CN105211829A - A kind of preparation method of deep-well salt - Google Patents

A kind of preparation method of deep-well salt Download PDF

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Publication number
CN105211829A
CN105211829A CN201510600168.0A CN201510600168A CN105211829A CN 105211829 A CN105211829 A CN 105211829A CN 201510600168 A CN201510600168 A CN 201510600168A CN 105211829 A CN105211829 A CN 105211829A
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bittern
flocculant
deep
preparation
filter
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CN201510600168.0A
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Chinese (zh)
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白森祥
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YULIN SALT INDUSTRY Co Ltd CNSG
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YULIN SALT INDUSTRY Co Ltd CNSG
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Abstract

The invention discloses a kind of preparation method of deep-well salt, belong to salt compound seasoner field.The preparation method of deep-well salt is: prepare 310-320g/L sodium chloride brine; After adding the flocculant of 0.1-0.12g/L NaOH and 3-5mg/L, stir, staticly settling 2 hours, filter with membrane filtration bucket, obtain a bittern; After adding the flocculant of 0.5-0.7g/L sodium carbonate and 3-5mg/L, stir, staticly settling 2 hours, filter with membrane filtration bucket, obtain secondary bittern; After adding 0.1-0.14g/L barium chloride, stir, staticly settling 2 hours, filter with film filter, obtain three bittern; Adopt vacuum process, the solid in evaporator and liquid fraction are 4: 11-14, one pressure 0.25-0.35Mpa, temperature 142 DEG C-149 DEG C, the time 2-4 hour of imitating heating clamber; Two effect heating clamber pressure 0.2-0.3Mpa, temperature 130-140 DEG C, time 2-4 hour, obtain particle deep-well salt.Flocculant and membrane filtration technique combine, and improve the quality of bittern purifying, avoid the phenomenon of evaporation equipment fouling.

Description

A kind of preparation method of deep-well salt
Technical field
The present invention relates to a kind of preparation method of compound seasoner, be specifically related to a kind of preparation method of deep-well salt.
Background technology
Salt is first of hundred tastes, and be indispensable flavoring in life, except edible, salt is also widely used in industry.Salt can be divided into sea salt, lake salt, well salt, rock salt etc. with different material.Deep-well salt raw material picks up from less than 500 meters deep-wells, and compared with common table salt, deep-well salt is rich in all kinds of natural minerals element, and impurity is few, compares other sources more pure.The raw material of salt manufacturing is bittern, is divided into natural bittern, artificial brine.Bittern, almost containing impurity, can not be directly used in salt manufacturing and produce, generally need remove objectionable impurities wherein, especially calcium magnesium plasma.The sedimentation of the calcium produced after bittern purifying during prior art salt manufacturing, magnesium salts mud often not thoroughly, sediment filters not exclusively, and cause salt slurry to enter salt manufacturing vaporising device, in heating tube, scale effect heat transfer, reduces production efficiency.
Summary of the invention
The object of this invention is to provide a kind of preparation method of deep-well salt, in preparation process, add suitable bittern purifying technique and flocculant, strengthen sediment filter effect, overcome the deficiency of prior art bittern purifying.
For this reason, the present invention adopts following technical proposals.
A. 310-320g/L sodium chloride brine is prepared;
B. bittern purifying:
B1., after adding the flocculant of NaOH and 3-5mg/L by 0.1-0.12g/L amount in bittern, stir, staticly settling 2 hours, filter with membrane filtration bucket, obtain a bittern;
B2., after adding the flocculant of sodium carbonate and 3-5mg/L by 0.5-0.7g/L amount in bittern, stir, staticly settling 2 hours, filter with membrane filtration bucket, obtain secondary bittern;
B3. in bittern, add barium chloride by 0.1-0.14g/L amount, after stirring, staticly settling 2 hours, filter with film filter, obtain three bittern;
C. bittern vacuum evaporation
Adopt vacuum process, the solid in evaporator and liquid fraction are 4: 11-14, and bittern at the running parameter of an effect heating clamber is, operating pressure 0.25-0.35Mpa, operating temperature 142 DEG C-149 DEG C, working time 2-4 hour; Bittern is that operating pressure 0.2-0.3Mpa, operating temperature 130-140 DEG C, working time 2-4 hour, obtain particle deep-well salt at the running parameter of two effect heating clambers.
The present invention at bittern once, double purification time add preferred flocculant respectively, complexing calcium magnesium plasma, accelerates sedimentary precipitation, improves the clean-up effect of bittern; Adopt membrane filtration pattern after bittern purifying, improve filter efficiency and effect; Membrane filtration shortens the bittern purifying time, increases brine treatment amount, improves production efficiency.Flocculant and membrane filtration technique combine, and the content making foreign ion in bittern after purification will be below 1mg/L, improve the quality of bittern purifying, will separately add appropriate polyacrylamide flocculant when bittern evaporation, thus avoid the phenomenon of evaporation equipment fouling.
Detailed description of the invention
The preparation method of deep-well salt of the present invention, comprises two key steps: bittern purifying and evaporation salt manufacturing.
From the bittern of underground mining all containing impurity, the general technique by purifying removes the impurity in bittern.Impurity contained in bittern is generally metal ion, as calcium, magnesium plasma, need add some chemical substances with the removal of impurities of insoluble matter sedimentation and filtration.
Bittern purifying refers to a kind of technique utilizing the method for physics and chemistry to remove the impurity in bittern.Nearly all bittern all contains Ca 2+, Mg 2+, SO 4 2-, Ba 2+, Fe 3+deng impurity, and the existence of these impurity affect product quality impact and to production process.CaSO in bittern 4, MgSO 4, CaCl 2, MgCl 2can make the elevation of boiling point of bittern Deng impurity, viscosity increases, and thus reduces effective heat transfer temperature poor; In addition, impurity is more, and the Mother liquid of vacuum salt production is larger, makes heat increase (namely energy consumption is high) on the one hand; Reduce the rate of recovery of NaCl on the other hand.Therefore, must purified brine in salt producing craft.Flocculant is used in bittern purifying is produced, can the sinking speed of suspended particulate in bittern after accelerated impurity ion reaction, reduce settling time, enhance productivity.
Bittern primary purification:
Saturated bittern is added purification bucket, before starting stirring, add the NaOH of 0.1-0.12g/L.Before stirring terminates, add the flocculant of 3-5mg/L.Close agitator and carry out mud sediment.Precipitate latter 2 hours, the limpid bittern in upper strata is transferred to membrane filtration bucket, and the bittern after filtration enters double purification reaction container, and the mud of precipitation then pours into mud tank.The flocculant used is acrylamide/acrylic acid copolymer flocculant.Containing a large amount of negative electric base in flocculating agent molecule, they are mutually exclusive and make large molecule be extended configuration, and molecule is longer and fully expose active group, and flocculating property is better; Acrylic acid carboxyl is due to electrostatic repulsion effect, the polymer chain of flexing is stretched, facilitates the functional group with adsorptivity to be exposed to surface, because these active sites adsorb in the solution on suspended particles, form interparticle bridge formation, thus accelerate the sedimentation of suspended particles.
The chemical equation related to is:
MgCl 2+2NaOH=Mg(OH) 2↓+2NaCl
FeCl 3+3NaOH=Fe(OH) 3↓+3NaCl
Bittern double purification:
The sodium carbonate of 0.5-0.7g/L and the flocculant of 3-5mg/L is added in the bittern of double purification reaction container, 2 hours are staticly settled after stirring, limpid for upper strata bittern is transferred to membrane filtration bucket, and the bittern after filtration enters three purification buckets, and the mud of precipitation then pours into mud tank.Flocculant is poly-aspartate/polyacrylic acid compound flocculant.Poly-aspartate, because of the design feature containing peptide bond and carboxyl isoreactivity group, have the effects such as extremely strong chelating, dispersion, absorption, and compatibility is splendid to calcium, magnesium plasma.Polyacrylic acid contains strong anion active group, by the effect of charge neutrality adsorption bridging, can suspended particulate effectively in adsorptive liquid, and aggegation is agglomerating mutually.Poly-aspartate/polyacrylic acid built-up flocculant can promote sedimentation, clarification, purification.
The chemical equation related to is:
CaSO 4+Na 2CO 3=2NaOH+CaCO 3
CaCl 2+Na 2CO 3=CaCO 3↓+2NaCl
Bittern three purifications:
In the bittern of three purification buckets, add the barium chloride of 0.1-0.14g/L and the flocculant of 3-5mg/L, after stirring, staticly settle 2 hours, limpid for upper strata bittern is transferred to membrane filtration bucket, filter to obtain three purified brines.
The chemical equation related to is:
Na 2SO 4+BaCl 2=BaSO 4↓+2NaCl
Through above-mentioned three bittern purifying techniques, the impurity in bittern is removed substantially, thus when bittern evaporation salt manufacturing, can reduce fouling, ensures product quality.
Film is the material with Selective Separation function.Utilize that the Selective Separation of film realizes the separation of the different component of feed liquid, purifying, concentrated process are called UF membrane.From the different of traditional filtering, it is that film can be separated in molecular range, and this process is a kind of physical process, does not need change and interpolation auxiliary agent that phase occurs.The filter membrane that the present invention adopts is film known in those skilled in the art, as the filter membrane product of Kai Mo company of Singapore, W. L. Gore & Associates, Inc. company.
Bittern after purification, Ca wherein 2+, Mg 2+, SO 4 2-detected level is about 0.1mg/L, shows the respond well of bittern purifying.
Still remain a certain amount of calcium, magnesium ion in bittern after bittern purifying, in subsequent evaporation operation, along with the continuous evaporation and concentration of bittern, the calcium in bittern, magnesium ion concentration also constantly increase, and also easily separate out, in addition CaSO in brine transportation, warm 4have the characteristic of retrograde solubility, fouling on the wall being attached to the equipment of pipeline, seriously can reduce heat transfer coefficient, dirty layer is larger, heat transfer coefficient is declined larger, thus equipment capacity is reduced.The elimination of dirt layer can extend the effective time, effcetive output.When bittern evaporation, add appropriate polyacrylamide flocculant, effectively can adsorb the calcium in bittern, magnesium plasma, prevent fouling bad phenomenon.
Evaporation salt manufacturing:
Adopt vacuum process, 2-3mg/L polyacrylamide flocculant is added in bittern, solid in evaporator and liquid fraction are 4: 11-14, and bittern at the running parameter of an effect heating clamber is, operating pressure 0.25-0.35Mpa, operating temperature 142 DEG C-149 DEG C, working time 2-4 hour; Bittern is that operating pressure 0.2-0.3Mpa, operating temperature 130-140 DEG C, working time 2-4 hour, obtain particle deep-well salt at the running parameter of two effect heating clambers.
Evaporation technology is preferably: bittern at the running parameter of an effect heating clamber is, operating pressure 0.3-0.35Mpa, operating temperature 145-147 DEG C, working time 3-4 hour, the bittern of one effect evaporator evaporation proceeds to two effect evaporators, and the running parameter of two effect heating clambers is, pressure 0.2-0.25Mpa, operating temperature 135-140 DEG C, working time 3-4 hour.
Below by specific embodiment, embodiment of the present invention is described further.
Embodiment 1:
A preparation method for deep-well salt, its preparation method comprises the steps:
A. 310g/L sodium chloride brine is prepared;
B. bittern purifying:
B1., after adding the flocculant of NaOH and 3mg/L by 0.1g/L amount in bittern, stir, staticly settling 2 hours, filter with membrane filtration bucket, obtain a bittern;
B2., after adding the flocculant of sodium carbonate and 3mg/L by 0.5g/L amount in bittern, stir, staticly settling 2 hours, filter with membrane filtration bucket, obtain secondary bittern;
B3. in bittern, add barium chloride by 0.1g/L amount, after stirring, staticly settling 2 hours, filter with film filter, obtain three bittern;
C. bittern vacuum evaporation
Adopt vacuum process, add 2mg/L polyacrylamide flocculant in bittern, the solid in evaporator and liquid fraction are 4: 11, and bittern at the running parameter of an effect heating clamber is, operating pressure 0.25Mpa, operating temperature 142 DEG C, 2 hours working times; Bittern is operating pressure 0.2Mpa, operating temperature 130 DEG C, 2 hours working times, obtain particle deep-well salt at the running parameter of two effect heating clambers.
Embodiment 2:
A preparation method for deep-well salt, its preparation method comprises the steps:
A. 310g/L sodium chloride brine is prepared;
B. bittern purifying:
B1., after adding the flocculant of NaOH and 4mg/L by 0.11g/L amount in bittern, stir, staticly settling 2 hours, filter with membrane filtration bucket, obtain a bittern;
B2., after adding the flocculant of sodium carbonate and 4mg/L by 0.6g/L amount in bittern, stir, staticly settling 2 hours, filter with membrane filtration bucket, obtain secondary bittern;
B3. in bittern, add barium chloride by 0.12g/L amount, after stirring, staticly settling 2 hours, filter with film filter, obtain three bittern;
C. bittern vacuum evaporation
Adopt vacuum process, add 2mg/L polyacrylamide flocculant in bittern, the solid in evaporator and liquid fraction are 4: 12, and bittern at the running parameter of an effect heating clamber is, operating pressure 0.3Mpa, operating temperature 145 DEG C, 3 hours working times; Bittern is operating pressure 0.25Mpa, operating temperature 135 DEG C, 3 hours working times, obtain particle deep-well salt at the running parameter of two effect heating clambers.
Embodiment 3:
A preparation method for deep-well salt, its preparation method comprises the steps:
A. 320g/L sodium chloride brine is prepared;
B. bittern purifying:
B1., after adding the flocculant of NaOH and 5mg/L by 0.12g/L amount in bittern, stir, staticly settling 2 hours, filter with membrane filtration bucket, obtain a bittern;
B2., after adding the flocculant of sodium carbonate and 5mg/L by 0.7g/L amount in bittern, stir, staticly settling 2 hours, filter with membrane filtration bucket, obtain secondary bittern;
B3. in bittern, add barium chloride by 0.14g/L amount, after stirring, staticly settling 2 hours, filter with film filter, obtain three bittern;
C. bittern vacuum evaporation
Adopt vacuum process, add 3mg/L polyacrylamide flocculant in bittern, the solid in evaporator and liquid fraction are 4: 14, and bittern at the running parameter of an effect heating clamber is, operating pressure 0.35Mpa, operating temperature 149 DEG C, 4 hours working times; Bittern is operating pressure 0.3Mpa, operating temperature 140 DEG C, 4 hours working times, obtain particle deep-well salt at the running parameter of two effect heating clambers.

Claims (5)

1. a preparation method for deep-well salt, is characterized in that, preparation method comprises the steps:
A. 310-320g/L sodium chloride brine is prepared;
B. bittern purifying:
B1., after adding the flocculant of NaOH and 3-5mg/L by 0.1-0.12g/L amount in bittern, stir, staticly settling 2 hours, filter with membrane filtration bucket, obtain a bittern;
B2., after adding the flocculant of sodium carbonate and 3-5mg/L by 0.5-0.7g/L amount in bittern, stir, staticly settling 2 hours, filter with membrane filtration bucket, obtain secondary bittern;
B3. in bittern, add barium chloride by 0.1-0.14g/L amount, after stirring, staticly settling 2 hours, filter with film filter, obtain three bittern;
C. bittern vacuum evaporation
Adopt vacuum process, the solid in evaporator and liquid fraction are 4: 11-14, and bittern at the running parameter of an effect heating clamber is, operating pressure 0.25-0.35Mpa, operating temperature 142 DEG C-149 DEG C, working time 2-4 hour; Bittern is that operating pressure 0.2-0.3Mpa, operating temperature 130-140 DEG C, working time 2-4 hour, obtain particle deep-well salt at the running parameter of two effect heating clambers.
2. the preparation method of a kind of deep-well salt according to claim 1, is characterized in that: flocculant described in step b1 is acrylamide/acrylic acid copolymer flocculant.
3. the preparation method of a kind of deep-well salt according to claim 1, is characterized in that: flocculant described in step b2 is poly-aspartate/polyacrylic acid compound flocculant.
4. the preparation method of a kind of deep-well salt according to claim 1, it is characterized in that: when vacuum salt, bittern at the running parameter of an effect heating clamber is, operating pressure 0.3-0.35Mpa, operating temperature 145-147 DEG C, working time 3-4 hour, the bittern of one effect evaporator evaporation proceeds to two effect evaporators, and the running parameter of two effect heating clambers is, pressure 0.2-0.25Mpa, operating temperature 135-140 DEG C, working time 3-4 hour.
5. the preparation method of a kind of deep-well salt according to claim 1, is characterized in that: when vacuum salt, adds 2-3mg/L polyacrylamide flocculant in bittern.
CN201510600168.0A 2015-09-20 2015-09-20 A kind of preparation method of deep-well salt Pending CN105211829A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110182831A (en) * 2019-05-28 2019-08-30 昌鑫生态科技(陕西)有限公司 The technology of salt lake extraction lithium carbonate
CN115708575A (en) * 2022-09-28 2023-02-24 山东肥城精制盐厂有限公司 Refined salt production process based on natural rock salt

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110182831A (en) * 2019-05-28 2019-08-30 昌鑫生态科技(陕西)有限公司 The technology of salt lake extraction lithium carbonate
CN115708575A (en) * 2022-09-28 2023-02-24 山东肥城精制盐厂有限公司 Refined salt production process based on natural rock salt
CN115708575B (en) * 2022-09-28 2023-12-01 山东肥城精制盐厂有限公司 Refined salt production process based on natural rock salt

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