CN108889126A - A kind of method of mixed salt in separation of high-concentration salting liquid - Google Patents
A kind of method of mixed salt in separation of high-concentration salting liquid Download PDFInfo
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- CN108889126A CN108889126A CN201810792760.9A CN201810792760A CN108889126A CN 108889126 A CN108889126 A CN 108889126A CN 201810792760 A CN201810792760 A CN 201810792760A CN 108889126 A CN108889126 A CN 108889126A
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Abstract
The high throughput of each salt component in high concentration mixed salt solution can be achieved in the present invention, separate to high rejection, mainly changed using solenoid valve control operating pressure by predetermined waveform, high concentration mixed salt solution is continuously separated using nanofiltration membrane circulating system, obtain two strands of mono-salt materials of penetrating fluid and trapped fluid, by the way that penetrating fluid is constantly removed system, realize the concentration of trapped fluid, then filter wash is carried out to gained retention concentrate under conditions of not exclusively vacuumizing, eluate merges with the penetrating fluid of removal Ji Wei a kind of mono-salt solution, concentrate will be washed another mono-salt solution for high-purity under high throughput, after two kinds of mono-salt solution are separately dried crystallization, obtained solid is the two kinds of mono-salt products separated.
Description
It is on April 22nd, 2014 that the application, which is the applying date, application No. is 201410163933.2, entitled " nanofiltration
Film high flux and high retention ratio separation of high-concentration mixed salt method " patent divisional application.
Technical field
The high concentration mixed salt in mixed salt solution is separated the present invention relates to nanofiltration membrane separation process high flux and high retention ratio, it should
Method controls operating pressure and changes by predetermined waveform, is carried out high concentration mixed salt solution continuously using nanofiltration membrane circulating system
Ground separation in conjunction with filter wash and becomes vacuum degree operation, obtains two kinds of mono-salt solution, after drying crystalline, isolated mono-salt product,
Continuous operation can be achieved, belong to the separation and recovery technology neck of multicomponent technical pure or reagent net product solution or actual industrial waste water
Domain.
Background technique
In recent years, many chemical processes are such as refined oil, metallurgy, the energy, light industry, petrochemical industry, environment, medicine, environmental protection all refer to
The processing problem of high concentration mixed salt, because waste water salt concentration is high, the biological cell in biochemical method understands plasmolysis under high salinity,
It is difficult to realize processing target；Existing physico-chemical process such as burns, ion exchange, electrochemical oxidation higher cost；Multiple technologies
Although group technology is the developing direction of high-salt wastewater processing, but technology path is complicated, it is more difficult to universal.With going deep into for film research
And fast development, membrane technology are shown one's talent, but under high salt concentration, existing film is difficult to maintain high rejection and high pass for a long time
Amount.For this problem, the creative method for combining pressure changeable and becoming vacuum degree of this technique really realizes brine waste or molten
High concentration mixed salt in liquid efficiently separating and recycling, applied widely, strong operability.
Summary of the invention
It is efficiently separated back from high concentration mixed salt solution the object of the present invention is to provide a kind of high-throughput, high rejection
The technology of one pack system salt is received, realizes that the technical solution of the invention is as follows, control operating pressure is by predetermined waveform variation, using receiving
High concentration mixed salt solution is continuously separated by membrane filtration circulating system, in conjunction with incomplete vacuum pumping method, utilizes filter wash
Obtain two kinds of mono-salt solution, after drying crystalline, isolated mono-salt product belongs to multicomponent industry, it can be achieved that continuous operation
The separation and recovery technology field of pure or reagent net product solution or industrial wastewater.The mono-salt separated by pure physical method.
Include the following steps：
1. mitigating concentration polarization to obtain high permeation flux, operating pressure is no longer a fixed value, but a variation
Value.Considering the tolerance of nanofiltration membrane, the speed of pressure value variation can neither be too fast, and cannot be too big, in practical operation, operation pressure
Power is controlled by solenoid valve 1, is changed by predetermined waveform, to obtain high throughput；
2. selecting suitable nanofiltration membrane, it is the key that realize high rejection separation, after determining film according to separation requirement, is packed into nanofiltration
Obtained penetrating fluid is removed system by film filtration cycle system, continuously separation of high-concentration mixed salt solution, and trapped fluid will be by
Gradually it is concentrated；
3. carrying out filter wash operation to concentrate, washing filtrate selected as needed, may be selected diluted salting liquid, tap water or
Pure water guarantees high permeation flux using the method not exclusively vacuumized, is subject to by the vacuum degree that control valve 2 adjusts fluid reservoir
It realizes, after filter wash, the salinity of trapped fluid keeps high membrane flux lower than the solubility under each salt component relevant temperature；
It is a kind of mono-salt solution 4. the eluate of filter wash process merges with the penetrating fluid of removal, this mono-salt solution is also recycled into
Head tank continues the desalinization of soil by flooding or leaching；
5. after two kinds of mono-salt solution are separately dried crystallization, obtaining two kinds of mono-salt products；It, then need to be into for the mixed salt more than number of components
Row separates two-by-two, recrystallizes after becoming mono-salt component, obtains corresponding mono-salt product.
The separation method of high concentration mixed salt provided by the invention has the characteristics that following：
1, this method can mono-salt component in high efficiente callback high concentration mixed salt waste water, generate higher economic benefit；
2, this method is a kind of pure Physical Separation Technology, the change operating pressure provided and incomplete evacuation process, is conducive to mitigate
Concentration polarization high-throughput can realize mixed salt separation；
3, the present invention is not only suitable for salt separation in laboratory multicomponent technical pure or reagent net product solution, is also applied for separating back
Receive the salt component in actual industrial high concentration mixed salt waste water；
4, the resistant material or plastics of the equipment choosing routine of contacting material, whole flow process only need control valve can be realized,
It is easy to industrialize.
Detailed description of the invention
The process flow of Fig. 1 for nanofiltration membrane high flux and high retention ratio separation of high-concentration mixed salt.Below with reference to embodiment pair
The present invention is further described.
The present invention will be further described below with reference to examples.
Embodiment 1：
The ATS (Ammonium thiosulphate) of mixed salt containing high concentration and ammonium thiocyanate in desulfurization waste liquor, concentration are respectively 60gL-1 and 120gL-1,
After removing solid content, control pressure changes according to square wave type, 2.0 ± 0.25MPa, 30 DEG C of temperature, permeates liquid measure 50Lm-2
H-1, the rejection 96% of ATS (Ammonium thiosulphate), is gradually adjusted to 0.08 for the vacuum degree of fluid reservoir in ATS (Ammonium thiosulphate) concentration process
± 0.005MPa obtains product purity 93% with tap water filter wash, yield 90%, 130gL-1 containing ammonium thiocyanate in penetrating fluid,
Decrease temperature crystalline, the purity 96% of product ammonium thiocyanate, yield 90%.
Embodiment 2：
In the pure mixing salt solution of the analysis of sodium chloride and sodium sulphate, the concentration of the two is respectively 100gL-1 and 80gL-1, control
Pressing pressure changes according to sinusoidal waveform, 1.5 ± 0.15MPa, 40 DEG C of temperature, permeates liquid measure 65Lm-2h-1, sodium sulphate is cut
Rate 95% is stayed, the vacuum degree of fluid reservoir is adjusted in concentration process and obtains product purity with pure water filter wash for 0.05 ± 0.01MPa
99%, yield 95%, sodium chloride-containing 110gL-1 in penetrating fluid, decrease temperature crystalline, the purity 99% of product sodium chloride, yield 90%.
Embodiment 3：
The pure mixed salt solution of high-concentration industrial of 100 gL-1 magnesium chlorides and 130 gL-1 sodium chloride controls pressure according to cosine
Wave mode variation, 2.4 ± 0.1MPa, permeate liquid measure 75Lm-2h-1, the rejection 95% of magnesium chloride, concentrate mistake by 30 DEG C of temperature
The vacuum degree of fluid reservoir is adjusted in journey obtains product purity with the sodium chloride solution filter wash of low concentration for 0.02 ± 0.005MPa
90%, yield 90%, sodium chloride-containing 120gL-1 in penetrating fluid, decrease temperature crystalline, the purity 90% of product sodium chloride, yield 90%.
Claims (1)
1. a kind of method of the mixed salt in separation of high-concentration salting liquid, which is characterized in that include the following steps：
1. being changed by predetermined waveform, by solenoid valve control operating pressure to obtain high throughput；
2. determining suitable nanofiltration membrane according to separation requirement, it is packed into nanofiltration membrane circulating system, is continuously separated highly concentrated
Mixed salt solution is spent, obtained penetrating fluid is removed into system, trapped fluid will be gradually concentrated；
3. carrying out filter wash operation to concentrate, washing filtrate selected as needed, may be selected diluted salting liquid, tap water or
Pure water guarantees high permeation flux using the method not exclusively vacuumized, is subject to by the vacuum degree that control valve adjusts fluid reservoir
It realizes, after filter wash, the salinity of trapped fluid keeps high membrane flux lower than the solubility under each salt component relevant temperature；
It is a kind of mono-salt solution 4. the eluate of filter wash process merges with the penetrating fluid of removal, this mono-salt solution is also recycled into
Head tank continues the desalinization of soil by flooding or leaching；
5. after two kinds of mono-salt solution are separately dried crystallization, obtaining two kinds of mono-salt products；It, then need to be into for the mixed salt more than number of components
Row separates two-by-two, recrystallizes after becoming mono-salt component, obtains corresponding mono-salt product；
1. used film can be rolled film to the step, be also possible to plate, tubular type or hollow fiber form film, material can be each
Kind high-molecular organic material, or in which the copolymer of two or more any material；0.001-1.00 μm of aperture, can be one
Or more be used in combination；According to the component type of mixed salt solution to be separated, the nanofiltration membrane of corresponding charge and suitable aperture is selected, with true
Realize separation with protecting high rejection；The operating pressure of film is controlled by solenoid valve 1 to be changed according to predetermined waveform, guarantees entire separation
Technique high throughput is carried out continuously；The operating condition of film is 5-90 DEG C of temperature, pressure 0.1-3.0MPa, crossflow velocity 0.01-6m
s-1；The concentration of mixed salt solution should be controlled lower than the solubility under each salt component relevant temperature；
The high concentration mixed salt solution of the step 2., salinity are greater than 5%（Mass percent）；Salt component in mixed salt solution is extremely
Less it is two kinds, AB+AnC type or ABn+CB type should be met（n≥2）；Mixed salt solution can be technical pure or reagent net product solution,
It is also possible to any actual mixed salt waste water without solid content；The method not exclusively vacuumized can be used, changed by control valve
Become the vacuum degree of fluid reservoir, to improve the membrane flux of concentration process；
The step 3. involved in filter wash process, washing filtrate used can select as needed, either diluted salting liquid,
It is also possible to tap water or pure water；Guarantee high permeation flux using the method not exclusively vacuumized, mainly passes through control valve
The vacuum degree of section fluid reservoir is realized；Salinity after filter wash is lower than the solubility under each salt component relevant temperature；Operation
Condition is 5-90 DEG C of temperature, pressure 0.1-3.0MPa, crossflow velocity 0.01-6ms-1, it is ensured that membrane flux is in higher level.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810792760.9A CN108889126A (en) | 2014-04-22 | 2014-04-22 | A kind of method of mixed salt in separation of high-concentration salting liquid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810792760.9A CN108889126A (en) | 2014-04-22 | 2014-04-22 | A kind of method of mixed salt in separation of high-concentration salting liquid |
| CN201410163933.2A CN105013325B (en) | 2014-04-22 | 2014-04-22 | Nanofiltration membrane high flux and high retention ratio separation of high-concentration mixed salt method |
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| CN201410163933.2A Division CN105013325B (en) | 2014-04-22 | 2014-04-22 | Nanofiltration membrane high flux and high retention ratio separation of high-concentration mixed salt method |
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| CN201810792760.9A Pending CN108889126A (en) | 2014-04-22 | 2014-04-22 | A kind of method of mixed salt in separation of high-concentration salting liquid |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1180322A (en) * | 1995-04-17 | 1998-04-29 | 凯梅蒂克斯国际有限公司 | Nanofiltration of concentrated aqueous salt solutions |
| CN101306885A (en) * | 2008-06-30 | 2008-11-19 | 南京工业大学 | Resource process method for coking sulfur-containing waste water |
| US7501065B1 (en) * | 2006-05-08 | 2009-03-10 | Bader Mansour S | Methods for treating agricultural drainage water and the like |
| CN102600722A (en) * | 2012-03-28 | 2012-07-25 | 于水利 | Membrane separation device for high-concentration feed liquid and separation method |
-
2014
- 2014-04-22 CN CN201410163933.2A patent/CN105013325B/en active Active
- 2014-04-22 CN CN201810792760.9A patent/CN108889126A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1180322A (en) * | 1995-04-17 | 1998-04-29 | 凯梅蒂克斯国际有限公司 | Nanofiltration of concentrated aqueous salt solutions |
| US7501065B1 (en) * | 2006-05-08 | 2009-03-10 | Bader Mansour S | Methods for treating agricultural drainage water and the like |
| CN101306885A (en) * | 2008-06-30 | 2008-11-19 | 南京工业大学 | Resource process method for coking sulfur-containing waste water |
| CN102600722A (en) * | 2012-03-28 | 2012-07-25 | 于水利 | Membrane separation device for high-concentration feed liquid and separation method |
Non-Patent Citations (1)
| Title |
|---|
| 殷娜等: "膜法处理焦化脱硫废液的工艺研究", 《膜科学与技术》 * |
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| CN105013325B (en) | 2019-01-18 |
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Application publication date: 20181127 |