CN1035811C - Method for preparing potassium sulfate from bittern and potassium chloride - Google Patents
Method for preparing potassium sulfate from bittern and potassium chloride Download PDFInfo
- Publication number
- CN1035811C CN1035811C CN 92110336 CN92110336A CN1035811C CN 1035811 C CN1035811 C CN 1035811C CN 92110336 CN92110336 CN 92110336 CN 92110336 A CN92110336 A CN 92110336A CN 1035811 C CN1035811 C CN 1035811C
- Authority
- CN
- China
- Prior art keywords
- bittern
- potassium
- potassium sulfate
- repone
- salt
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
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- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 title claims abstract description 34
- 241001131796 Botaurus stellaris Species 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000001103 potassium chloride Substances 0.000 title claims abstract description 14
- 235000011164 potassium chloride Nutrition 0.000 title claims abstract description 14
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 title claims abstract description 13
- 229910052939 potassium sulfate Inorganic materials 0.000 title claims abstract description 13
- 235000011151 potassium sulphates Nutrition 0.000 title claims abstract description 13
- 150000003839 salts Chemical class 0.000 claims abstract description 19
- 239000000047 product Substances 0.000 claims abstract description 10
- 239000006227 byproduct Substances 0.000 claims abstract description 7
- 208000006558 Dental Calculus Diseases 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- 238000005188 flotation Methods 0.000 claims description 13
- 229910052736 halogen Inorganic materials 0.000 claims description 10
- 150000002367 halogens Chemical class 0.000 claims description 10
- 229940037003 alum Drugs 0.000 claims description 9
- 239000006210 lotion Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- GMLLYEDWRJDBIT-UHFFFAOYSA-J magnesium;dipotassium;disulfate Chemical compound [Mg+2].[K+].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GMLLYEDWRJDBIT-UHFFFAOYSA-J 0.000 claims description 6
- -1 amine compound Chemical class 0.000 claims description 2
- 125000002091 cationic group Chemical group 0.000 claims description 2
- 239000008396 flotation agent Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000011591 potassium Substances 0.000 abstract description 4
- 229910052700 potassium Inorganic materials 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 abstract description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 abstract description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052794 bromium Inorganic materials 0.000 abstract description 2
- 239000003337 fertilizer Substances 0.000 abstract description 2
- 229940050906 magnesium chloride hexahydrate Drugs 0.000 abstract description 2
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 abstract description 2
- 229940072033 potash Drugs 0.000 abstract description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 abstract description 2
- 235000015320 potassium carbonate Nutrition 0.000 abstract description 2
- 239000012267 brine Substances 0.000 abstract 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000001704 evaporation Methods 0.000 description 7
- 230000008020 evaporation Effects 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000012452 mother liquor Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 3
- 238000003672 processing method Methods 0.000 description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000005068 transpiration Effects 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- 241000272875 Ardeidae Species 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229960002337 magnesium chloride Drugs 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 229940091250 magnesium supplement Drugs 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000001120 potassium sulphate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Cosmetics (AREA)
- Fertilizers (AREA)
Abstract
The present invention relates to a method for preparing potassium sulfate by using bittern of salt field and potassium chloride. The quality of the potassium sulfate product reaches the index of imported potash fertilizer, the industrial salt reaches the national standard, and the old brine can be used as a raw material for extracting bromine and producing magnesium chloride hexahydrate. The recovery rate of potassium in the whole process is more than 95%, and each 1 ton of potassium sulfate needs about 20 tons of bittern, 1.9 tons of byproduct salt and 7.5 tons of old bittern. No waste material is discharged in the process. If the technology is adopted to reform domestic bittern plants, very obvious social and economic benefits can be generated.
Description
The present invention relates to a kind of production Technique of Potassium Sulphate, is to be the processing method that raw material is produced vitriolate of tartar with salt pan bittern and Repone K.
Bittern is the bittern of by-product in a kind of preparing salt by working up seawater industry, wherein contains mineral ions such as potassium, magnesium, Sulfuric acid disilver salt, chlorine.For many years, people have carried out number of research projects to the extractive technique of sylvite wherein, and to produce Repone K technology the most ripe for the halogen method of evaporation of converting that adopts with China salinization factory at present.Its production process is: bittern at first with after later the material ginseng is converted is forced high temperature evaporation, and complete evaporation of liquid goes out the mixing salt by product through insulation is settlement separate, obtains the high temperature clear liquor simultaneously and cools off, and makes the intermediates carnallitite and pays the old halogen of product.Carnallitite adds the water decomposition washing through twice again and finally makes product Repone K.Production reality by decades as can be seen, this method exists following weak point.At first because technical process is longer, pay in addition the product mixing salt band lose, cause the potassium rate of recovery of bittern lower.Secondly, when decomposing carnallitite, need replenish big water gaging, improve energy consumption, thereby increased the cost of Repone K.In addition, in its production process, need to pay to produce a large amount of mixing salt waste residues that does not still have industrial use, caused the wasting of resources and environmental pollution.For above-mentioned reasons, the Repone K production cost of present many bittern chemical factory is higher than market value far away, causes enterprise to be in the very situation of difficulty.
Propose a kind of solarization method bittern in the U.S. Pat 4306880 and produced the method for Repone K.Its technical process is: at first bittern is gone out sodium sulfate through subzero fractionation, then make operations such as bittern is concentrated through Exposure to Sunlight, pulverizing, stage floatation, conversion produce products such as vitriolate of tartar, sodium-chlor and magnesium chloride again.Because the meteorological conditions of China's Coastal Areas is limit, the difficulty that Exposure to Sunlight concentrates bittern is bigger, causes this technology to be difficult to implement in China.
The present invention is directed to the problems referred to above, proposition is the operational path that raw material is produced vitriolate of tartar with bittern and Repone K, thereby make product form become the higher vitriolate of tartar of price, and the vitriol in the bittern has been carried out sufficient utilization and effectively separated with the magnesium salts and the salt of receiving, eliminated salt waste residue problem.
The present invention is a kind of processing method of being produced vitriolate of tartar by bittern and Repone K, its concrete grammar is that at first bittern is produced mixing sylvite and paid and produce an old halogen after transpiration cooling, to mix sylvite and alum washing lotion then transforms by proportioning (weight), flotation separation makes thick leonite and Industrial Salt again, at last, to react by this proportioning (weight) with Repone K and water through the schoenite after the potassium sulfate mother liquid washing and obtain vitriolate of tartar and potassium sulfate mother liquid, the latter recycles.
Technical process of the present invention and processing condition are as follows:
(1) the raw material bittern concentration that is suitable for of the present invention is between 28 ° of be '-35 ° Be '.At first will evaporate and be warming up to 118 ℃-135 ℃, cool then between 20 ℃-80 ℃, pulp separation must be mixed sylvite and the old halogen of by-product by the mixing bittern that bittern and thick leonite mother liquor are converted.
(2) will mix sylvite and mix with alum washing lotion later and carry out one section conversion, its proportioning (weight) is: mixing sylvite: alum washing lotion=1: 0.5-0.1, and invert point is 20 ℃-80 ℃, transformation time is 0.5-24 hour.
(3) one section conversion is finished feed liquid and is added in the flotation machine and carry out flotation separation, the thick leonite of floating product and tailings Industrial Salt and thick leonite mother liquor.Flotation flowsheet is that one-level is roughly selected, one-level is selected and one-level is scanned, and flotation collector is that the consumption of cationic fat amine compound, leonite per ton is the 10-1000 gram, adds pore forming material in the floatation process.
(4) thick leonite is separated with potassium sulfate mother liquid washing back, get schoenite and alum washing lotion, press schoenite then: Repone K: the proportioning of water=1: 0.1-1.0: 1.0-3.0 (weight), under 10 ℃-80 ℃ temperature, carry out two sections conversions, after 0.5-24 hour, can prepare vitriolate of tartar, obtain the vitriolate of tartar mother liquor of precipitation of ammonium simultaneously and recycle.
In the whole technological process of the present invention, the total rate of recovery of sylvite is more than 95%, and the 60-80% of this and present bittern Repone K technology is greatly improved, and obtains Industrial Salt byproduct and old halogen when making vitriolate of tartar again.Quality of potassium sulfate reaches international potash fertilizer standard, and KCE content is more than 50%, and Industrial Salt also reaches country and uses the salt index for three grades, and the old halogen of by-product can be as the raw material that extracts bromine and production magnesium chloride hexahydrate.Vitriolate of tartar per ton consumes 20 tons of bittern 29 Be ', and 0.5 ton in Repone K is paid and produced 1.9 tons of Industrial Salts, 7.5 tons of old halogen.
In sum, processing method of the present invention has value of the product height (price of vitriolate of tartar is 2 times of Repone K), bittern comprehensive utilization degree height, and production cost is low, characteristics such as no waste material.If adopt present method that domestic bitter chemical plant is transformed, will produce tangible economic results in society.
Embodiment 1:
Get bittern (29 ° of Be ') 2000 gram and mix with mother liquid of vitriol 520 grams later and carry out evaporation concentration, evaporate termination boiling point and be controlled at 124 ℃, be cooled to 35 ℃ then.The feed liquid separation be will cool off and mixed potassium 528 grams and old halogen 750 grams made.
528 grams that front and back are made mix sylvite and restrain to mix with the alum washing lotion 390 of turning one's head and carry out one section conversion reaction, control reaction temperature is 20 ℃, time drops into reaction material flotation machine again after reaching 5 hours and carries out flotation separation, add amine collector 0.2 gram and pore forming material 0.3 gram, through one-level roughly select, one-level is selected and one-level is scanned, separate obtaining thick leonite 206 grams and 191 gram Industrial Salts (sodium chloride-containing 93.20%), obtain mother liquid of vitriol 521 grams simultaneously.
The thick leonite of 206 grams that flotation separation is obtained separates after with mother liquor washing later to such an extent that schoenite 190 grams and alum washing lotion 390 restrain.190 gram schoenites, 234 gram water and 51 gram Repone K are carried out two sections conversion reactions, and temperature of reaction is 60 ℃, and controlling reaction time is separated to such an extent that product vitriolate of tartar 101 restrains (K after 0.5 hour
2O=50.51%) and potassium sulfate mother liquid 374 gram.
Embodiment 2:
Carry out evaporation concentration after getting 32 ° of Be ' bitterns, 2000 grams and later mother liquid of vitriol 772 grams mixing, the evaporation final temperature is 132 ℃.Separate after complete evaporation of liquid is cooled to 60 ℃, make and mix sylvite 620 grams and old halogen 1002 restrains.
620 grams that transpiration cooling is made mix sylvite and carry out one section conversion reaction with alum washing lotion 582 grams later under 60 ℃ of temperature, controls to transform after 0.5 hour in the slurry adding flotation machine and carry out flotation separation.Add fatty amine collector 0.3 gram, pore forming material 0.5 gram is roughly selected through one-level, and one-level is selected scans with one-level and separate to such an extent that thick leonite 305 grams and Industrial Salt 125 restrain (sodium chloride-containing 90.50%), makes mother liquid of vitriol 772 simultaneously and restrains.
The thick leonite of 305 grams that flotation is made separates after with 561 gram potassium sulfate mother liquids washings to such an extent that soft arcanite 284 grams and alum washing lotion 582 restrain.Schoenite 284 gram, water 351 grams and Repone K 78 grams are mixed carry out two sections conversion reactions, temperature of reaction is 10 ℃, the period separate after reaching 2 hours vitriolate of tartar 152 gram (K
2O=51.01%), get potassium sulfate mother liquid 561 grams.
Claims (4)
- One, a kind ofly prepare the method for vitriolate of tartar with bittern and Repone K, this method may further comprise the steps:1, concentration be the bittern of 28-35 ° of Be ' through being evaporated to 118-135 ℃ of postcooling to 25-80 ℃, produce then and mix sylvite and the old halogen of by-product;
- 2, will mix sylvite and alum washing lotion by 1: the proportioning of 0.5-1.0 (weight) transforms 0.5-24 hour under 28-80 ℃ of temperature;
- 3, be flotation agent with cationic fat amine compound, the employing flotation step that one-level is roughly selected, one-level is selected, one-level is scanned is carried out flotation separation and is obtained thick leonite and Industrial Salt;
- 4, will be through the schoenite after the potassium sulfate mother liquid washing and Repone K and water by 1: the proportioning of 0.1-1.0: 1.0-3.0 (weight), under 10-80 ℃ temperature, reacted 0.5-24 hour, obtain the product vitriolate of tartar.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92110336 CN1035811C (en) | 1992-09-12 | 1992-09-12 | Method for preparing potassium sulfate from bittern and potassium chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92110336 CN1035811C (en) | 1992-09-12 | 1992-09-12 | Method for preparing potassium sulfate from bittern and potassium chloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1084492A CN1084492A (en) | 1994-03-30 |
| CN1035811C true CN1035811C (en) | 1997-09-10 |
Family
ID=4944752
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92110336 Expired - Fee Related CN1035811C (en) | 1992-09-12 | 1992-09-12 | Method for preparing potassium sulfate from bittern and potassium chloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1035811C (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1075041C (en) * | 1996-06-19 | 2001-11-21 | 死海工业有限公司 | CO-production of potassium sulfate and sodium sulfate |
| CA2552104C (en) * | 2003-12-31 | 2009-11-24 | Council Of Scientific And Industrial Research | Process for recovery of sulphate of potash |
| US7041268B2 (en) | 2004-03-30 | 2006-05-09 | Council Of Scientific And Industrial Research | Process for recovery of sulphate of potash |
| EP1945567B1 (en) * | 2005-11-10 | 2010-07-21 | Council Of Scientific & Industrial Research | Improved process for the recovery of sulphate of potash (sop) from sulphate rich bittern |
| CN104774069A (en) * | 2015-04-14 | 2015-07-15 | 张义盼 | Novel fertilizer and preparation method thereof |
| CN105237049A (en) * | 2015-09-01 | 2016-01-13 | 格尔木康生钾业科技发展有限公司 | Production process of potassium sulfate specially used for drop irrigation |
| CN106698480A (en) * | 2016-11-30 | 2017-05-24 | 东至天孚化工有限公司 | Preparation of potassium sulfate by employing bittern evaporation-flotation method |
| CN107188208B (en) * | 2017-07-06 | 2019-11-22 | 化工部长沙设计研究院 | A method of Shoenite is extracted with the carnallite of containing magnesium sulfate |
| CN111547745A (en) * | 2020-05-18 | 2020-08-18 | 天津君瑞和科技有限公司 | Method for removing sodium chloride from bittern produced by seawater |
| CN115304083B (en) * | 2022-08-25 | 2023-07-07 | 湖北振华化学股份有限公司 | Method for circularly extracting bromine from glaserite mother liquor in production process of preparing potassium sulfate from mirabilite |
-
1992
- 1992-09-12 CN CN 92110336 patent/CN1035811C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1084492A (en) | 1994-03-30 |
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