CN108314062A - A kind of hot method of continuously saltouing puies forward the production technology of nitre - Google Patents
A kind of hot method of continuously saltouing puies forward the production technology of nitre Download PDFInfo
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- CN108314062A CN108314062A CN201810118553.5A CN201810118553A CN108314062A CN 108314062 A CN108314062 A CN 108314062A CN 201810118553 A CN201810118553 A CN 201810118553A CN 108314062 A CN108314062 A CN 108314062A
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- mother liquor
- salt
- nitre
- production technology
- preheating
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/16—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
Abstract
The invention discloses the production technologies that a kind of hot method of continuously saltouing carries nitre, belong to sal prunella co-production technology field.Raw brine and salt slurry in desalinization of soil by flooding or leaching device are carried out three stage countercurrents and emulsify floating washing by the present invention, the direct centrifugal drying of salt slurry after washing is packaged as finished product salt, the overflowing liquid of discharge enters turning barrel in mother liquor jointly with a small amount of mother liquor discharged in evaporator, then after multistage preheating (preheating heat source is the extra condensed water of each effect), it send in crystallizer and being warming up to 95 100 DEG C, simultaneously by 2 4% addition NaCl of mother liquor solid content, according to common-ion effect principle, sodium chloride crystal is precipitated, and takes out and is dehydrated up to saltcake product after system.The technique steam consumption is low, production cost is low, and technical process is simple, and equipment investment is few, and easy to operate and production is continuous controllable.
Description
Technical field
The present invention relates to sal prunella co-production technology fields, and in particular to a kind of hot method of continuously saltouing puies forward the production technology of nitre.
Background technology
The brine type in the main areas Chan Yan of China is sodium sulfate type, and in addition to main content sodium chloride, secondary content sodium sulphate is flat
Equal content is up to 25g/l or more, additionally contains a small amount of calcium sulfate, magnesium sulfate.The salt manufacturing production process of this type brine
It is generally used joint production process of salt and salt-cake, salt, nitre are crystallized out from system respectively in production.In order to control salt matter, it is ensured that saltcake
It is not crystallized out in salt system, needs mother liquor in a large amount of blowdown vessels, cause huge thermal loss, therefore joint production process of salt and salt-cake
Steam consumption is more, and the ton product steam consumption causes production cost high, deficiency in economic performance up to 1.1 or more.
Main problem existing for joint production process of salt and salt-cake is:Joint production process of salt and salt-cake steam consumption is high, leads to production cost height:Sulphur
Sodium chloride content is generally 295~300g/l, sodium sulphate 25g/l in sour sodium form brine, and calcium sulfate, magnesium sulfate are a small amount of.It is steaming
During hair, if be not controlled, four kinds of sodium chloride, sodium sulphate, calcium sulfate, magnesium sulfate substances will cocrystallization be precipitated, it is special
A kind of double salt of indissoluble can be compounded to form by not being sodium sulphate, calcium sulfate --- and glauberite seriously affects product quality, leads to product
Criterion of acceptability is not achieved in quality.For this purpose, the impurity in brine must be removed in technique.Traditional joint production process of salt and salt-cake passes through row
Put mother liquor in evaporator, it is ensured that sodium sulphate, calcium sulfate, magnesium sulfate are unsaturated in evaporator, prevent sodium sulphate in evaporator, sulfuric acid
The impurity such as calcium, magnesium sulfate crystallize to achieve the purpose that control salt matter.Recycling Mother Solution rich in impurity is to nitre system, after evaporating moisture content
Crystallization obtains saltcake product.Joint production process of salt and salt-cake in the actual production process, if raw brine not purified treatment, will form five
First system, production control process it is extremely complex, product quality it is difficult to ensure that.Thus, the necessary mating brine of joint production process of salt and salt-cake is net
Change, remove the impurity such as calcium sulfate, the magnesium sulfate in brine, is produced into tank using purified brine (sodium chloride-containing, sodium sulphate).Although
Product quality can be guaranteed, but apparatus investment is more, and process route is complicated, operation and control difficulty, wherein bittern purifying at
This is 10 yuan of ton product or more, and 1.1 or more the ton product steam consumption, economically pole is not cost-effective.B, Technological adaptability is poor:Sal prunella coproduction work
There are one very fatal defects for skill, that is, Technological adaptability is poor.When raw brine ingredient changes, especially sulphur
When sour sodium content increases suddenly, since the cured design of system inevitably results in heat, material once Mother liquid increases
Imbalance so that salt yield falls sharply, and also some mother liquors have to discharge system, causes not up to standard in environmental protection;If do not increased
Add discharge capacity, then sodium sulphate can be crystallized out in salt system, influence product quality.
Invention content
In view of the deficienciess of the prior art, the present invention is intended to provide a kind of hot method of continuously saltouing puies forward the production technology of nitre,
Raw brine and salt slurry in desalinization of soil by flooding or leaching device are carried out three stage countercurrents and emulsify floating washing by the production technology, and the salt slurry after washing directly centrifuges
It dehydrating, is packaged as finished product salt, the overflowing liquid of discharge enters turning barrel in mother liquor jointly with a small amount of mother liquor discharged in evaporator,
Then it after multistage preheating (preheating heat source is the extra condensed water of each effect), send in crystallizer and being warming up to 95-100 DEG C,
NaCl is added by the 2-4% of mother liquor solid content simultaneously, according to common-ion effect principle, sodium chloride crystal is precipitated, is taken out after system
It dehydrates up to saltcake product.
Inventor passes through many experiments and unremitting effort, is finally obtained the production work that a kind of hot method of continuously saltouing carries nitre
Skill includes the following steps:
(1) raw brine and the salt slurry of evaporator discharge, which enter in desalinization of soil by flooding or leaching device, carries out three stage countercurrents emulsification floating washing, after washing
The direct centrifugal drying of salt slurry, be packaged as finished product salt, the overflowing liquid of discharge enters turning barrel in mother liquor;
The mass ratio of the raw brine and salt slurry is 1:1;
(2) a small amount of mother liquor of discharge in evaporator enters turning barrel in mother liquor jointly with the overflowing liquid of step (1), the two
Mass ratio is 1:3;
(3) mother liquor in turning barrel in step (2) mother liquor is continued through into level-one pre-heating system, two-stage preheating circuit carries out in advance
Heat, at 50-55 DEG C, the temperature of two level preheating is controlled at 55-65 DEG C for the temperature control of the level-one preheating;
(4) mother liquor for passing through two level preheating enters in OSL types crystallizer and is further warming up to 95-100 DEG C, the residence time
30 minutes or more, while NaCl is added by the 2-4% of mother liquor solid content, the crystal deposition of precipitation drains into centrifugation in bottom by pump
Machine is dehydrated, and through drying, is packaged as saltcake product, is carried the hot mother liquor after nitre, directly with being pumped to evaporation ladle addition.
Compared with prior art, advantage obtained by the present invention is:
1. steam consumption is low, five effect evaporation of this technique cooperation, the ton product steam consumption is said up to 0.75t/t, five effect evaporation technologies
It is bright:The brine that mine is come enters each effect evaporator, and the steam that boiler comes enters I effect and heats room, and steam passes through circulating pump with brine
Forced circulation heat exchange, the indirect steam that generates enters II effect and heats room after brine boiling, as II effect evaporator of heat source heating
Brine, and so on, until V effect generate indirect steam enter atmospheric condenser condensation, drastically form vacuum, as
The motive force of heat transfer.It after bittern evaporation, is crystallized in evaporator, the salt slurry of formation is emitted into desalinization of soil by flooding or leaching system, through Over emulsfication floating washing
Improve salt matter.
2. production cost is low, joint production process of salt and salt-cake is compared, ton cost of goods manufactured can decline 45 yuan.
3. technical process is simple, equipment investment is few.
4. easy to operate, production is continuous controllable.
5. the present apparatus is using OSL salting-out crystallizers as the salting-out crystallizer of the mother liquor containing nitre, by designing rational knot
Brilliant device volume, saltcake crystal crystal under the suitable residence time can adequately be grown up;Mother liquor containing nitre has suitable mistake
Temperature so that the degree of supersaturation of crystallization process avoids the appearance of crystal primary nucleation in Metastable zone, the solute crystallized out
It is grown on relatively limited seed surface, to obtain larger crystal size, ensures the separating effect of crystal and mother liquor, and
This Technological adaptability is strong, can adapt to Na in raw brine completely2SO4Changes of contents requirement, sodium sulphate content is sent out suddenly in former halogen
When changing, system can voluntarily be adjusted from technique and be adapted to.
6. entering evaporator charging due to carrying nitre hot mother liquor in this technique, mother liquor system closed cycle is not discharged, is saved
A large amount of brine reduce brine consumption.
Description of the drawings
Fig. 1 is the flow diagram of production technology of the present invention.
Fig. 2 is that five effects evaporate flow chart.
Specific embodiment
According to raw brine characteristic, it is therefore apparent that key technology point is the separation of impurity component and to be carried in raw brine
It takes, raw brine and salt slurry are carried out three stage countercurrents by the production technology in desalinization of soil by flooding or leaching device and emulsify floating washing by us, after washing
The direct centrifugal drying of salt slurry is packaged as finished product salt, the overflowing liquid of discharge and a small amount of mother liquor for being discharged in evaporator jointly into
Enter turning barrel in mother liquor, then after multistage preheating (preheating heat source is the extra condensed water of each effect), send in crystallizer and rising
Temperature adds NaCl to 95-100 DEG C, while by the 2-4% of mother liquor solid content, and according to common-ion effect principle, sodium chloride crystal is precipitated,
It takes out and is dehydrated up to saltcake product after system.
Emulsify floating washing method washing principle:The salt slurry of salt manufacturing evaporator discharge enters desalinization of soil by flooding or leaching system, solid-phase component sodium chloride-containing,
Separately containing impurity components such as sodium sulphate, magnesium sulfate, calcium sulfate.Sodium chloride approaches saturation in raw brine and sodium sulphate is unsaturated,
When the raw brine desalinization of soil by flooding or leaching, the concentration difference of sodium chloride is small, and solution rate is slow, and the concentration difference of sodium sulphate is big, and solution rate is fast, corresponding chlorine
It is high to change na concn, crystallization is fast, and sodium sulfate concentration is low, and crystallization is slow.When the desalinization of soil by flooding or leaching reaches balance, i.e. dissolving and crystallization reaches balance
When, a portion saltcake (little particle) dissolving, undissolvable saltcake also becomes smaller, to keep saltcake particle relatively uniform
0.01mm is maintained hereinafter, it is largely present in the form of the ground that suspends in old halogen, makes old halogen that emulsified state be presented.Then, according to
The difference of the crystalline form of sodium chloride and sodium sulphate, weight, surface area and viscosity, the salt and nitre of identical weight, the specific surface area ratio of nitre
Salt is big, and ratio of viscosities salt is big, and crystalline form is not as good as salt rule, to the flow velocity (5.5mm/s) certain by emulsifying halogen, irregular in salt
Fine grained nitre taken out of with brine, to ensure that the quality of salt.
It is acted on by the counter flow washing of raw brine, a part of solid phase impurity is dissolved in brine, due to particle in solid phase
The difference of degree, sodium chloride particle degree are far longer than impurity component, and sodium chloride crystal settles down, most of solid phase impurity component with
Mother liquor overflow detaches, and the salt slurry for meeting quality requirement can be obtained by the desalinization of soil by flooding or leaching device of reasonable design, after washing.Stablize in order to obtain
Product quality, evaporator domestic demand discharges a small amount of mother liquor, and turning barrel during discharge mother liquor enters together with desalinization of soil by flooding or leaching system overflowing liquid leads to
After crossing two level preheating, mother liquor enters OSL salting-out crystallizers, is further heated to suitable temperature spot, after adding salt, chlorination
Sodium reaches saturation, according to common-ion effect principle, then sodium sulphate is then due to homo-ion Na+Supersaturation and cause homo-ion effect
It answers, sulfate crystal is precipitated, and sodium chloride is far from saturation point without being precipitated.In the process, a small amount of sulfuric acid contained in brine
Also crystallization is precipitated together for magnesium, calcium sulfate.After the sodium sulphate that crystallization is precipitated takes out, by centrifugal dehydration, drying, it is packaged as finished product
Nitre.
A kind of hot method of continuously saltouing puies forward the production technology of nitre, which includes the following steps:
(1) raw brine and the salt slurry of evaporator discharge, which enter in desalinization of soil by flooding or leaching device, carries out three stage countercurrents emulsification floating washing, after washing
The direct centrifugal drying of salt slurry, be packaged as finished product salt, the overflowing liquid of discharge enters turning barrel in mother liquor;
The mass ratio of the raw brine and salt slurry is 1:1;
(2) a small amount of mother liquor of discharge in evaporator enters turning barrel in mother liquor jointly with the overflowing liquid of step (1), the two
Mass ratio is 1:3;
(3) mother liquor in turning barrel in step (2) mother liquor is continued through into level-one pre-heating system, two-stage preheating circuit carries out in advance
Heat, at 50-55 DEG C, the temperature of two level preheating is controlled at 55-65 DEG C for the temperature control of the level-one preheating;
(4) the step of passing through two level preheating (3) mother liquor enters in OSL types crystallizer and is further warming up to 95-100 DEG C,
30 minutes residence times or more, while NaCl is added by the 2-4% of mother liquor solid content, the crystal deposition of precipitation is in bottom, by pumping
Centrifuge dewatering is drained into, through drying, saltcake product is packaged as, carries the hot mother liquor after nitre, directly with being pumped in each effect evaporator
Charging.
A kind of hot method of continuously saltouing puies forward the production technology of nitre, the heat of level-one pre-heating system, two-stage preheating circuit in step (3)
Source is the condensed water that salt making system respectively imitates that heating room generates.
A kind of hot method of continuously saltouing puies forward the production technology of nitre, and the heat source of step (4) is the secondary steaming that I effect evaporator generates
Vapour.
The following is specific embodiments of the present invention, is described further to technical scheme of the present invention, but the present invention's is interior
Hold the range being not limited solely to described in embodiment, it is every to be included in this without departing substantially from the change of present inventive concept or equivalent substitute
Within the protection domain of invention.
Embodiment 1
The joint production process of salt and salt-cake production technology that generally uses the present invention be directed to domestic sodium sulphate type bittern salt making enterprises and
Equipment falls behind, the high present situation of manufacturing cost, develop it is a set of using sodium sulphate against dissolubility, sodium ion common-ion effect principle,
By discharging a small amount of mother liquor in tank, discharge salt slurry three stage countercurrents in vertical desalinization of soil by flooding or leaching device emulsify floating washing, adjust washing brine amount
With salt slurry mass ratio 1:1, control washing Mother liquor temperature≤35 DEG C can reach best washing effect, and the salt slurry quality after washing is closed
Lattice, entirely reach national standard top grade product (sodium chloride content >=99.1%), and the salt slurry after washing is directly gone centrifugal drying, wrapped again
Dress is finished product salt.The a small amount of mother liquor being discharged in cleaning solution and tank mix that (mass ratio of the two is 1:3), by multistage pre-heating temperature elevation
(wherein level-one pre-heating temperature elevation is to 50-55 DEG C, and two level pre-heating temperature elevation is to 55-65 DEG C) afterwards enters back into an OSL type crystallizer,
(heat source is the indirect steam that 1 effect generates) to (temperature is controlled at 95-100 DEG C) after suitable temperature is further heated up, according to
H2O——NaCl——Na2SO4Ternary system phasor is it is found that (additive amount is solid to mother liquor after adding certain NaCl in systems
The 2-4% of content), according to common-ion effect principle, sodium sulphate crystallizes precipitation from system at this time, after considering Quinary system, sulphur
Sour magnesium, calcium sulfate are also precipitated from system.Cleverly designed by OSL salting-out crystallizers, the crystal deposition of precipitation in bottom, by
Pump drains into centrifuge dewatering, through drying, is packaged as saltcake product.The hot mother liquor after nitre is carried, sodium chloride content is generally up to 305g/
L, due to being high temperature mother liquor, directly with being pumped to evaporation ladle addition.
The present invention is combined with five effect vacuum processes, can embody its optimum economic benefit.It is each in five-effective evaporation
Mother liquor is discharged in effect, and total amount accounts for about the 1/3 of desalinization of soil by flooding or leaching mother liquor, compared with the mother liquor amount of joint production process of salt and salt-cake discharge, just corresponds to
20%, during Recycling Mother Solution, heat-energy losses are serious, therefore mother liquor discharge is more, and heat-energy losses are more serious.Though two kinds of productions
Technique can guarantee product quality more than top grade product, but production cost difference is more, five effect life especially in terms of steam consumption
It is 35 yuan/ton lower than joint production process of salt and salt-cake that production+sal prunella puies forward nitre technique.Five effects, which are produced+saltoutd, puies forward nitre production technology and sal prunella coproduction life
Production. art technical-economic index is compared as follows:
Claims (3)
1. a kind of hot method of continuously saltouing puies forward the production technology of nitre, it is characterised in that:The production technology includes the following steps:
(1) raw brine and the salt slurry of evaporator discharge, which enter in desalinization of soil by flooding or leaching device, carries out three stage countercurrents emulsification floating washing, the salt after washing
It starches direct centrifugal drying, be packaged as finished product salt, the overflowing liquid of discharge enters turning barrel in mother liquor;
The mass ratio of the raw brine and salt slurry is 1:1;
Both (2) a small amount of mother liquor of discharge in evaporator enters turning barrel in mother liquor jointly with the overflowing liquid of step (1), wherein
Mass ratio is 1:3;
(3) by the mother liquor in turning barrel in step (2) mother liquor continues through level-one pre-heating system, two-stage preheating circuit preheats,
At 50-55 DEG C, the temperature of two level preheating is controlled at 55-65 DEG C for the temperature control of the level-one preheating;
(4) the step of passing through two level preheating (3) mother liquor enters in crystallizer and is further warming up to 95-100 DEG C, the residence time 30
Minute or more, while NaCl is added by the 2-4% of mother liquor solid content, the crystal deposition of precipitation drains into centrifuge in bottom by pump
Dehydration, through drying, is packaged as saltcake product, carries the hot mother liquor after nitre, directly with being pumped to evaporation ladle addition.
2. a kind of hot method of continuously saltouing as described in claim 1 puies forward the production technology of nitre, it is characterised in that:One in step (3)
Grade pre-heating system, two-stage preheating circuit heat source be salt making system respectively imitate heating room generation condensed water.
3. a kind of hot method of continuously saltouing as described in claim 1 puies forward the production technology of nitre, it is characterised in that:The heat of step (4)
Source is the indirect steam that salt manufacturing I imitates that evaporator generates.
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Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109453532A (en) * | 2018-12-20 | 2019-03-12 | 四川久大蓬莱盐化有限公司 | One kind five imitates hexasomic vacuum salt production mother liquor concentrations device and its method for concentration |
CN109534363A (en) * | 2018-12-10 | 2019-03-29 | 中盐枣阳盐化有限公司 | A kind of thick nitre extracting method |
CN109607569A (en) * | 2018-12-10 | 2019-04-12 | 中盐枣阳盐化有限公司 | A kind of three-level desalinization of soil by flooding or leaching method |
CN109896535A (en) * | 2019-02-21 | 2019-06-18 | 中国中轻国际工程有限公司 | A kind of well mine salt Galuber's salt type brine production natural green edible salt technique |
CN110065956A (en) * | 2019-05-17 | 2019-07-30 | 湖南省湘衡盐化有限责任公司 | A kind of salt producing craft and its system |
CN110330037A (en) * | 2019-07-17 | 2019-10-15 | 江苏汉凯工程技术有限公司 | The method of sodium chloride is recycled in a kind of glyphosate mother solution |
CN110422862A (en) * | 2019-07-15 | 2019-11-08 | 中国中轻国际工程有限公司 | A kind of less salt glass gall multi-stage countercurrent, which is saltoutd, produces sodium sulfate in high purity technique |
CN111533143A (en) * | 2020-06-05 | 2020-08-14 | 上海力脉环保设备有限公司 | Industrial-grade anhydrous sodium sulfate preparation device and method |
CN113896361A (en) * | 2021-10-18 | 2022-01-07 | 中南大学 | Method for cleaning and disposing stainless steel pickling acid waste liquid and recycling resources |
CN115557518A (en) * | 2022-10-31 | 2023-01-03 | 孝感广盐华源制盐有限公司 | Method for salt-nitrate co-production through six-effect TVR evaporation glauberite double salt separation method |
CN115974213A (en) * | 2022-12-13 | 2023-04-18 | 江苏苏盐井神股份有限公司 | High-nitrate salt washing and floating separation device and process |
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Cited By (13)
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CN109534363A (en) * | 2018-12-10 | 2019-03-29 | 中盐枣阳盐化有限公司 | A kind of thick nitre extracting method |
CN109607569A (en) * | 2018-12-10 | 2019-04-12 | 中盐枣阳盐化有限公司 | A kind of three-level desalinization of soil by flooding or leaching method |
CN109453532A (en) * | 2018-12-20 | 2019-03-12 | 四川久大蓬莱盐化有限公司 | One kind five imitates hexasomic vacuum salt production mother liquor concentrations device and its method for concentration |
CN109453532B (en) * | 2018-12-20 | 2023-09-01 | 四川久大蓬莱盐化有限公司 | Five-effect six-body vacuum salt-making mother liquor concentrating device and concentrating method thereof |
CN109896535A (en) * | 2019-02-21 | 2019-06-18 | 中国中轻国际工程有限公司 | A kind of well mine salt Galuber's salt type brine production natural green edible salt technique |
CN110065956A (en) * | 2019-05-17 | 2019-07-30 | 湖南省湘衡盐化有限责任公司 | A kind of salt producing craft and its system |
CN110422862A (en) * | 2019-07-15 | 2019-11-08 | 中国中轻国际工程有限公司 | A kind of less salt glass gall multi-stage countercurrent, which is saltoutd, produces sodium sulfate in high purity technique |
CN110330037A (en) * | 2019-07-17 | 2019-10-15 | 江苏汉凯工程技术有限公司 | The method of sodium chloride is recycled in a kind of glyphosate mother solution |
CN111533143A (en) * | 2020-06-05 | 2020-08-14 | 上海力脉环保设备有限公司 | Industrial-grade anhydrous sodium sulfate preparation device and method |
CN113896361A (en) * | 2021-10-18 | 2022-01-07 | 中南大学 | Method for cleaning and disposing stainless steel pickling acid waste liquid and recycling resources |
CN115557518A (en) * | 2022-10-31 | 2023-01-03 | 孝感广盐华源制盐有限公司 | Method for salt-nitrate co-production through six-effect TVR evaporation glauberite double salt separation method |
CN115974213A (en) * | 2022-12-13 | 2023-04-18 | 江苏苏盐井神股份有限公司 | High-nitrate salt washing and floating separation device and process |
CN115974213B (en) * | 2022-12-13 | 2024-03-22 | 江苏苏盐井神股份有限公司 | High-nitrate floatation separation device and process |
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