistant and the brewer's yeast of buffer reagent, nutrient chemical, potassium metaphosphate processed etc.; In agricultural, potassium primary phosphate is a kind of efficient phosphorus potassium complex fertilizer of high density; Pharmaceutically, potassium primary phosphate can be used for making uric acid, makes nutrition agent etc.; On food, potassium primary phosphate can be used as the seasonings of synthetic sake.
At present, the processing method of China's production potassium primary phosphate mainly contains neutralisation, extraction process, double decomposition and ion exchange method etc.Above-mentioned preparation method's common ground is: first by reaction, make potassium dihydrogen phosphate, then gained solution is obtained to the finished product through concentrated, crystallization, centrifugation, drying and other steps.Wherein, concentrated, crystallization, centrifugation, drying and other steps all belong to technological process separated, purification potassium primary phosphate, and in this technological process, crystallisation step is its core procedure.
Industrial crystallization method mainly contains following several: cooling method, method of evaporation, vacuum cooling method, salting-out process, reaction-crystallization method.Wherein, the crystallisation process of cooling method is not removed solvent substantially, but makes the cooling supersaturated solution that becomes of solution, and the method is applicable to the reduction of solubility with temperature and the system that significantly declines.Cooling method is divided into again nature cooling, directly contact cooling cooling, partition and cools.Wherein, partition cools because energy consumption is little, equipment is constructed and operation is comparatively simply widely used in the crystallization processes of potassium primary phosphate.But the crystallizer adopting due to this technique is main mainly with simple stirring pot type crystallizer, so its crystallization processes exists following shortcoming: be 1) intermittent type crystallization, be unsuitable for operate continuously; 2) time of crystallisation process is long, equipment therefor floor space is huge; 3) crystallisation process operational requirement is high, need adjust at any time coolant temperature and flow, stir pot type crystallizer and be prone to local overcooling, cause material to be crystallized to be agglomerated on the heat-transfer surface of crystallizer, and then make heat-transfer effect variation, finally cause the labor capacity of crystallization subsequent disposal to strengthen; 4) in crystallisation process, material easily occurs due to stirring reveal and splash, and operating environment is more severe; 5) crystallization operation is mainly completed by a large amount of personnel, and running cost is higher; 6), because the professional qualities between personnel and personnel there are differences, so the poor stability of whole crystallization operation and product, the quality product of different batches may there are differences.
Summary of the invention
The technical issues that need to address of the present invention are to provide a kind of crystallization processes of production potassium primary phosphate that can be continuous, stable.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is:
Potassium primary phosphate continuous crystallisation technique, the secondary continuous crystallisation mode that adopts flash crystallization to add crystallisation by cooling obtains potassium primary phosphate solid, and the idiographic flow of described secondary continuous crystallisation is:
A, the opening for feed of the feed liquid to be crystallized of coming from liquor inlet to be crystallized from one-level successive flash vaporization crystallizer bottom passes into one-level successive flash vaporization crystallizer, described feed liquid to be crystallized is lowered the temperature in one-level successive flash vaporization crystallizer, crystallization, be separated into clear liquid one time, magma and secondary steam, magma of gained is discharged and is entered mother liquor tank along pipeline from the discharge port of one-level successive flash vaporization crystallizer bottom, clear liquid of gained is discharged from the relief outlet at one-level successive flash vaporization crystallizer middle part, gained secondary steam is discharged through secondary steam outlet from the air outlet at one-level successive flash vaporization crystallizer top,
B, a magma of discharging from the discharge port of one-level successive flash vaporization crystallizer bottom be admitted in secondary continuous cooling crystallizer lower the temperature, crystallization; Described secondary continuous cooling crystallizer consists of Oslo crystallizer and Outer Cooler; A described magma is admitted to the central downtake at Oslo crystallizer top, and along central downtake, arrive the bottom of Oslo crystallizer internal cavity, then from the bottom of Oslo crystallizer, rising through fluidised crystallization bed, there is crystallization and forms secondary magma and secondary clear liquid in a magma herein; Secondary magma is discharged from the discharge port of Oslo crystallizer bottom, secondary clear liquid continues to move up to upper straight section, the crystallisation cycle pump that a part for secondary clear liquid is arranged at Oslo crystallizer top pumps into Outer Cooler to carry out heat exchange and shifts out entrained heat, secondary clear liquid after heat exchange is discharged from the discharge port of Outer Cooler, and the central downtake that enters Oslo crystallizer top mixes with a magma, form a circulation loop; Another part of secondary clear liquid overflows and enters mother liquor tank by pipeline from the overflow port on the top of Oslo crystallizer;
C, the secondary magma of discharging from the discharge port of Oslo crystallizer bottom are admitted to thickener and carry out thickening processing, described secondary magma is separated into three clear liquids and three magmas in thickener, three magmas of gained are discharged from the discharge port of thickener bottom, and the overflow port of three clear liquids of gained from thickener top overflows and enter mother liquor tank by pipeline;
D, three magmas of discharging from thickener bottom are admitted to and in whizzer, carry out centrifuging treatment, described three magmas are separated into potassium primary phosphate solid and centrifugate in whizzer, described potassium primary phosphate solid is from the discharge port of whizzer and through products export discharge, and described centrifugate escapes and enter mother liquor tank in whizzer.
Further improvement of the present invention is: the mother liquor in described mother liquor tank by a mother liquor pump part, be pumped to thickener another part and discharge from mother liquor outlet; Described Outer Cooler is shell and tube heat exchanger, adopt water quench mode, described water coolant enters the shell-side of Outer Cooler from cooling water inlet, the water coolant after heat exchange is discharged through cooling water outlet and discharged from Outer Cooler, and described water coolant carries out pump circulation in Outer Cooler by cooling water circulating pump.
Further improvement of the present invention is: described Outer Cooler is equipped with cleaning system, and the rate of flow of fluid in the heat transfer tube of Outer Cooler is 1.5m/s～1.8m/s.
Further improvement of the present invention is: described one-level successive flash vaporization crystallizer is DTB vacuum cyrsytalliser; The feed liquid that contains thin crystalline substance that overflow port from DTB vacuum cyrsytalliser middle part overflows by thin brilliant eliminate pump pump in thin brilliant eliminator, add thermosol brilliant process eliminate thin brilliant, eliminate thin brilliant feed liquid and discharge and enter DTB vacuum cyrsytalliser from the opening for feed of DTB vacuum cyrsytalliser bottom from the discharge port of thin brilliant eliminator, form a circulation loop; Described thin brilliant eliminator is shell and tube heat exchanger, takes steam heating mode.
Further improvement of the present invention is: after described flow process A processes, the temperature that enters a magma before flow process B is 60 ℃～65 ℃.
Owing to having adopted technique scheme, the technical progress that the present invention obtains is:
The invention provides a kind of potassium primary phosphate continuous crystallisation technique, crystallization processes stable operation, less energy consumption, and it is low that crystallization processes operates required labour intensity, stability and the quality product of crystallization process operation have greatly been improved, improve the environment of operation site, reduced the production cost of potassium primary phosphate.In addition, this technique corollary apparatus used also has advantages of that floor space is little, production capacity is high.
The secondary continuous crystallisation mode that potassium primary phosphate continuous crystallisation process using flash crystallization of the present invention adds crystallisation by cooling realizes, first adopt flash crystallization, in vacuum flashing mode, reduce the temperature of feed liquid to be crystallized, then adopt crystallisation by cooling mode to flash distillation after magma of gained carry out crystallization again.This kind of mode can effectively reduce the thermal load of material, and then reduces the heat interchanging area of crystallizer, finally reduces the investment of crystallization processes support equipment.In the present invention, after the crystallization of one-level successive flash vaporization, the temperature control of a magma of gained, within the scope of 60～65 ℃, has greatly reduced the thermal load of secondary continuous cooling crystallizer, and then provides favourable condition for the miniaturization of secondary continuous cooling crystallizer.
One-level successive flash vaporization crystallizer of the present invention is DTB vacuum cyrsytalliser, DTB vacuum cyrsytalliser is typical magma inner circulation type crystallizer, the pressure head required due to this crystallizer internal recycle is very low, water screw can be worked under lower rotating speed, so greatly reduced the secondary nucleation phenomenon that impeller brings the collision of crystal, finally can effectively improve the crystal size in a magma of gained after flow process A processes.The present invention in the outer setting of described one-level successive flash vaporization crystallizer thin brilliant eliminator, reduced the impact of thin crystalline substance on grain size number, realize the effective control to the grain size number of feed liquid in one-level successive flash vaporization crystallizer, further guaranteed the homogeneity of gained potassium primary phosphate solid fine grain granularity.
Secondary continuous cooling crystallizer of the present invention consists of Oslo crystallizer and Outer Cooler, the region that this set-up mode produces degree of supersaturation and crystal production region are divided and are arranged, gained secondary clear liquid forms a compulsory outer circulation between Oslo crystallizer and Outer Cooler by crystallisation cycle pump, make fluidized suspension in the circulation fluid of crystal in Oslo crystallizer, for crystal production provides good condition, can produce granularity compared with large and crystal uniformly.In addition, employing Oslo crystallizer has also reduced the possibility of crystal knot wall widely, has improved the utilization ratio of equipment, has extended equipment life.The flow velocity of the heat transfer tube inner fluid of Outer Cooler of the present invention can reach 1.5～1.8m/s, and heat transfer coefficient is larger, and ant-scaling performance is good, is convenient to switch and clean under operate continuously state.
Potassium primary phosphate crystallization processes of the present invention can operate continuously, and crystallization condition is stable, quality product homogeneous, and production capacity exceeds several times even tens times compared with batch operation.Corollary apparatus floor space of the present invention is little, is to stir 1/5～1/10 of pot type crystallizer floor space.
Accompanying drawing explanation
Fig. 1 is potassium primary phosphate continuous crystallisation process flow sheet of the present invention.
Wherein, 1, thin brilliant eliminator; 2, one-level successive flash vaporization crystallizer; 3, secondary continuous cooling crystallizer; 3-1, Outer Cooler; 3-2, Oslo crystallizer; 4, thickener; 5, whizzer; 6, mother liquor tank; 7, the thin brilliant pump of eliminating; 8, crystallization punishment in advance pump; 9, cooling water circulating pump; 10, crystallisation cycle pump; 11, crystallization discharging pump; 12, mother liquor pump; 13, secondary steam outlet; 14, liquor inlet to be crystallized; 15, steam-in; 16, vapor condensation water out; 17, products export; 18, mother liquor outlet; 19, cooling water inlet; 20, cooling water outlet.
Embodiment
Below in conjunction with embodiment, the present invention is described in further details:
Embodiment 1
Feed liquid to be crystallized is the potassium dihydrogen phosphate of producing by neutralisation, and the material state of described feed liquid to be crystallized is: temperature is that 95 ℃, concentration are 44.2%.
Equipment used in the present invention mainly comprises one-level successive flash vaporization crystallizer 2, secondary continuous cooling crystallizer 3, thickener 4 and whizzer 5.One-level successive flash vaporization crystallizer 2 is DTB vacuum cyrsytalliser, the opening for feed of its bottom is connected with liquor inlet 14 to be crystallized, described feed liquid to be crystallized enters in the opening for feed of DTB vacuum cyrsytalliser with the inlet amount of 22500kg/h, and enter the guide shell bottom of DTB vacuum cyrsytalliser inside center, then under the promotion of water screw, the bottom from guide shell starts to rise along guide shell, the liquid level place rising in DTB vacuum cyrsytalliser carries out shwoot, cooling, effusion secondary steam, the secondary steam of overflowing is discharged from the air outlet at DTB vacuum cyrsytalliser top, and through secondary steam outlet 13, enter steam and condensate system along pipeline, the bottom that flow to DTB vacuum cyrsytalliser along guide shell and the circular channel between baffle plate of DTB vacuum cyrsytalliser through shwoot, cooled feed liquid to be crystallized, and be again inhaled in guide shell, a circulation loop formed.Along with constantly carrying out of circulation, feed liquid to be crystallized in DTB vacuum cyrsytalliser starts crystallization, the concentration of feed liquid to be crystallized reduces from bottom to top gradually, the concentration of the feed liquid to be crystallized of DTB vacuum cyrsytalliser bottom constantly increases, and form a magma in the bottom of DTB vacuum cyrsytalliser, on the top of DTB vacuum cyrsytalliser, form a clear liquid.
A described clear liquid is discharged from the relief outlet at DTB vacuum cyrsytalliser middle part, and passes in mother liquor tank 6 along pipeline.That from the overflow port at DTB vacuum cyrsytalliser middle part, discharges is pumped in the tube side of thin brilliant eliminator 1 by the thin brilliant pump 7 of eliminating containing thin brilliant feed liquid, steam 15 enters the shell-side of thin brilliant eliminator 1 from steam-in through the inlet mouth of thin brilliant eliminator 1 along pipeline, and carry out heat exchange with the feed liquid containing thin crystalline substance of tube side, after heat exchange, the steam condensate of gained is discharged from the air outlet of thin brilliant eliminator 1, and enters vapor condensation water treatment system through vapor condensation water out 16; In feed liquid after heat exchange, contained thin crystalline substance is eliminated and is again sent in DTB vacuum cyrsytalliser and material liquid-phase mixing to be crystallized, forms a circulation loop.A described magma is discharged from the discharge port of DTB vacuum cyrsytalliser bottom.
The temperature of a magma of discharging from the discharge port of DTB vacuum cyrsytalliser bottom is 60 ℃, a described magma is pumped in the central downtake on Oslo crystallizer 3-2 top by crystallization punishment in advance pump 8, and along central downtake, arrive the bottom of Oslo crystallizer 3-2 inner chamber, and start rising from the bottom of Oslo crystallizer 3-2, in uphill process, pass fluidised crystallization bed, in crystallization bed, start crystallization, and form gradually herein secondary magma and secondary clear liquid; Gained secondary magma is discharged from the discharge port of Oslo crystallizer 3-2 bottom, secondary clear liquid continues to move up to the upper straight section of Oslo crystallizer 3-2, in uphill process, the concentration of secondary clear liquid continues to reduce, and substantially contains crystal after arrival upper straight section in described secondary clear liquid.
The a part of secondary clear liquid that enters the upper straight section of Oslo crystallizer 3-2 is forced to be sent in the tube side of Outer Cooler 3-1 by crystallisation cycle pump 10, and the flow velocity of secondary clear liquid in the tube side of Outer Cooler 3-1 is 1.5m/s.Water coolant 19 enters the shell-side of Outer Cooler 3-1 from cooling water inlet through the water-in of Outer Cooler 3-1 along pipeline, and carry out partition heat exchange to remove the heat in secondary clear liquid with secondary clear liquid, and make secondary clear liquid produce supersaturation, described water coolant moves at Outer Cooler 3-1 internal recycle by cooling water circulating pump 9, and the water coolant after heat exchange is discharged and from cooling water outlet 20, enters cooling water treatment system along pipeline from the water outlet of Outer Cooler 3-1.Secondary clear liquid after heat exchange is discharged from the discharge port of Outer Cooler 3-1, and again enters the central downtake at Oslo crystallizer 3-2 top, mixes with a magma, forms a circulation loop.The top of Oslo crystallizer 3-2 arranges an overflow port, and a part of secondary clear liquid overflowing from overflow port enters mother liquor tank 6.Outer Cooler 3-1 outside is equipped with cleaning system, can guarantee long-term effectively the normal operation of Outer Cooler 3-1.
The secondary magma of discharging from the discharge port of Oslo crystallizer 3-2 bottom is pumped in thickener 4 by crystallization discharging pump 11, and secondary magma is separated into three magmas and three clear liquids further eliminate degree of supersaturation in thickener 4 after.The overflow port of three clear liquids of gained from thickener 4 tops overflows, and is discharged into mother liquor tank 6.Three magmas that gained solid content is higher are discharged from the discharge port of thickener 4 bottoms, then enter and in whizzer 5, carry out centrifuging treatment, three times magma is separated into potassium primary phosphate solid and centrifugate in whizzer 5, gained potassium primary phosphate solid is discharged from the discharge port of whizzer 5, and through products export 17, enters potassium primary phosphate solid drying, packing department along pipeline.Gained centrifugate is discharged from the leakage fluid dram of whizzer 5, and enters mother liquor tank 6 along pipeline.
Mother liquor in mother liquor tank 6 is discharged from the liquid outlet of mother liquor tank 6 bottoms, and through mother liquor outlet 18, enters mother liquid disposal system and the discharging hole through thickener 4 bottoms enters thickener 4 respectively through mother liquor pump 12.
The state of a magma of discharging from the discharge port of one-level successive flash vaporization crystallizer 2, the secondary magma of discharging from the discharge port of secondary continuous cooling crystallizer 3 and three magmas of discharging from the discharge port of thickener 4 sees the following form 1.
Table 1
| ? | A magma | Secondary magma | Three magmas |
| Temperature/℃ | 62 | 41 | 41 |
| Concentration/the % of contained liquid in magma | 34.4 | 25.6 | 25.4 |
The mean particle size of gained solid phosphoric acid potassium dihydrogen crystal is 0.3mm, and after former stirring pot type crystallization treatment, the mean particle size of the potassium dihydrogen phosphate crystal of gained is 0.15mm, and novel process goes out greatly 1 times than the crystal mean particle size of old technology.
The plant personnel required of this continuous crystallisation technique is: crystallization operation 2 people/classes, take up an area for long 18m * wide 10m.
Embodiment 2
The difference of the present embodiment and embodiment 1 is: the potassium dihydrogen phosphate of feed liquid to be crystallized for producing by ion exchange method, and the material state of feed liquid to be crystallized is: temperature is 96 ℃, concentration is 44.1%.
The opening for feed of one-level successive flash vaporization crystallizer 2 is connected with dynamic filter, and the opening for feed of dynamic filter is connected with liquor inlet 14 to be crystallized.
Feed liquid to be crystallized enters in dynamic filter with the inlet amount of 6430kg/h, from dynamic filter feed liquid to be crystallized out, enters DTB vacuum cyrsytalliser.The flow velocity of secondary clear liquid in the tube side of Outer Cooler 3-1 is 1.65m/s.
The state of a magma of discharging from the discharge port of one-level successive flash vaporization crystallizer 2, the secondary magma of discharging from the discharge port of secondary continuous cooling crystallizer 3 and three magmas of discharging from the discharge port of thickener 4 sees the following form 2.
Table 2
| ? | A magma | Secondary magma | Three magmas |
| Temperature/℃ | 63 | 42 | 42 |
| Concentration/the % of contained liquid in magma | 34.8 | 26.0 | 25.6 |
The mean particle size of gained solid phosphoric acid potassium dihydrogen crystal is 0.4mm, and after former stirring pot type crystallization treatment, the mean particle size of the potassium dihydrogen phosphate crystal of gained is 0.15mm, and novel process goes out greatly 1.67 times than the crystal mean particle size of old technology.
The plant personnel required of this continuous crystallisation technique is: crystallization operation 2 people/classes, take up an area for long 15m * wide 6m.
Embodiment 3
The difference of the present embodiment and embodiment 1 is: the potassium dihydrogen phosphate of feed liquid to be crystallized for producing by ion exchange method, and the material state of feed liquid to be crystallized is: temperature is 93 ℃, concentration is 39.6%.
Feed liquid to be crystallized enters DTB vacuum cyrsytalliser with the inlet amount of 12380kg/h.The flow velocity of secondary clear liquid in the tube side of Outer Cooler 3-1 is 1.8m/s.
The state of a magma of discharging from the discharge port of one-level successive flash vaporization crystallizer 2, the secondary magma of discharging from the discharge port of secondary continuous cooling crystallizer 3 and three magmas of discharging from the discharge port of thickener 4 sees the following form 3.
Table 3
| ? | A magma | Secondary magma | Three magmas |
| Temperature/℃ | 63 | 40 | 40 |
| Concentration/the % of contained liquid in magma | 34.7 | 25.3 | 25.1 |
The mean particle size of gained solid phosphoric acid potassium dihydrogen crystal is 0.35mm, and after former stirring pot type crystallization treatment, the mean particle size of the potassium dihydrogen phosphate crystal of gained is 0.15mm, and novel process goes out greatly 1.33 times than the crystal mean particle size of old technology.
The plant personnel required of this continuous crystallisation technique is: crystallization operation 2 people/classes, take up an area for long 17m * wide 8m.
Claims (5)
1. potassium primary phosphate continuous crystallisation technique, is characterized in that: the secondary continuous crystallisation mode that adopts flash crystallization to add crystallisation by cooling obtains potassium primary phosphate solid, and the idiographic flow of described secondary continuous crystallisation is:
A, the opening for feed of the feed liquid to be crystallized of coming from liquor inlet to be crystallized (14) from one-level successive flash vaporization crystallizer (2) bottom passes into one-level successive flash vaporization crystallizer (2), described feed liquid to be crystallized is lowered the temperature in one-level successive flash vaporization crystallizer (2), crystallization, be separated into clear liquid one time, magma and secondary steam, magma of gained is discharged and is entered mother liquor tank (6) along pipeline from the discharge port of one-level successive flash vaporization crystallizer (2) bottom, clear liquid of gained is discharged from the relief outlet at one-level successive flash vaporization crystallizer (2) middle part, gained secondary steam is discharged through secondary steam outlet (13) from the air outlet at one-level successive flash vaporization crystallizer (2) top,
B, a magma of discharging from the discharge port of one-level successive flash vaporization crystallizer (2) bottom be admitted in secondary continuous cooling crystallizer (3) lower the temperature, crystallization; Described secondary continuous cooling crystallizer (3) consists of Oslo crystallizer (3-2) and Outer Cooler (3-1); A described magma is admitted to the central downtake at Oslo crystallizer (3-2) top, and along central downtake, arrive the bottom of Oslo crystallizer (3-2) inner chamber, then from the bottom of Oslo crystallizer (3-2), rising through fluidised crystallization bed, there is crystallization and forms secondary magma and secondary clear liquid in a magma herein; Secondary magma is discharged from the discharge port of Oslo crystallizer (3-2) bottom, secondary clear liquid continues to move up to upper straight section, the crystallisation cycle pump (10) that a part for secondary clear liquid is arranged at Oslo crystallizer (3-2) top pumps into Outer Cooler (3-1) to carry out heat exchange and shifts out entrained heat, secondary clear liquid after heat exchange is discharged from the discharge port of Outer Cooler (3-1), and the central downtake that enters Oslo crystallizer (3-2) top mixes with a magma, form a circulation loop; Another part of secondary clear liquid overflows and enters mother liquor tank (6) by pipeline from the overflow port on the top of Oslo crystallizer (3-2);
C, the secondary magma of discharging from the discharge port of Oslo crystallizer (3-2) bottom are admitted to thickener (4) and carry out thickening processing, described secondary magma is separated into three clear liquids and three magmas in thickener (4), three magmas of gained are discharged from the discharge port of thickener (4) bottom, and the overflow port of three clear liquids of gained from thickener (4) top overflows and enter mother liquor tank (6) by pipeline;
D, three magmas of discharging from thickener (4) bottom are admitted in whizzer (5) and carry out centrifuging treatment, described three magmas are separated into potassium primary phosphate solid and centrifugate in whizzer (5), described potassium primary phosphate solid is from the discharge port of whizzer (5) and through products export (17) discharge, and described centrifugate escapes and enter mother liquor tank (6) in whizzer (5).
2. potassium primary phosphate continuous crystallisation technique according to claim 1, is characterized in that: the mother liquor in described mother liquor tank (6) is pumped to thickener (4) another part by mother liquor pump (12) part and discharges from mother liquor outlet (18); Described Outer Cooler (3-1) is shell and tube heat exchanger, adopt water quench mode, from cooling water inlet, (19) enter the shell-side of Outer Cooler (3-1) to described water coolant, water coolant after heat exchange is discharged through cooling water outlet (20) and is discharged from Outer Cooler (3-1), and described water coolant carries out pump circulation by cooling water circulating pump (9) in Outer Cooler (3-1).
3. potassium primary phosphate continuous crystallisation technique according to claim 2, is characterized in that: described Outer Cooler (3-1) is equipped with cleaning system, and the rate of flow of fluid in the heat transfer tube of Outer Cooler (3-1) is 1.5m/s～1.8m/s.
4. potassium primary phosphate continuous crystallisation technique according to claim 1, is characterized in that: described one-level successive flash vaporization crystallizer (2) is DTB vacuum cyrsytalliser; The feed liquid that contains thin crystalline substance that overflow port from DTB vacuum cyrsytalliser middle part overflows is pumped into and in thin brilliant eliminator (1), adds brilliant processing of thermosol and eliminate crystallite by the thin brilliant pump (7) of eliminating, eliminate the feed liquid of crystallite and discharge and enter DTB vacuum cyrsytalliser from the opening for feed of DTB vacuum cyrsytalliser bottom from the discharge port of thin brilliant eliminator (1), form a circulation loop; Described thin brilliant eliminator (1) is shell and tube heat exchanger, takes steam heating mode.
5. according to the arbitrary described potassium primary phosphate continuous crystallisation technique of claim 1 or 4, it is characterized in that: after described flow process A processes, the temperature that enters a magma before flow process B is 60 ℃～65 ℃.
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| CN1789117A (en) * | 2004-12-14 | 2006-06-21 | 自贡鸿鹤化工股份有限公司 | Method for producing potassium dihydrogen phosphate and gypsum using hydrochloric acid method |
| CN102424374A (en) * | 2011-09-07 | 2012-04-25 | 湖北三宁化工股份有限公司 | Production method of potassium dihydrogen phosphate |
| CN202410226U (en) * | 2012-01-12 | 2012-09-05 | 中粮生物化学（安徽）股份有限公司 | Continuous evaporation crystallization device |
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2013
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