CN111573646A - Preparation method of disodium hydrogen phosphate large particles by double-effect crystallization method - Google Patents
Preparation method of disodium hydrogen phosphate large particles by double-effect crystallization method Download PDFInfo
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- CN111573646A CN111573646A CN202010253182.9A CN202010253182A CN111573646A CN 111573646 A CN111573646 A CN 111573646A CN 202010253182 A CN202010253182 A CN 202010253182A CN 111573646 A CN111573646 A CN 111573646A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
- C01B25/301—Preparation from liquid orthophosphoric acid or from an acid solution or suspension of orthophosphates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
- B01D9/0031—Evaporation of components of the mixture to be separated by heating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
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Abstract
The invention discloses a preparation method of disodium hydrogen phosphate large particles by a double-effect crystallization method, which comprises the steps of crystallizing a sodium phosphate product in a double-effect crystallization mode, and producing a disodium hydrogen phosphate large particle product by combining a secondary acid and alkali adding recrystallization process; on one hand, as the continuous feeding and concentration can be realized, the stability of crystal particles is ensured, the product percent of pass is improved, the steam balance and stability of the system are ensured, and the steam consumption is reduced; on the other hand, the double-effect concentration crystallization process is combined with a secondary acid and alkali adding recrystallization process, so that fine crystal particles continue to grow into medium coarse particles, and large-particle products of the disodium hydrogen phosphate dihydrate can be produced.
Description
Technical Field
The invention relates to a preparation method of disodium hydrogen phosphate large particles, in particular to a method for producing sodium phosphate by adopting a double-effect crystallization method, crystallizing a sodium phosphate product in a double-effect crystallization mode, and combining a secondary acid and alkali adding recrystallization process to produce a disodium hydrogen phosphate dihydrate large particle product.
Background
The traditional production process flow of sodium phosphate is as follows: and (3) pumping the disodium hydrogen phosphate neutralization solution prepared in the neutralization process into a concentration kettle through a feeding pump, simultaneously starting the concentration kettle for stirring, paying attention to the liquid level of the concentration kettle, starting an atmospheric condenser water supply pump of the concentration kettle while feeding, and closing an emptying valve of the concentration kettle. And after the feeding is finished, backflushing the feeding pipeline by using steam, stopping the feeding pump and the feeding valve of the concentration kettle, and starting the steam valve of the tube-array heater of the concentration kettle to start concentration. When the concentration is ready for a large amount of particles, the circulating water pump is turned off and emptied. And opening a discharge valve of the concentration kettle, putting the material into the crystallization kettle, naturally cooling to 65-80 ℃, and taking out for dehydration.
This discontinuous feed concentration process suffers from the following drawbacks: 1. the crystal particles are easy to fluctuate greatly, and the product percent of pass is influenced; 2. the steam is also used discontinuously, which is not beneficial to the steam balance of the production system; 3. the steam consumption is large, and the steam consumption is increased.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of large fluctuation of crystallized particles and large steam consumption in the discontinuous feeding concentration process adopted in the production of sodium phosphate in the prior art, and provides a method for preparing large disodium hydrogen phosphate particles by a continuous feeding concentration double-effect crystallization method.
In order to solve the technical problems, the invention provides the following technical scheme:
firstly, material flow:
a preparation method of disodium hydrogen phosphate large particles by a double-effect crystallization method comprises the following specific steps:
s1, conveying the disodium hydrogen phosphate dilute solution to a two-effect separator through a feeding pump, then conveying the solution into a tube pass of a two-effect heater after kinetic energy is obtained by a two-effect circulating pump, heating the solution to a boiling point, conveying the solution into the two-effect separator to finish solvent vaporization and vapor-liquid separation, conveying a liquid phase of the two-effect separator into the two-effect circulating pump, and conveying the two-effect finished solution pressurized by the two-effect circulating pump into the next circulation;
s2, pressurizing the double-effect finished liquid by a double-effect discharge pump, then feeding the liquid into a single-effect evaporation crystallizer, then feeding the liquid into a single-effect circulating pump, feeding the liquid into a single-effect heater tube pass after the single-effect circulating pump obtains kinetic energy, heating the liquid to a boiling point, and feeding the liquid into the single-effect evaporation crystallizer to finish solvent vaporization and vapor-liquid separation again;
and S3, adding phosphoric acid and caustic soda into the primary-effect evaporation crystallizer again for neutralization, and performing secondary recrystallization to ensure that fine crystal particles in the primary-effect evaporation crystallizer continue to grow into medium coarse particles, thereby producing the large-particle disodium hydrogen phosphate dihydrate product.
Second, steam and noncondensable gas flow path
One part of primary-effect secondary steam generated by the primary-effect evaporation crystallizer enters the TVR heat pump, and the TVR heat pump carries out thermal compression on the primary-effect secondary steam by taking the generated steam as power; compressed steam of the TVR heat pump enters a shell pass of the single-effect heater to provide effective heat transfer temperature difference for system evaporation;
the other part of the primary steam enters the shell pass of the double-effect heater to become a heat source of the double-effect evaporation; and the secondary steam generated by the secondary evaporation enters the shell pass of the condenser and exchanges heat with the cooling water of the tube pass of the condenser, so that the secondary steam is condensed on the shell pass of the condenser.
The non-condensable gas of the system is discharged from the shell passes of the primary-effect heater and the secondary-effect heater, and enters the shell pass of the condenser together with the secondary steam for condensation; the residual non-condensable gas is pumped by a vacuum pump and exhausted to the atmosphere.
Third, condensed water flow
Condensed water of the two-effect heater, the one-effect heater and the condenser is concentrated into a condensed water tank, and is finally discharged out of the system after being pressurized by a condensed water pump.
Furthermore, the two-effect heater and the one-effect heater are forced circulation heaters.
Further, a thickener is integrated at the lower part of the first-effect evaporative crystallizer, a mother liquor phase of the first-effect evaporative crystallizer enters the thickener through a bottom flow pipeline and then is settled to the bottom of the thickener to form thickened crystal slurry, the thickened crystal slurry is detected on line through a densimeter arranged on a crystal slurry circulating pipeline, and the thickened crystal slurry is discharged out of the system when the detected density reaches a set value; the mother liquor of the less dense one-effect evaporative crystallizer is gathered at the upper part of the thickener, then enters the one-effect circulating pump, is pressurized by the one-effect circulating pump, and then enters the tube side of the one-effect heater to be continuously concentrated and crystallized.
Has the advantages that:
the invention adopts a double-effect crystallization method to prepare the large disodium hydrogen phosphate particles, on one hand, the crystallization particles are ensured to be stable and the product percent of pass is improved because the continuous feeding and concentration can be carried out, the product percent of pass is improved to 80 percent of the patent from about 50 percent of the traditional process, the steam balance and stability of the system are ensured, the steam consumption is reduced, and the steam consumption is reduced to 2t/h from 2.5t/h of the traditional process; on the other hand, the double-effect concentration crystallization process is combined with a secondary acid and alkali adding recrystallization process, so that fine crystal particles continue to grow into medium coarse particles, and large-particle products of the disodium hydrogen phosphate dihydrate can be produced.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic diagram of a system for preparing large disodium hydrogen phosphate particles by a double-effect crystallization method according to the present invention;
1, a one-effect evaporative crystallizer; 2, a two-effect separator; 3, a one-effect heater; 4, a double-effect heater; 5, a condenser; 6, a condensed water tank; 7, a clear liquid groove; 8, a feed pump; 9, a two-effect circulating pump; 10, a double-effect discharge pump; 11, a one-effect circulating pump; 12, a crystal slurry circulating pump; 13, a condensate pump; 14, a vacuum pump; 15, TVR heat pump.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Examples
A preparation method of disodium hydrogen phosphate large particles by a double-effect crystallization method comprises the following specific steps:
firstly, material flow:
s1, feeding a disodium hydrogen phosphate dilute solution with a dry matter content of 43.7% to a two-effect separator 2 through a feeding pump 8, then feeding the solution into a tube pass of a two-effect heater 4 after kinetic energy is obtained by a two-effect circulating pump 9, wherein the two-effect heater 4 is a forced circulation type heater, the material is forced to circulate and flow in the tube pass of the two-effect heater 4, heat exchange is carried out between the material and steam of a shell pass in the flowing process, the material is heated to a boiling point by latent heat generated by condensation of the steam of the shell pass, the material heated to the boiling point enters the two-effect separator 2 to complete solvent vaporization and vapor-liquid separation, a liquid phase of the two-effect separator 2 enters the two-effect circulating pump 9, and the two-effect completion liquid pressurized by the two-effect circulating pump;
s2, pressurizing the double-effect finished liquid by a double-effect discharge pump 10, then feeding the pressurized liquid into a single-effect evaporative crystallizer 1, then feeding the pressurized liquid into a single-effect circulating pump 11, feeding the pressurized liquid into a single-effect heater 3 after the kinetic energy of the single-effect circulating pump 11 is obtained, heating the liquid to a boiling point, feeding the heated liquid into the single-effect evaporative crystallizer, and finishing solvent vaporization and vapor-liquid separation again;
the first-effect heater 3 is a forced circulation type heater, materials are forced to flow circularly on the tube side of the first-effect heater 3, heat exchange is carried out between the materials and steam on the shell side in the flowing process, and the materials are heated to the boiling point by latent heat released by condensation of the steam on the shell side.
The lower part of the single-effect evaporative crystallizer 1 is integrated with an integrated thickener, the liquid phase of the single-effect evaporative crystallizer 1 enters the thickener through a bottom flow pipeline, and the crystal particles with higher density are settled to the bottom of the thickener under the action of gravity to form thickened crystal slurry. Through the online detection of a densimeter arranged on the crystal mush circulating pipeline, when the detected density reaches a set value (about 1.83kg/L), the qualified thickened crystal mush is discharged out of the system after the crystal mush circulating pump 12 obtains kinetic energy. The mother liquor with lower density is gathered at the upper part of the thickener, then enters the first-effect circulating pump 11, is pressurized by the first-effect circulating pump 11, and then enters the tube side of the first-effect heater 3 to be continuously concentrated and crystallized.
S3, on the basis of double-effect concentration crystallization, adding 80% phosphoric acid and 32% caustic soda into the single-effect evaporative crystallizer 1 for neutralization again, and performing secondary recrystallization to enable fine crystal particles in the single-effect evaporative crystallizer 1 to continue to grow into medium and coarse particles, so that a large-particle disodium hydrogen phosphate dihydrate product is produced;
secondly, steam and noncondensable gas flow:
a part of primary-effect secondary steam generated by the primary-effect evaporative crystallizer 1 enters the TVR heat pump 15, and the TVR heat pump 15 carries out thermal compression on the primary-effect secondary steam by taking the generated steam as power; compressed steam of the TVR heat pump 15 enters a shell pass of the primary heater 3 to provide effective heat transfer temperature difference for system evaporation;
the other part of the primary steam enters the shell pass of the secondary heater 4 to become a heat source for secondary evaporation; the secondary steam generated by the secondary evaporation enters the shell pass of the condenser 5, and exchanges heat with the cooling water of the tube pass of the condenser, so that the secondary steam is condensed in the shell pass of the condenser 5;
the non-condensable gas of the system is discharged from the first-effect heater 3 and the second-effect heater 4 and the shell pass, enters the shell pass of the condenser 5 together with the second-effect secondary steam, and is subjected to heat exchange with the tube pass cooling water, so that the water vapor carried by the non-condensable gas is completely condensed. Finally, the non-condensable gas is pumped by a vacuum pump 14 and exhausted to the atmosphere, so that the system is ensured to operate in a designed vacuum state.
Third, condensed water flow
Condensed water of the two-effect heater 4, the one-effect heater 3 and the condenser 5 is concentrated into the condensed water tank 6, and is finally pressurized by the condensed water pump 13 and discharged out of the system.
Comparative experiment:
by comparison experiments, the method for preparing the large disodium hydrogen phosphate particles by the double-effect crystallization method is used for producing the disodium hydrogen phosphate dihydrate, and is compared with the method for producing the disodium hydrogen phosphate dihydrate by the traditional intermittent feeding and concentrating process.
The production device is simulated, and a secondary acid and alkali adding recrystallization process is adopted in a laboratory to produce a dihydrate disodium hydrogen phosphate large-particle product, and the production device specifically comprises the following steps:
firstly, taking about 22L of dihydrate disodium hydrogen phosphate neutralization solution, putting the dihydrate disodium hydrogen phosphate neutralization solution into a 70L ceramic reaction kettle, introducing low-pressure steam into a reaction kettle jacket for heat tracing, ensuring that the temperature in the whole reaction process is about 80 ℃, and stirring the whole reaction process.
Secondly, adding about 2.2L of 75 percent phosphoric acid into the reaction kettle, controlling the time to be finished within 10 minutes, and adjusting the pH of the mother liquor to be 6.54 and the solid-to-liquid ratio of the mother liquor to be 18 percent.
③ after the acid is added, about 2.65L of 50 percent sodium hydroxide is added into the reaction kettle, the time is controlled to be about 30 minutes, the PH of the mother liquor is adjusted to be 8.43, and the specific gravity of the mother liquor is 1.65 g/ml. Because the evaporation rate of the reaction kettle is high, the solid-liquid ratio of the mother liquor is higher than 50%, and then the water is added for dilution adjustment.
Note: the base addition was slow, the addition rate was controlled at 3mL/s, and the base addition tube was inserted below the liquid level.
Fourthly, after the alkali is added, the reaction stays for 10 minutes, the reaction solution is taken out to a centrifuge for dehydration, the dehydrated material is dried, and the prepared sample is sent to a laboratory for analysis.
Comparative analysis of test results with conventional discontinuous feed concentration process
Analytical reports of the products obtained from both processes:
as can be seen from the above table, the process of the present invention enables the production of large particles of disodium hydrogen phosphate dihydrate.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A preparation method of disodium hydrogen phosphate large particles by a double-effect crystallization method is characterized by comprising the following steps:
s1, conveying the disodium hydrogen phosphate dilute solution to a two-effect separator through a feeding pump, then conveying the solution into a tube pass of a two-effect heater after kinetic energy is obtained by a two-effect circulating pump, heating the solution to a boiling point, conveying the solution into the two-effect separator to finish solvent vaporization and vapor-liquid separation, conveying a liquid phase of the two-effect separator into the two-effect circulating pump, and conveying the two-effect finished solution pressurized by the two-effect circulating pump into the next circulation;
s2, pressurizing the double-effect finished liquid by a double-effect discharge pump, then feeding the liquid into a single-effect evaporation crystallizer, then feeding the liquid into a single-effect circulating pump, feeding the liquid into a single-effect heater tube pass after the single-effect circulating pump obtains kinetic energy, heating the liquid to a boiling point, and feeding the liquid into the single-effect evaporation crystallizer to finish solvent vaporization and vapor-liquid separation again;
and S3, adding phosphoric acid and caustic soda into the primary-effect evaporation crystallizer again for neutralization, and performing secondary recrystallization to ensure that fine crystal particles in the primary-effect evaporation crystallizer continue to grow into medium coarse particles, thereby producing the large-particle disodium hydrogen phosphate dihydrate product.
2. The method for preparing disodium hydrogen phosphate granules by double effect crystallization as claimed in claim 1, wherein the condensed water from the double effect heater, the single effect heater and the condenser is collected into a condensed water tank, and finally discharged out of the system after being pressurized by a condensed water pump.
3. The method of claim 1, wherein the double effect heater and the single effect heater are forced circulation heaters.
4. The method for preparing disodium hydrogen phosphate large particles by double effect crystallization of claim 1, wherein the thickener is integrated at the lower part of the single effect evaporative crystallizer, the mother liquor phase of the single effect evaporative crystallizer enters the thickener through an underflow pipe and then settles to the bottom of the thickener to become thickened magma, the thickened magma is detected on line by a densimeter arranged on a magma circulating pipe, and the thickened magma is discharged out of the system when the detected density reaches a set value.
5. The method for preparing large disodium hydrogen phosphate particles by double-effect crystallization of claim 4, wherein the mother liquor of the less dense single-effect evaporative crystallizer is accumulated at the upper part of the thickener, and then enters the single-effect circulating pump, and after being pressurized by the single-effect circulating pump, the mother liquor enters the tube side of the single-effect heater to be continuously concentrated and crystallized.
6. The method of claim 1, wherein a portion of the primary steam generated from the primary evaporative crystallizer enters the TVR heat pump, and the TVR heat pump uses the raw steam as power to perform thermal compression on the primary steam; compressed steam of the TVR heat pump enters a shell pass of the single-effect heater to provide effective heat transfer temperature difference for system evaporation;
the other part of the primary steam enters the shell pass of the double-effect heater to become a heat source of the double-effect evaporation; and the secondary steam generated by the secondary evaporation enters the shell pass of the condenser and exchanges heat with the cooling water of the tube pass of the condenser, so that the secondary steam is condensed on the shell pass of the condenser.
7. The method for preparing the large disodium hydrogen phosphate particles by the double-effect crystallization method as claimed in claim 1, wherein the non-condensable gas of the system is discharged from the shell sides of the primary heater and the secondary heater and enters the shell side of the condenser together with the secondary steam for condensation; the residual non-condensable gas is pumped by a vacuum pump and exhausted to the atmosphere.
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