CN1130152A - Process for producing potassium sulfate from bittern and potassium chloride - Google Patents
Process for producing potassium sulfate from bittern and potassium chloride Download PDFInfo
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- CN1130152A CN1130152A CN 95104278 CN95104278A CN1130152A CN 1130152 A CN1130152 A CN 1130152A CN 95104278 CN95104278 CN 95104278 CN 95104278 A CN95104278 A CN 95104278A CN 1130152 A CN1130152 A CN 1130152A
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Abstract
Raw material of bittern is first through evaporated for concentration, hydraulic separation and cooling procedures to obtain intermediate potassium-magnesium double salt and by-product industrial salt and old bittern, then the potassium-magnesium double salt undergoes conversion reaction with potassium chloride and water to make potassium sulfate. The flow path is sufficiently simplified, because this invention adopts such measures as direct hydraulic separation for removing salt of evaporation-prepared liquid, direct cooling of high-temp. mixture after desalting, etc., and to create conditions for raising recovery rate and reducing production cost, the qualities of product and by-products all reach first grade of national standard. Potassium recovery rate in whole process reaches over 96%.
Description
The invention belongs to technical field of inorganic chemical industry, be a kind of be the method that raw material is produced vitriolate of tartar with bittern and Repone K.
Bittern is the by product of preparing salt by working up seawater industry, wherein contains useful chemical ingredientss such as a large amount of sodium, potassium, magnesium, sulfate radical and chlorion.According to statistics, nearly 2,000 ten thousand tons of China's sea salt annual production, about 2000 ten thousand steres of corresponding by-product bittern contain useful chemical substance altogether and reach more than 1,500 ten thousand tons.Bittern is the huge resource treasure-house that can fully utilize in the preparing salt by working up seawater industry.The bittern comprehensive utilization production technique that China is existing mainly is to convert the halogen method of evaporation to produce Repone K.Because this production method exists that technical process is long, the rate of recovery is low, production cost is high and major product Repone K is worth problems such as low, cause most of bittern chemical enterprise to be in the loss situation.
About the exploitation of bittern comprehensive utilization novel process product innovation, present domestic colleague has reached a common recognition, promptly replaces lower Repone K by being worth higher vitriolate of tartar, and the exploitation bittern is produced the vitriolate of tartar novel technique.Research in this respect, more existing at present patent reports.The technology that proposes in the U.S. Pat 430699 is with the freezing sodium sulfate of producing of bittern process, concentrates, pulverizes through Exposure to Sunlight again behind the face.Processes such as classification, flotation, conversion are produced products such as vitriolate of tartar, sodium-chlor and magnesium chloride.China's Coastal Areas is owing to the restriction of meteorological conditions, and the difficulty that solarization method concentrates bittern is bigger.Chinese patent 8810273.8 and the method for applying for a patent the high temp. salt production vitriolate of tartar that has all proposed institute of the existing bittern chemical factory of utilization by-product in 93105556.3.Most of process has adopted existing Repone K production technique in these technologies, be that bittern will make high temp. salt through converting operations such as halogen, evaporation, insulation sedimentation, filtering separation, produce Repone K by operations such as the decomposition of cooling carnallitite, washings again, produce vitriolate of tartar with high temp. salt and Repone K again.Thereby, fundamentally do not change shortcomings such as the numerous length of technical process, the rate of recovery is low.China applies for a patent in 92110336.0 the bittern that proposes, and to utilize technology be that the bittern forced evaporation is concentrated, and produces vitriolate of tartar, byproduct sodium chloride and magnesium chloride through operations such as conversion, flotation separation again after the cooling.More aforementioned two inventions of this technology have had aspect flow process significantly to be simplified.But owing in the process flotation operation is arranged, then exist the big and flotation reagent of flotation machine power consumption to problems such as the quality of byproduct Industrial Salt and purposes can exert an influence.
The objective of the invention is the problem at above-mentioned technological method existence, having released a kind of is the novel method that raw material is produced vitriolate of tartar with bittern and Repone K.This new technological method has been broken through the sorting of complete evaporation of liquid waterpower and has directly been separated desalination, high temperature mixed liquor directly cooling and cooled product (potassium magnesium double salt) are participated in key problem in technology such as conversion reaction directly, and then simplified technical process, improved the rate of recovery of bittern.
The concrete grammar of producing vitriolate of tartar with bittern and Repone K involved in the present invention: at first with bittern with later material salt washing lotion, mother liquid of vitriol carry out forced evaporation, isolate high temperature mixed liquor and crude salt slurry with the waterpower sorting method then, again the direct refrigerated separation of high temperature mixed liquor is produced potassium magnesium double salt, make potassium magnesium double salt and material potassium mother liquor later carry out one section conversion reaction again, make schoenite and mother liquid of vitriol, make schoenite, Repone K and water carry out two sections conversion reactions at last again, make the product vitriolate of tartar.
Technical process of the present invention and technical qualification are as follows:
1, at first bittern is carried out forced evaporation with later material salt washing lotion, mother liquid of vitriol, stop after reaching certain termination boiling point, obtain evaporation and finish feed liquid.Termination boiling point is controlled at 120-132 ℃.Utilize hydrocyclone that feed liquid is finished in evaporation then and carry out the waterpower sorting, make crude salt slurry and high temperature mixed liquor.During the waterpower sorting, crude salt slurry solid-liquid weight ratio was controlled at 1: 0.5-2; Temperature is 40-80 ℃.The crude salt slurry obtains Industrial Salt after the bittern washing separates, the salt washing lotion later participates in evaporation.
2, separate making potassium magnesium double salt and old halogen (magnesium chloride brine) after the high temperature mixed liquor that will obtain above cools off, cool off whole temperature and be 25-70 ℃.The further evaporation of old halogen promptly obtains another byproduct magnesium chloride.
3, potassium magnesium double salt and potassium mother liquor later are mixed in proportion carry out one section conversion reaction, make schoenite and mother liquid of vitriol.The weight proportion of conversion reaction is a potassium magnesium double salt: potassium mother liquor=1: 1-4; Temperature of reaction is 20-80 ℃, 0.5-48 hours reaction times.Mother liquid of vitriol later participates in evaporation.
4, schoenite is mixed with Repone K, water carry out two sections conversion reactions, make wet product vitriolate of tartar and potassium mother liquor.Wet vitriolate of tartar drying promptly gets the product vitriolate of tartar.The weight proportion that schoenite and Repone K and water carry out two sections conversions is: schoenite: Repone K: water=1: 0.1-1: 1.0-3.0; 20-80 ℃ of temperature of reaction; Reaction times is 0.2-48 hours.
Above-mentioned technical process is meant the flow process of formal cyclic production, the salt washing lotion, and mother liquid of vitriol can later use, and embodiment 1 and embodiment 2 are seen in concrete operations.When beginning to produce, salt washing lotion and mother liquid of vitriol that the first step evaporization process does not return then can directly evaporate with bittern, see embodiment 3.
The method of producing vitriolate of tartar involved in the present invention, feed liquid is finished in evaporation, the high temperature mixed liquor directly cools off and cooled product (potassium magnesium double salt) is participated in one section measure such as conversion directly because employing waterpower sorting technology directly separates, saved all multiple operation such as insulation sedimentation, carnallitite decomposition washing, high temp. salt separation, Repone K separation, technical process is greatly simplified.Simultaneously, add water in a large number when having avoided carnallitite to decompose, reduced the energy expenditure of bringing because of evaporation moisture content.
The present invention is the novel method that a kind of perfect bittern is produced vitriolate of tartar, obviously reduces the production cost of vitriolate of tartar.The total yield of sylvite can reach more than 96%, and this compares with 60-80% of prior art and is significantly improved.Several Chemical Composition sodium in the bittern, magnesium, potassium, sulfate radical, chlorine root have all obtained good recycling, have obtained product vitriolate of tartar, sodium-chlor, magnesium chloride respectively, and the quality of several prods all is up to state standards.Vitriolate of tartar per ton consumes 13 tons of bitterns (31 ° of Be '), 0.55 ton in Repone K, 1 ton of by-product Industrial Salt, 4.5 tons of magnesium chloride hexahydrates.
Of the present invention promoting the use of produces tangible economic results in society with the technological transformation to bittern chemical factory.
Embodiment 1
2000 kilograms of 30 ° of Be ' bitterns are added in 4000 liters of reactors with 650 kilograms of mother liquid of vitriol and 720 kilograms of salt washing lotions, open steam and carry out heating evaporation, when the feed liquid boiling point reaches 131 ℃, stop.With an impeller pump slurry is delivered in the swirler group that is made of two ∮ 100mm hydrocyclones, carried out spinning liquid and separate.Control underflow salt slurry solid-to-liquid ratio is 1: 1 (weight).Swirler underflow salt slurry enters in 2000 liters of steel basins, washs 10 minutes at 50 ℃ with 500 kilograms of bitterns, sends into then and carries out centrifugation in the whizzer, gets 724 kilograms of 245 kilograms of byproduct Industrial Salts [Nacl, 98.9% (butt)] and salt washing lotions.
The high temperature feed liquid that swirler top stream is obtained is collected in the cooling tank that a band stirs, be cooled to 65 ℃ after, suction filtration separate 363 kilograms in potassium magnesium double salt and old halogen (MgCl
2, 32%) and 1020 kilograms.
363 kilograms of potassium magnesium double salt and 550 kilograms of potassium mother liquors are sent into 1500 liters of reactors react, 30 ℃ of control reaction temperature, the reaction times is sent into whizzer after reaching 0.5 hour and separates, 665 kilograms of 258 kilograms of schoenites and mother liquid of vitriol.
258 kilograms of schoenites, 370 kg water and 93 kilograms of Repone K are dropped in 1800 liters of reactive tanks, 50 ℃ of control reaction temperature, after reaction times reaches 0.3 hour, slurry sent in the whizzer separate, and drying obtains 148 kilograms of finished product vitriolate of tartar and 562 kilograms in potassium mother liquor later.
Embodiment 2
Carry out evaporation concentration after getting 2000 kilograms of 31 ° of Be ' bitterns and 620 kilograms of later 1700 kilograms of mother liquid of vitriol and salt washing lotions being mixed.Control is evaporated termination boiling point in the time of 126 ℃, with pump slurry is sent into and is carried out the spinning liquid separation in the ∮ 100mm hydrocyclone group, and control underflow solid-to-liquid ratio is 1: 1.5 (weight).Swirler underflow salt slurry enters in 2000 liters of steel basins, washs 70 ℃ the time with 400 kilograms of bitterns, send into after 10 minutes whizzer separate byproduct Industrial Salt 152[NaCl:99.3% (butt)] kilogram, 628 kilograms of salt washing lotions.
The high temperature mixed liquor that swirler top stream is obtained is collected in the cooling tank, and after being cooled to 45 ℃ suction filtration separate 1302 kilograms of 594 kilograms in potassium magnesium double salt and old halogen.
To carry out one section conversion in 594 kilograms of potassium magnesium double salt and 2000 liters of reactors of 1500 kilograms of potassium mother liquor inputs, control reaction temperature is 50 ℃, and the reaction times is sent into after reaching 2 hours in the whizzer and separates, 1674 kilograms of 420 kilograms of schoenites and mother liquid of vitriol.
420 kilograms of schoenites and 1240 kg water, 123 kilograms of Repone K are dropped in 2000 liters of reactors, carry out two sections conversion reactions.Control reaction temperature is 15 ℃, and the reaction times separates and 202 kilograms of dry finished product vitriolate of tartar with whizzer after reaching 1 hour, 1510 kilograms in potassium mother liquor.
Embodiment 3
4000 kilograms 30 ° Be ' bitterns are added in 4000 liters of reactors, open steam and carry out heating evaporation.When reaching 128 ℃, the feed liquid boiling point stops.With an impeller pump slurry is delivered in the swirler group of being made up of 2 ∮ 100mm hydrocyclones, carried out spinning liquid and separate, control underflow salt slurry solid-to-liquid ratio was 1: 1 (weight).Salt slurry enters in 2000 liters of steel basins, washs 60 ℃ the time with 700 kilograms of bitterns, after 10 minutes, send into whizzer and carry out centrifugation, 452 kilograms of byproduct Industrial Salts [NaCl, 98.2% (butt)] and 1148 kilograms of salt washing lotions.
The high temperature mixed liquor that swirler top stream is obtained is collected in the cooling tank of strap clamp cover, be cooled to 45 ℃ after, suction filtration separate 482 kilograms in potassium magnesium double salt, old halogen (MgCl
2, 31%) and 1250 kilograms.
482 kilograms of potassium magnesium double salt and 750 kilograms of potassium mother liquors are sent in 1500 liters of reactive tanks carry out conversion reaction, controlled temperature is at 35 ℃, and the time is sent into whizzer and separates after reaching 1 hour, 911 kilograms of 321 kilograms of schoenites and mother liquid of vitriol.
321 kilograms of schoenites, 642 kg water and 180 kilograms of Repone K are dropped in 1800 liters of reactive tanks, control reaction temperature is 30 ℃, after 0.5 hour reaction times, slurry sent into that whizzer separates and drying obtains 945 kilograms in 185 kilograms of finished product vitriolate of tartar and potassium mother liquor.
Claims (7)
1, a kind of method of producing vitriolate of tartar with bittern and Repone K, it is characterized in that, at first bittern and mother liquid of vitriol, the salt washing lotion is evaporated together, reach termination boiling point and obtain finishing feed liquid, utilize hydrocyclone to isolate crude salt slurry and high temperature mixed liquor then, the crude salt slurry gets Industrial Salt after separating with the bittern washing, the direct refrigerated separation of high temperature mixed liquor is produced potassium magnesium double salt and the old halogen of byproduct, make potassium magnesium double salt and material potassium mother liquor later carry out one section conversion reaction again, make schoenite and mother liquid of vitriol, at last, make schoenite again, Repone K and water carry out two sections conversion reactions, make product vitriolate of tartar and potassium mother liquor.
2, the method for producing vitriolate of tartar according to claim 1 is characterized in that, the termination boiling point temperature that bittern evaporates with mother liquid of vitriol, salt washing lotion is 124-132 ℃.
3, the method for producing vitriolate of tartar according to claim 1 is characterized in that, when utilizing hydrocyclone to separate crude salt slurry and high temperature mixed liquor, swirler underflow solid-liquid weight ratio was controlled at 1: 0.5-2.0.
4, the method for producing vitriolate of tartar according to claim 1 is characterized in that the high temperature mixed liquor cools off the whole temperature control of the cooling of producing potassium magnesium double salt at 40-70 ℃.
5, the method for producing vitriolate of tartar according to claim 1, it is characterized in that one section conversion produces in the method for schoenite, the weight proportion of potassium magnesium double salt and potassium mother liquor is: potassium magnesium double salt: potassium mother liquor=1: 1-4, temperature of reaction: 20-60 ℃, reaction times: 0.5-48 hour.
6, the method for producing vitriolate of tartar according to claim 1, it is characterized in that two sections conversion reactions produce the weight proportion of vitriolate of tartar and be: schoenite: Repone K: water=1: 0.1-1: 1-3, temperature of reaction: 10-60 ℃, the reaction times is 0.2-48 hours.
7, the method for producing vitriolate of tartar according to claim 1, it is characterized in that with bittern washing crude salt slurry weight proportion being: the crude salt slurry: bittern=1: 1-2, temperature is 40-80 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95104278 CN1130152A (en) | 1995-04-26 | 1995-04-26 | Process for producing potassium sulfate from bittern and potassium chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95104278 CN1130152A (en) | 1995-04-26 | 1995-04-26 | Process for producing potassium sulfate from bittern and potassium chloride |
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| Publication Number | Publication Date |
|---|---|
| CN1130152A true CN1130152A (en) | 1996-09-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 95104278 Pending CN1130152A (en) | 1995-04-26 | 1995-04-26 | Process for producing potassium sulfate from bittern and potassium chloride |
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| CN (1) | CN1130152A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100439248C (en) * | 2003-12-31 | 2008-12-03 | 科学与工业研究委员会 | Process for recovery of potassium sulphate |
| CN105753019A (en) * | 2016-03-04 | 2016-07-13 | 南阳东方应用化工研究所 | Comprehensive utilization method for producing potassium sulfate and magnesium resources through magnesium sulfate conversion method |
-
1995
- 1995-04-26 CN CN 95104278 patent/CN1130152A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100439248C (en) * | 2003-12-31 | 2008-12-03 | 科学与工业研究委员会 | Process for recovery of potassium sulphate |
| CN105753019A (en) * | 2016-03-04 | 2016-07-13 | 南阳东方应用化工研究所 | Comprehensive utilization method for producing potassium sulfate and magnesium resources through magnesium sulfate conversion method |
| CN105753019B (en) * | 2016-03-04 | 2017-07-04 | 南阳东方应用化工研究所 | A kind of method of comprehensive utilization of magnesium sulfate conversion method production potassium sulfate and magnesium resource |
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