CN113797562A - Evaporative crystallization method and system - Google Patents
Evaporative crystallization method and system Download PDFInfo
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- CN113797562A CN113797562A CN202010538082.0A CN202010538082A CN113797562A CN 113797562 A CN113797562 A CN 113797562A CN 202010538082 A CN202010538082 A CN 202010538082A CN 113797562 A CN113797562 A CN 113797562A
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- 238000002425 crystallisation Methods 0.000 title claims abstract description 52
- 239000002002 slurry Substances 0.000 claims abstract description 193
- 239000007788 liquid Substances 0.000 claims abstract description 125
- 238000011010 flushing procedure Methods 0.000 claims abstract description 92
- 238000001704 evaporation Methods 0.000 claims abstract description 78
- 230000008020 evaporation Effects 0.000 claims abstract description 58
- 150000003839 salts Chemical class 0.000 claims abstract description 51
- 230000008025 crystallization Effects 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 44
- 238000007599 discharging Methods 0.000 claims abstract description 32
- 238000012544 monitoring process Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 85
- 239000000463 material Substances 0.000 claims description 42
- 238000000926 separation method Methods 0.000 claims description 36
- 239000012452 mother liquor Substances 0.000 claims description 28
- 238000011001 backwashing Methods 0.000 claims description 14
- 239000013078 crystal Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 229920006395 saturated elastomer Polymers 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 6
- 238000004891 communication Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000011144 upstream manufacturing Methods 0.000 claims description 3
- 238000005265 energy consumption Methods 0.000 abstract description 9
- 230000008901 benefit Effects 0.000 abstract description 7
- 238000004140 cleaning Methods 0.000 abstract description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 24
- 239000011780 sodium chloride Substances 0.000 description 14
- 239000010842 industrial wastewater Substances 0.000 description 12
- 101100298222 Caenorhabditis elegans pot-1 gene Proteins 0.000 description 10
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 10
- 239000002245 particle Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
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- 239000007832 Na2SO4 Substances 0.000 description 3
- 239000012267 brine Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 210000004911 serous fluid Anatomy 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- -1 salt ions Chemical class 0.000 description 2
- 239000002562 thickening agent Substances 0.000 description 2
- 101100298225 Caenorhabditis elegans pot-2 gene Proteins 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 239000011552 falling film Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
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- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0094—Evaporating with forced circulation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
- B01D1/305—Demister (vapour-liquid separation)
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/043—Details
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/01—Density
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/03—Pressure
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/10—Solids, e.g. total solids [TS], total suspended solids [TSS] or volatile solids [VS]
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/04—Flow arrangements
- C02F2301/046—Recirculation with an external loop
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/14—Maintenance of water treatment installations
Abstract
The present disclosure relates to a method and a system for evaporative crystallization, wherein the operation of discharging the lower concentrated slurry from the evaporation tank through a slurry discharge pipeline comprises a first positive flushing, a back flushing, a slurry discharge and a second positive flushing which are sequentially performed. This is disclosed through carrying out real-time on-line monitoring to the solid-to-liquid ratio of upper concentrated thick liquid, has realized the automatic of the interior salt thick liquid of evaporating pot and has got rid of and the self-cleaning of pipeline, has ensured the steady operation of evaporation crystallization process, improves the productivity and the quality of crystallization salt, has the advantage that the suitability is strong, the device operation is stable, energy consumption and operating cost are low simultaneously.
Description
Technical Field
The disclosure relates to the field of solid-liquid separation, in particular to a method and a system for evaporative crystallization.
Background
In inorganic salt chemical industry and water treatment industry, salt ions in brine are generally precipitated in the form of crystalline salt solids by an evaporative crystallization process, so that solid-liquid separation is realized. The crystallization treatment of the salt-containing water comprises a hot method and a cold method: the cold crystallization method mainly adopts a cooling medium to cool the brine until salt crystals are separated out; the thermal crystallization mainly includes multiple-effect evaporation, falling film evaporation, Mechanical Vapor Recompression (MVR) technique and other methods.
To the concentrated process of salt-containing water, along with moisture constantly evaporates in the evaporating pot, salinity concentration risees, reaches the saturated concentration of salt after, further concentration, can separate out salt crystallization solid particle in the salt water, when it reaches certain content, in time eduction gear. In the prior art, a manual salt discharging mode is usually adopted, on one hand, the operation is carried out according to personal experience, more manpower is consumed, the salt discharging is not thorough enough, pipelines and equipment are easy to block, and the device is stopped in serious cases; on the other hand, salt solid particles are remained in the salt discharge pipeline, so that the valve is not closed tightly, concentrated feed liquid can continuously enter the separation device, and the normal operation of the solid separation device is influenced.
Disclosure of Invention
The invention aims to provide a method and a system for evaporative crystallization, which can realize automatic discharge of slurry in an evaporation tank and automatic cleaning of pipelines and have the advantages of stable operation, high operation flexibility, easiness in control and the like.
In order to achieve the above object, a first aspect of the present disclosure provides a method of evaporative crystallization, the method comprising:
s1: after heat exchange, introducing the material to be evaporated containing salt water into an evaporation tank for evaporation to obtain steam and concentrated slurry; the concentrated slurry comprises an upper layer of concentrated slurry and a lower layer of concentrated slurry;
s2: leading out and mixing the upper concentrated slurry of the concentrated slurry into the material to be evaporated, and then returning to perform the heat exchange and the evaporation;
s3: carrying out real-time online monitoring on the solid-liquid ratio of the upper concentrated slurry, and discharging the lower concentrated slurry from the evaporation tank through a slurry discharge pipeline and carrying out solid-liquid separation to obtain crystals and a mother solution when the real-time solid-liquid ratio of the upper concentrated slurry is greater than the critical solid-liquid ratio;
s4: doping the mother liquor into the material to be evaporated, and then returning to perform the heat exchange and the evaporation;
and the operation of discharging the lower layer concentrated slurry from the evaporation tank through a slurry discharge pipeline comprises a first positive flushing, a back flushing, a slurry discharge and a second positive flushing which are sequentially carried out.
Optionally, an outlet of a flushing line is arranged between the inlet and the outlet of the slurry discharge line; the operation of discharging the lower concentrated slurry from the evaporation tank through a slurry discharge line comprises:
SS1, closing the inlet of the slurry discharge pipeline and opening the outlet of the slurry discharge pipeline; introducing rinse water through the rinse line for the first positive rinse;
SS2, opening the inlet of the slurry discharge pipeline and closing the outlet of the slurry discharge pipeline; introducing rinse water through the rinse line for the backwash;
SS3, closing the inlet of the flushing pipeline and opening the outlet of the pulp discharge pipeline; carrying out slurry discharge on the lower layer concentrated slurry in the evaporation tank through a slurry discharge pipeline until the real-time solid-liquid ratio of the upper layer concentrated slurry is smaller than the critical solid-liquid ratio, and closing an inlet of the slurry discharge pipeline;
SS4, opening the inlet of the flush line, introducing flush water through the flush line for the second positive flush, and then closing the outlet of the discharge line.
Alternatively, the critical solid-to-liquid ratio is any value in the range of 0.15 to 0.3 times the ratio of the saturated density of the upper concentrated slurry to the density of water.
Optionally, performing real-time online monitoring on the solid-to-liquid ratio of the upper concentrated slurry by using an online detector to obtain the real-time solid-to-liquid ratio;
the online detector is an online solid content detector, a density detector or a pressure detector.
Optionally, the time of the first positive flush is 1-10 minutes; the backwashing time is 1-5 minutes; the time of the second positive flushing is 1-6 minutes; the flow rate of the washing water is 1-10 m/s.
Optionally, the first positive flush further comprises: monitoring the amount of water in the first positive flush;
wherein the ratio of the lumen volume of the flush line to the volume of the first positively flushed volume of water is 1: 0.1-15.
Optionally, the backwashing further comprises: monitoring the amount of the backwashing water;
wherein the ratio of the volume of the lumen of the flushing line to the volume of the amount of water for backwashing is 1: 0.1-12.
Optionally, the second positive flush further comprises: monitoring the amount of water in the second positive flush;
wherein the ratio of the volume of the lumen of the flush line to the volume of the second volume of positive flush is 1: 0.1-12.
A second aspect of the present disclosure provides a system for evaporative crystallization using the method of the first aspect of the present disclosure, the system comprising an evaporative crystallization unit, a slurry discharge and flushing unit and a solid-liquid separation unit which are sequentially arranged; the evaporative crystallization unit comprises an evaporation tank and a material circulation pipeline positioned outside the evaporation tank; the material circulating pipeline comprises a raw material inlet, a mother liquid circulating inlet and a heating chamber which are sequentially arranged along the material flow direction;
the solid-liquid separation unit comprises a solid-liquid separation device and a mother liquor circulating pipeline, and the solid-liquid separation device is provided with a slurry inlet, a mother liquor outlet and a crystallization pipeline outlet; the mother liquid outlet is communicated with the inlet of the mother liquid circulating pipeline, and the outlet of the mother liquid circulating pipeline is communicated with the mother liquid circulating inlet on the material circulating pipeline;
the slurry discharging and flushing unit comprises an automatic flushing control device, a slurry discharging pipeline and a flushing pipeline; the automatic flushing control device comprises an online detector, a first slurry discharge valve, a second slurry discharge valve, a first flushing water valve and a controller which are in communication connection with each other; the online detector is arranged at the bottom of the evaporation tank, or is arranged at the upstream of the raw material inlet on the material circulating pipeline and is used for detecting the real-time solid-liquid ratio of the evaporation tank; the entry of row's thick liquid pipeline set up in the bottom of evaporating pot, the export of row's thick liquid pipeline with thick liquid entry intercommunication, be provided with the export of flushing line between the entry of row's thick liquid pipeline and the export.
Optionally, the slurry discharge pipeline is sequentially provided with the first slurry discharge valve and a second slurry discharge valve along the material flow direction; the flushing pipeline is provided with the first flushing water valve; the controller is used for receiving the real-time solid-liquid ratio and controlling the opening and closing of the first slurry discharge valve, the second slurry discharge valve and the first flushing water valve according to the real-time solid-liquid ratio;
a flushing water flowmeter is also arranged on the flushing pipeline; and a material circulating pump is arranged on the material circulating pipeline between the mother liquid circulating inlet and the heating chamber, and a mother liquid circulating pump is arranged on the mother liquid circulating pipeline.
This is disclosed through carrying out real-time on-line monitoring to the solid-to-liquid ratio of upper concentrated thick liquid, has realized the automatic of the interior salt thick liquid of evaporating pot and has got rid of and the self-cleaning of pipeline, has ensured the steady operation of evaporation crystallization process, improves the productivity and the quality of crystallization salt, has the advantage that the suitability is strong, the device operation is stable, energy consumption and operating cost are low simultaneously.
Additional features and advantages of the disclosure will be set forth in the detailed description which follows.
Drawings
The accompanying drawings, which are included to provide a further understanding of the disclosure and are incorporated in and constitute a part of this specification, illustrate embodiments of the disclosure and together with the description serve to explain the disclosure without limiting the disclosure. In the drawings:
FIG. 1 is a schematic diagram of the structure of an evaporative crystallization system in example 1 of the present disclosure;
FIG. 2 is a schematic diagram of the structure of an evaporative crystallization system in example 2 of the present disclosure;
FIG. 3 is a schematic diagram of the structure of an evaporative crystallization system in example 3 of the present disclosure;
FIG. 4 is a schematic structural diagram of an evaporative crystallization system in example 4 of the present disclosure.
Description of the reference numerals
1. Evaporating pot 2, material circulating pump 3, heating chamber
3a, a heating chamber 4, a salt slurry tank 5, a salt slurry pump
6.1# solid-liquid separation device 7.2# solid-liquid separation device 8 mother liquor tank
9. Mother liquor circulating pump
102. Condensate 102a, 103, salt water lines
104. Material circulation pipeline 105, secondary steam 105a, secondary steam
106.1# flushing water 107, salt foot 108, and pulp discharge pipeline
109. Flushing pipeline 110, pumping salt slurry 111.1# salt-containing clear water
112. Salt-containing slurry 113.2# salt-containing clear water 114 crystalline salt
115. Mother liquor circulating pipeline 116, concentrated slurry 201 and flushing water valve
202. First slurry discharging valve 203, second slurry discharging valve
204. First flushing water valve 301, on-line detector
Detailed Description
The following detailed description of specific embodiments of the present disclosure is provided in connection with the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present disclosure, are given by way of illustration and explanation only, not limitation.
In the present disclosure, unless otherwise stated, the use of directional words such as "up" and "down" generally refers to the up and down of the device in normal use, and specifically refers to the orientation of the drawing in fig. 1. "inner and outer" are meant to refer to the profile of the device itself.
As shown in fig. 1, the present disclosure provides a method of evaporative crystallization, the method comprising: s1: after heat exchange, introducing the material to be evaporated containing salt water into an evaporation tank 1 for evaporation to obtain steam and concentrated slurry; the concentrated serous fluid comprises upper concentrated serous fluid and lower concentrated serous fluid; s2: leading out the upper concentrated slurry of the concentrated slurry, mixing the upper concentrated slurry with a material to be evaporated, and then returning to perform heat exchange and evaporation; s3: carrying out real-time online monitoring on the solid-liquid ratio of the upper concentrated slurry, and when the real-time solid-liquid ratio of the upper concentrated slurry is larger than the critical solid-liquid ratio, discharging the lower concentrated slurry from the evaporation tank 1 through a slurry discharge pipeline 108 and carrying out solid-liquid separation to obtain crystals and mother liquor; s4: doping the mother liquor into a material to be evaporated, and then returning to perform heat exchange and evaporation; wherein the operation of discharging the lower concentrated slurry from the evaporation tank 1 through the slurry discharge line 108 comprises a first positive washing, a back washing, a slurry discharge and a second positive washing in this order.
This is disclosed through carrying out real-time on-line monitoring to the solid-to-liquid ratio of upper concentrated thick liquid, has realized the automatic of the interior salt thick liquid of evaporating pot and has got rid of and the self-cleaning of pipeline, has ensured the steady operation of evaporation crystallization process, improves the productivity and the quality of crystallization salt, has the advantage that the suitability is strong, the device operation is stable, energy consumption and operating cost are low simultaneously.
According to the present disclosure, in order to discharge the lower concentrated slurry from the evaporation tank 1 through the slurry discharge line 108 when the real-time solid-to-liquid ratio is greater than the critical solid-to-liquid ratio, the first positive washing, the back washing, the slurry discharge, and the second positive washing may be sequentially performed. In one embodiment, an outlet of the flushing line 109 may be provided between the inlet and the outlet of the slurry discharge line 108 for slurry discharge and flushing with flushing water; in a further embodiment, the operation of discharging the lower concentrated slurry from the evaporation tank 1 through the slurry discharge line 108 may comprise: SS1, closing the inlet of the slurry discharge pipeline 108 and opening the outlet of the slurry discharge pipeline 108; introducing washing water through a washing line 109 to perform a first positive washing to ensure the inside of the slurry discharge line 108 is clean; SS2, opening the inlet of the slurry discharge pipeline 108 and closing the outlet of the slurry discharge pipeline 108; introducing washing water through the washing line 109 for back washing to form a brine mixture in the evaporation tank 1 to ensure smooth progress of the slurry discharge process; SS3, closing the inlet of the flushing line 109, opening the outlet of the slurry discharge line 108; discharging the lower layer concentrated slurry in the evaporation tank 1 through a slurry discharge pipeline 108 until the real-time solid-liquid ratio of the upper layer concentrated slurry is less than the critical solid-liquid ratio, and closing the inlet of the slurry discharge pipeline 108; SS4, opening the inlet of the flush line 109, introducing flush water through the flush line 109 for a second positive flush to discharge the saline slurry remaining in the slurry discharge line 108, and then closing the outlet of the slurry discharge line 108.
The method of determining the critical solid-to-liquid ratio according to the present disclosure is not limited and may be conventionally selected in the art, and in one embodiment, the critical solid-to-liquid ratio may be any value within a range of 0.15 to 0.3 times the ratio of the saturation density of the upper concentrated slurry to the density of water, preferably within a range of 0.2 to 0.25 times the ratio of the saturation density of the upper concentrated slurry to the density of water, depending on the crystallization operation conditions.
In an embodiment according to the present disclosure, in order to obtain a real-time solid-liquid ratio of the upper concentrated slurry, an online detector 301 may be installed on the tank body of the evaporation tank 1 or on a delivery line of the upper concentrated slurry to perform real-time online monitoring on the solid-liquid ratio of the upper concentrated slurry, and further in an embodiment, the online detector 301 may be an online solid content detector, a density detector, or a pressure detector, preferably an online solid content detector. Specifically, in the embodiment where the online detector 301 is an online solid content detector, the real-time solid-liquid ratio of the upper concentrated slurry can be directly calculated according to the ratio of the solid particle content to the liquid volume, so as to control the opening and closing of the valve; in an embodiment where the online detector 301 is a density detector, the method for determining the real-time solid-liquid ratio may be: according to the saturated density and the crystallized particle density of the upper concentrated slurry under the crystallization operation condition and the measured real-time density of the upper concentrated slurry, the real-time solid-liquid ratio is (the real-time density of the upper concentrated slurry-the saturated density of the upper concentrated slurry)/(the crystallized particles)Density-real-time density of the upper concentrated slurry), and calculating to obtain the real-time solid-liquid ratio of the upper concentrated slurry; in an embodiment where the online detector 301 is a pressure detector, the method for determining the real-time solid-liquid ratio may be: two points A and B with a certain height difference h are determined on the evaporating pot 1 and/or the material circulating pipeline 104, and the pressure value between the two points is respectively measured by a pressure detector and recorded as PA、PB(suppose PA＞PB) Pressure difference Δ P ═ PA-PBAnd calculating the real-time density rho of the upper concentrated slurry according to a formula delta P-rho gh (g is the gravity acceleration and is 9.8N/kg), and then calculating the real-time solid-liquid ratio of the upper concentrated slurry according to the implementation mode that the online detector 301 is a density detector.
According to the present disclosure, in order to clean the pipeline as much as possible in the flushing process, the flushing process may be performed within a certain time, and in one embodiment, the time of the first positive flushing may be 1 to 10 minutes; the backwashing time can be 1-5 minutes; the time for the second positive flush may be 1-6 minutes; in a further embodiment, the instantaneous flow rate of the flush line 109 may be 1-10 m/s.
To further control the water usage of the flushing process, and to save water as much as possible on the basis of the completed flushing, the water usage of the first forward flushing, the back flushing and the second forward flushing processes may be monitored in real time, and preferably, the volume ratio of the lumen volume of the flushing line 109 to the water volume of the first forward flushing may be 1: 0.1-15, the volume ratio of the lumen volume of the flush line 109 to the amount of water for backwash may be 1: 0.1-12, the volumetric ratio of the lumen volume of flush line 109 to the volume of water of the second positive flush may be 1: 0.1-12.
According to the present disclosure, in order to enable the above-described flushing process of the flushing water in the flushing line 109, the line pressure of the flushing line 109 may be higher than the line pressure of the slurry discharge line 108, the pressure in the evaporation tank 1 and the pressure in the apparatus for performing solid-liquid separation.
The second aspect of the present disclosure provides a system for evaporative crystallization by using the method of the first aspect of the present disclosure, the system comprising an evaporative crystallization unit, a slurry discharge and flushing unit and a solid-liquid separation unit which are arranged in sequence; the evaporative crystallization unit comprises an evaporation tank 1 and a material circulation pipeline 104 positioned outside the evaporation tank 1; the material circulating pipeline 104 comprises a raw material inlet, a mother liquid circulating inlet and a heating chamber 3 which are arranged in sequence along the material flow direction; the solid-liquid separation unit comprises a solid-liquid separation device and a mother liquor circulating pipeline 115, and the solid-liquid separation device is provided with a slurry inlet, a mother liquor outlet and a crystallization pipeline outlet; the mother liquor outlet is communicated with the inlet of a mother liquor circulating pipeline 115, and the outlet of the mother liquor circulating pipeline 115 is communicated with the mother liquor circulating inlet on the material circulating pipeline 104; the slurry discharging and flushing unit comprises an automatic flushing control device, a slurry discharging pipeline 108 and a flushing pipeline 109; the automatic flushing control device comprises an online detector 301, a first slurry discharge valve 202, a second slurry discharge valve 203, a first flushing water valve 204 and a controller which are in communication connection with each other; an inlet of the online detector 301 is arranged at the bottom of the evaporation tank 1, or an inlet of the slurry discharge pipeline 108 is arranged at the upstream of the raw material inlet on the material circulation pipeline 104, and is used for detecting the real-time solid-liquid ratio of the evaporation tank 1; an inlet of the slurry discharge pipe 108 is arranged at the bottom of the evaporation tank 1, an outlet of the slurry discharge pipe 108 is communicated with the slurry inlet, and an inlet of the flushing pipe 109 is arranged between the inlet and the outlet of the slurry discharge pipe 108.
This is disclosed through carrying out real-time on-line monitoring to the solid-to-liquid ratio in the outside circulation pipeline of evaporating pot or evaporating pot, has realized the automatic of the inside salt thick liquid of evaporating pot and has got rid of and the self-cleaning of pipeline, has ensured the steady operation of evaporation crystallization process, improves the productivity and the quality of crystallization salt, has the advantage that the suitability is strong, the device operation is stable, energy consumption and operating cost are low simultaneously.
In one embodiment, the slurry discharge pipeline 108 is provided with a first slurry discharge valve 202 and a second slurry discharge valve 203 in sequence along the material flow direction; the flush line 109 is provided with a first flush water valve 204; the controller is used for receiving the real-time solid-liquid ratio and controlling the opening and closing of the first slurry discharging valve 202, the second slurry discharging valve 203 and the first flushing water valve 204 according to the real-time solid-liquid ratio so as to complete slurry discharging of the evaporation tank 1 and flushing of the slurry discharging pipeline 108; in a further embodiment, a flushing water flow meter may be further disposed on the flushing line 109 to monitor the flushing water amount in the first positive flushing, the back flushing and the second positive flushing in real time, so as to better control the flushing water amount.
The present disclosure is not limited by the length of the discharge line 108, and according to the present disclosure, in order to minimize the accumulation of salt slurry in the discharge line 108 or the accumulation of salt slurry in the line due to an excessively long line, and to reduce the difficulty of flushing the line, the distance between the inlet and the opening of the discharge line 108 may be as short as possible, for example, the distance may be 0.5 to 3 m. The specific type of the solid-liquid separation device is not limited in the present disclosure, and may be a conventional choice in the art, and may be one or more of a thickener, a hydrocyclone, a centrifuge, or a settling tank, for example.
The present disclosure is further illustrated by the following examples, but is not to be construed as being limited thereby.
Example 1
NaCl industrial waste water (feed rate 580t/h, TDS 25000mg/L, COD 230mg/L) was subjected to evaporative crystallization (operating temperature of the evaporator tank was 130 ℃ C., operating pressure was 0.115MPaG, respectively) using the system shown in FIG. 1. Specifically, the method comprises the following steps:
the evaporative crystallization system comprises an evaporative crystallization unit, a slurry discharge and flushing unit and a solid-liquid separation unit; the evaporative crystallization unit comprises an evaporation tank 1 and a material circulation pipeline 104 provided with a material circulation pump 2 (axial flow pump) and a heating chamber 3; the solid-liquid separation unit comprises a solid-liquid separation device and a mother liquor circulation pipeline 115, the solid-liquid separation device shown in figure 1 comprises a # 1 solid-liquid separation device 6 (a thickener), a # 2 solid-liquid separation device 7 (a centrifuge) and a mother liquor tank 8, a mother liquor circulating pump 9 (the centrifuge) is arranged on the mother liquor circulation pipeline 115, and an outlet of the mother liquor circulation pipeline 115 is communicated with the material circulation pipeline 104;
the slurry discharging and flushing unit comprises an automatic flushing control device, a slurry discharging pipeline 108 and a flushing pipeline 109; the automatic flushing control device comprises an online detector 301, a first slurry discharge valve 202, a second slurry discharge valve 203, a first flushing water valve 204 and a controller which are in communication connection with each other; the online solid content detector 301 is arranged on the material circulating pipeline 104 and used for detecting the real-time solid-liquid ratio of the evaporating pot 1; an inlet of the slurry discharge pipeline 108 is arranged at the bottom of the evaporation tank 1, an outlet of the slurry discharge pipeline is communicated with the salt slurry tank 4 of the solid-liquid separation unit, and an outlet of the flushing pipeline 109 is arranged between the inlet and the outlet of the slurry discharge pipeline 108;
the evaporative crystallization method comprises the following steps of S1: sending the industrial wastewater containing NaCl into a circulating pipe 104 through a saline water pipeline 103, heating by a heater 3 to generate steam, and then sending the steam into an evaporation tank 1 for evaporation and crystallization to obtain upper concentrated slurry and lower concentrated slurry;
s2: leading out the upper concentrated slurry of the concentrated slurry through a circulating pipeline 104, mixing the upper concentrated slurry with the material to be evaporated from a saline water pipeline 103, and returning to perform heat exchange and evaporation in the step S1;
s3: an online solid content detector 301 arranged on the material circulating pipeline 104 is adopted to perform real-time online monitoring on the solid-liquid ratio of the upper concentrated slurry, when the real-time solid-liquid ratio of the upper concentrated slurry is more than 20% of the critical solid-liquid ratio, the lower concentrated slurry is discharged from the evaporation tank 1 through a slurry discharge pipeline 108 and subjected to solid-liquid separation, and crystals and mother liquor are obtained;
wherein the critical solid-to-liquid ratio is 0.21 times of the ratio of the saturated density of the upper concentrated slurry to the density of water; the operation of discharging the lower concentrated slurry from the evaporation tank 1 through the slurry discharge line 108 includes:
SS1, automatically closing the first slurry discharge valve 202 on the slurry discharge pipeline 108, automatically opening the second slurry discharge valve 203, and then automatically opening the valve on the flushing pipeline 109 to perform the first positive flushing for 3 minutes; SS2, first automatically opening a first slurry discharge valve 202 on a slurry discharge pipeline 108, automatically closing a second slurry discharge valve 203, and performing backwashing for 3 minutes by using flushing water in a flushing pipeline 109; SS3, firstly closing a valve on the flushing pipeline 109, opening a second slurry discharge valve 203 on the slurry discharge pipeline 108, discharging slurry until the real-time solid-liquid ratio is less than the critical solid-liquid ratio, and closing a first slurry discharge valve 202 on the slurry discharge pipeline 108; SS4, open valve on flush line 109, perform a second positive flush for 3 minutes using the flush water in flush line 109, then close second discharge valve 203;
the flow rate of the flushing water is 2 m/s; the ratio of the lumen volume of flush line 109 to the volume of the first volume of water being flushed is 1: 3 the ratio of the volume of the lumen of the flush line 109 to the volume of the amount of water backwashed is 1: 5; the ratio of the lumen volume of flush line 109 to the volume of the second volume of water being flushed is 1: 4.
the water content of the NaCl industrial salt crystal obtained by separation is 5%, the yield is 95.3%, and the stable operation time of the system exceeds 1500 h. Na in secondary steam condensate at the top of the evaporating pot 1+、Cl-Are all less than 100ppmw, COD is less than 15mg/L, and the PH value is 7.0. The comprehensive energy consumption (converted into steam amount) of unit crystalline salt is 8t steam/tNaCl crystalline salt, and the operation cost is 960 yuan/tNaCl crystalline salt.
Example 2
Na was carried out by the method of example 12SO4Evaporative crystallization of industrial wastewater, with the following differences: in the system of this example, as shown in FIG. 2, a # 1 solid-liquid separator 6 is a suspension separator; na (Na)2SO4The feeding amount of the industrial wastewater is 300t/h, the TDS is 55000mg/L, and the COD is 500 mg/L; the operating temperatures of the evaporators were 145 ℃ and the operating pressures were 0.2MPaG, respectively; the critical solid-to-liquid ratio was 25%, which was 0.22 times the ratio of the saturated density of the upper concentrated slurry to the density of water.
Separating the obtained Na2SO4The water content of the industrial nitre crystal is 7.3%, the yield is 98%, and the stable operation time of the system exceeds 1000 h. Na in secondary steam condensate at the top of the evaporating pot 1+、SO4 2-Are all less than 100ppmw, COD is less than 15mg/L, and the PH value is 7.0. The integrated energy consumption (converted into steam amount) of the unit crystal nitre is 7.2t steam/tNa2SO4The operating cost of the crystal nitre is 864 Yuan/tNa2SO4And (4) crystallizing the nitre.
Example 3
Na was carried out by the method of example 22SO4Evaporative crystallization of industrial wastewater, with the following differences: in the system of the embodiment, as shown in fig. 3, saline clear water 111 at the top of the # 1 solid-liquid separation device 6 is sent to a material circulation pipeline 104; na (Na)2SO4The feeding amount of the industrial wastewater is 350t/h, the TDS is 60000mg/L, and the COD is 750 mg/L; the critical solid-to-liquid ratio was 23%, which was taken as 0.205 times the ratio of the saturated density of the upper concentrated slurry to the density of water.
Separating the obtained Na2SO4The water content of the industrial nitre crystal is 5.5%, the yield is 97.5%, and the stable operation time of the system exceeds 1050 h. Na in secondary steam condensate at the top of the evaporating pot 1+、SO4 2-All are less than 110ppmw, COD is less than 20mg/L, and the PH value is 7.2. The integrated energy consumption (converted into steam amount) of the unit crystal nitre is 7.0t steam/tNa2SO4Crystallizing nitre at 840 yuan/tNa2SO4And (4) crystallizing the nitre.
Example 4
Evaporative crystallization of NaCl industrial wastewater was carried out using the method of example 1, with the following differences: the system of the embodiment adopts a two-stage arrangement as shown in fig. 4, wherein a first-effect heating heat source is external heating steam 101, secondary steam generated by the first effect is used as a second-effect heat source, and first-effect concentrated salt slurry enters a second-effect circulating pipe from a salt foot 107 through a material transferring pipe (concentrated slurry) 116; the discharged salt slurry is discharged from the evaporation tank from the double-effect salt foot 107 through a slurry discharge pipeline 108; the operating temperature of the evaporator is 110 ℃ and 82 ℃ respectively, and the operating pressure is 0.015MPaG and-0.07 MPaG respectively; the feeding amount of the NaCl industrial wastewater is 500t/h, the TDS is 18000mg/L, and the COD is 400 mg/L; the critical solid-to-liquid ratio was 18%, which was 0.19 times the ratio of the saturated density of the upper concentrated slurry to the density of water.
The water content of the NaCl industrial salt crystal obtained by separation is 3%, the yield is 96.5%, and the stable operation time of the system is over 1800 h. Na in secondary steam condensate at the top of the evaporating pot 1+、Cl-Are all less than 80ppmw, COD is less than 30mg/L, and the PH value is 7.2. The comprehensive energy consumption (converted into steam amount) of unit crystalline salt is 8.3t steam/tNaCl crystalline salt, and the operation cost is 996 yuan/tNaCl crystalline salt.
Comparative example 1
Evaporative crystallization of NaCl industrial wastewater was carried out using the method of example 1, with the following differences: and (3) sampling the feed liquid at a sampling port to obtain a real-time solid-liquid ratio in the evaporating pot 1, and manually discharging salt when the measured real-time solid-liquid ratio exceeds a critical solid-liquid ratio.
In the embodiment, the treatment capacity of the NaCl industrial wastewater is 500t/h, the water content of the NaCl industrial salt crystal obtained by separation is 7.5%, the yield is 89.5%, and the system stably operatesThe time does not exceed 240 h. Na in secondary steam condensate at the top of the evaporating pot 1+、Cl-130-250ppmw, COD 23-55mg/L and pH 7.0-7.1. In this example, the treatment capacity of the feed is reduced by 13.8% compared with that of example 1, and the system stabilization time is greatly reduced (the reduction is 84%). The secondary steam condensate contains trace Na+、Cl-The COD value is higher, and the quality of the steam condensate is reduced to different degrees. The operating cost of NaCl crystallized salt is about 1400 yuan/t.
Comparative example 2
Na was carried out by the method of example 22SO4Evaporative crystallization of industrial wastewater, with the following differences: and (3) sampling the feed liquid at a sampling port to obtain a real-time solid-liquid ratio in the evaporating pot 1, and manually discharging salt when the measured real-time solid-liquid ratio exceeds a critical solid-liquid ratio.
In this example Na2SO4The treatment capacity of the industrial wastewater is 280t/h, and Na obtained by separation2SO4The water content of the industrial nitre crystal is 4.4%, the yield is 92%, and the stable operation time of the system is not more than 200 h. Na in secondary steam condensate at the top of the evaporating pot 1+、SO4 2-140-300ppmw, COD 20-60mg/L and pH 6.95-7.1. Compared with example 2, the treatment capacity of the feed is reduced by 6.7%, and the system stability time is greatly reduced (the reduction is up to 80%). The secondary steam condensate contains trace Na+、SO4 2-The COD value is higher, and the quality of the steam condensate is reduced to different degrees. Na (Na)2SO4The operating cost of the nitre crystallization is about 1550 yuan/t.
As can be seen from the above examples and comparative examples, the evaporative crystallization method and system disclosed by the invention can treat different COD and salt ion concentration conditions, are suitable for use conditions of various treatment amounts, have strong applicability, are particularly suitable for treatment systems with large water amount, and have more obvious energy-saving effect; meanwhile, the device has the function of automatically discharging salt slurry, pipelines and equipment are not easy to block, the device is stable in operation and low in energy consumption and operation cost, the quality of the reuse water meets the industrial reuse water standard, the requirement for external water is reduced, and the overall economic benefit is improved.
The preferred embodiments of the present disclosure are described in detail with reference to the accompanying drawings, however, the present disclosure is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present disclosure within the technical idea of the present disclosure, and these simple modifications all belong to the protection scope of the present disclosure.
It should be noted that, in the foregoing embodiments, various features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various combinations that are possible in the present disclosure are not described again.
In addition, any combination of various embodiments of the present disclosure may be made, and the same should be considered as the disclosure of the present disclosure, as long as it does not depart from the spirit of the present disclosure.
Claims (10)
1. A method of evaporative crystallization, the method comprising:
s1: after heat exchange, the material to be evaporated containing salt water is led into an evaporation tank (1) for evaporation to obtain steam and concentrated slurry; the concentrated slurry comprises an upper layer of concentrated slurry and a lower layer of concentrated slurry;
s2: leading out and mixing the upper concentrated slurry of the concentrated slurry into the material to be evaporated, and then returning to perform the heat exchange and the evaporation;
s3: carrying out real-time online monitoring on the solid-liquid ratio of the upper concentrated slurry, and when the real-time solid-liquid ratio of the upper concentrated slurry is larger than the critical solid-liquid ratio, discharging the lower concentrated slurry from the evaporation tank (1) through a slurry discharge pipeline (108) and carrying out solid-liquid separation to obtain crystals and mother liquor;
s4: doping the mother liquor into the material to be evaporated, and then returning to perform the heat exchange and the evaporation;
wherein the operation of discharging the lower concentrated slurry from the evaporation tank (1) through a slurry discharge line (108) comprises a first positive washing, a back washing, a slurry discharge and a second positive washing which are sequentially performed.
2. A method according to claim 1, wherein an outlet of a flushing line (109) is provided between the inlet and the outlet of the discharge line (108); the operation of discharging the lower concentrated slurry from the evaporation tank (1) through a slurry discharge line (108) comprises:
SS1, closing the inlet of the slurry discharge pipeline (108) and opening the outlet of the slurry discharge pipeline (108); -conducting said first positive flush by introducing flush water through said flush line (109);
SS2, opening the inlet of the slurry discharge pipeline (108) and closing the outlet of the slurry discharge pipeline (108); introducing flushing water through the flushing line (109) for the backwashing;
SS3, closing the inlet of the flushing line (109) and opening the outlet of the slurry discharge line (108); carrying out slurry discharge on the lower layer concentrated slurry in the evaporation tank (1) through a slurry discharge pipeline (108), and closing an inlet of the slurry discharge pipeline (108) until the real-time solid-liquid ratio of the upper layer concentrated slurry is smaller than the critical solid-liquid ratio;
SS4, opening the inlet of the flush line (109), introducing flush water through the flush line (109) for the second positive flush, and then closing the outlet of the discharge line (108).
3. The method of claim 1 or 2, wherein the critical solid-to-liquid ratio is any value in the range of 0.15 to 0.3 times the ratio of the saturated density of the upper concentrated slurry to the density of water.
4. The method according to claim 1 or 2, wherein an online detector (301) is used for carrying out real-time online monitoring on the solid-to-liquid ratio of the upper concentrated slurry to obtain the real-time solid-to-liquid ratio;
the online detector (301) is an online solid content detector, a density detector or a pressure detector.
5. The method of claim 1 or 2, wherein the time of the first positive flush is 1-10 minutes; the backwashing time is 1-5 minutes; the time of the second positive flushing is 1-6 minutes; the flow rate of the washing water is 1-10 m/s.
6. The method of claim 1 or 2, wherein the first positive flush further comprises: monitoring the amount of water in the first positive flush;
wherein the volume ratio of the lumen volume of the flush line (109) to the amount of water being flushed is 1: 0.1-15.
7. The method of claim 1 or 2, wherein the backwashing further comprises: monitoring the amount of the backwashing water;
wherein the volume ratio of the lumen volume of the flushing line (109) to the amount of water for the backwash is 1: 0.1-12.
8. The method of claim 1 or 2, wherein the second positive flush further comprises: monitoring the amount of water in the second positive flush;
wherein the volume ratio of the lumen volume of the flush line (109) to the volume of water of the second positive flush is 1: 0.1-12.
9. A system for evaporative crystallization by adopting the method of any one of claims 1 to 8, wherein the system comprises an evaporative crystallization unit, a slurry discharge and flushing unit and a solid-liquid separation unit which are arranged in sequence; the evaporative crystallization unit is characterized by comprising an evaporation tank (1) and a material circulation pipeline (104) positioned outside the evaporation tank (1); the material circulating pipeline (104) comprises a raw material inlet, a mother liquid circulating inlet and a heating chamber (3) which are sequentially arranged along the material flow direction;
the solid-liquid separation unit comprises a solid-liquid separation device and a mother liquor circulating pipeline (115), and the solid-liquid separation device is provided with a slurry inlet, a mother liquor outlet and a crystallization pipeline outlet; the mother liquor outlet is communicated with the inlet of the mother liquor circulating pipeline (115), and the outlet of the mother liquor circulating pipeline (115) is communicated with the mother liquor circulating inlet on the material circulating pipeline (104);
the slurry discharging and flushing unit comprises an automatic flushing control device, a slurry discharging pipeline (108) and a flushing pipeline (109); the automatic flushing control device comprises an online detector (301), a first slurry discharge valve (202), a second slurry discharge valve (203), a first flushing water valve (204) and a controller which are in communication connection with each other; the online detector (301) is arranged at the bottom of the evaporation tank (1), or the online detector (301) is arranged at the upstream of the raw material inlet on the material circulation pipeline (104) and is used for detecting the real-time solid-liquid ratio of the evaporation tank (1); the entry of arranging thick liquid pipeline (108) set up in the bottom of evaporating pot (1), the export of arranging thick liquid pipeline (108) with thick liquid entry intercommunication, be provided with the export of flushing line (109) between the entry and the export of arranging thick liquid pipeline (108).
10. The system of claim 9, wherein the slurry discharge line (108) is provided with the first slurry discharge valve (202) and a second slurry discharge valve (203) in sequence in a material flow direction; the flushing line (109) is provided with the first flushing water valve (204); the controller is used for receiving the real-time solid-liquid ratio and controlling the opening and closing of the first slurry discharge valve (202), the second slurry discharge valve (203) and the first flushing water valve (204) according to the real-time solid-liquid ratio;
a flushing water flow meter is also arranged on the flushing pipeline (109); a material circulating pump (2) is arranged on the material circulating pipeline (104) between the mother liquid circulating inlet and the heating chamber (3), and a mother liquid circulating pump (9) is arranged on the mother liquid circulating pipeline (115).
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