CN1156397C - Method of formulating alkali metal salts - Google Patents
Method of formulating alkali metal salts Download PDFInfo
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- CN1156397C CN1156397C CNB998143782A CN99814378A CN1156397C CN 1156397 C CN1156397 C CN 1156397C CN B998143782 A CNB998143782 A CN B998143782A CN 99814378 A CN99814378 A CN 99814378A CN 1156397 C CN1156397 C CN 1156397C
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- Prior art keywords
- solution
- sodium bicarbonate
- vitriolate
- tartar
- sodium
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- 238000000034 method Methods 0.000 title claims abstract description 47
- 229910052783 alkali metal Inorganic materials 0.000 title 1
- -1 alkali metal salts Chemical class 0.000 title 1
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 132
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 66
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 65
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 45
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 33
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 33
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 27
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 22
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000013305 food Nutrition 0.000 claims abstract description 10
- 238000001556 precipitation Methods 0.000 claims abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 86
- 208000006558 Dental Calculus Diseases 0.000 claims description 44
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 42
- 239000011734 sodium Substances 0.000 claims description 40
- 150000001875 compounds Chemical class 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 19
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 14
- 229910021529 ammonia Inorganic materials 0.000 claims description 13
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 12
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 12
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 12
- 235000019270 ammonium chloride Nutrition 0.000 claims description 9
- 229910052700 potassium Inorganic materials 0.000 claims description 9
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 7
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 7
- 239000004571 lime Substances 0.000 claims description 7
- 239000011591 potassium Substances 0.000 claims description 7
- 229920006395 saturated elastomer Polymers 0.000 claims description 7
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 6
- YTAHJIFKAKIKAV-XNMGPUDCSA-N [(1R)-3-morpholin-4-yl-1-phenylpropyl] N-[(3S)-2-oxo-5-phenyl-1,3-dihydro-1,4-benzodiazepin-3-yl]carbamate Chemical compound O=C1[C@H](N=C(C2=C(N1)C=CC=C2)C1=CC=CC=C1)NC(O[C@H](CCN1CCOCC1)C1=CC=CC=C1)=O YTAHJIFKAKIKAV-XNMGPUDCSA-N 0.000 claims description 6
- 235000011089 carbon dioxide Nutrition 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 5
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims description 4
- 239000012047 saturated solution Substances 0.000 claims description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims 1
- 239000003337 fertilizer Substances 0.000 abstract description 4
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 abstract description 3
- 229910052939 potassium sulfate Inorganic materials 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 abstract 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 abstract 2
- 239000001099 ammonium carbonate Substances 0.000 abstract 2
- 235000011151 potassium sulphates Nutrition 0.000 abstract 2
- 239000012267 brine Substances 0.000 abstract 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 abstract 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 abstract 1
- 241001131796 Botaurus stellaris Species 0.000 description 32
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 11
- 239000000706 filtrate Substances 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 229910052708 sodium Inorganic materials 0.000 description 8
- 239000006200 vaporizer Substances 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 239000011780 sodium chloride Substances 0.000 description 7
- 239000012071 phase Substances 0.000 description 6
- 230000018044 dehydration Effects 0.000 description 5
- 238000006297 dehydration reaction Methods 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 239000001110 calcium chloride Substances 0.000 description 3
- 229910001628 calcium chloride Inorganic materials 0.000 description 3
- 235000011148 calcium chloride Nutrition 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000010977 unit operation Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 229910052925 anhydrite Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- HMMFCFULKBCODX-UHFFFAOYSA-M azanium sodium sulfuric acid sulfate Chemical compound S(=O)(=O)([O-])[O-].[Na+].S(=O)(=O)(O)O.[NH4+] HMMFCFULKBCODX-UHFFFAOYSA-M 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 1
- VVJRSSJSRXEOQL-UHFFFAOYSA-N calcium;potassium;sulfuric acid;hydrate Chemical compound O.[K].[K].[Ca].OS(O)(=O)=O.OS(O)(=O)=O VVJRSSJSRXEOQL-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000013066 combination product Substances 0.000 description 1
- 229940127555 combination product Drugs 0.000 description 1
- AXZAYXJCENRGIM-UHFFFAOYSA-J dipotassium;tetrabromoplatinum(2-) Chemical compound [K+].[K+].[Br-].[Br-].[Br-].[Br-].[Pt+2] AXZAYXJCENRGIM-UHFFFAOYSA-J 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- 229910001487 potassium perchlorate Inorganic materials 0.000 description 1
- ILRLTAZWFOQHRT-UHFFFAOYSA-N potassium;sulfuric acid Chemical compound [K].OS(O)(=O)=O ILRLTAZWFOQHRT-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000015424 sodium Nutrition 0.000 description 1
- BAZAXWOYCMUHIX-UHFFFAOYSA-M sodium perchlorate Chemical compound [Na+].[O-]Cl(=O)(=O)=O BAZAXWOYCMUHIX-UHFFFAOYSA-M 0.000 description 1
- 229910001488 sodium perchlorate Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/02—Preparation by double decomposition
-
- 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
-
- 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
- C01D5/06—Preparation of sulfates by double decomposition
- C01D5/08—Preparation of sulfates by double decomposition with each other or with ammonium sulfate
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D1/00—Fertilisers containing potassium
- C05D1/02—Manufacture from potassium chloride or sulfate or double or mixed salts thereof
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D7/00—Fertilisers producing carbon dioxide
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Fertilizers (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treating Waste Gases (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Methodology for formulating sodium bicarbonate and potassium sulfate. In one embodiment, sodium sulfate and ammonium bicarbonate are reacted to form sodium bicarbonate with the remaining liquor or brine treated with sulfuric acid to remove carbonates with subsequent precipitation of potassium sulfate. A further embodiment employs ammonium bicarbonate, ammonia gas or carbon dioxide to precipitate sodium bicarbonate. The result of the methods is the production of high quality fertilizer and food grade sodium bicarbonate.
Description
The present invention relates to the compound method of alkaline earth salt, specifically, the present invention relates to the production method of food grade sodium bicarbonate and fertilizer grade vitriolate of tartar.
The technology issue of existing a large amount of relevant preparation alkaline earth salts.For example, the making of sodium bicarbonate just has many diverse ways.However, original supercarbonate synthesis unit methodology causes improving synthetic cost, thereby is restricted because energy use efficiency is low.Another further limits is that known technology can't effectively utilize the unit operation method to carry out the making of salt.Usually, the making of certain high-quality product has the byproduct of association usually, and the non-conformity of quality of these byproducts closes commercial requirement, perhaps needs to carry out excessive investment and makes these byproducts meet commercial requirement.
The representative of previous technology is the United States Patent (USP) 3.429.657 that authorized D ' Arcy on February 25th, 1969, discloses a kind of method that reclaims and make sodium salt.In this reference paper, the bittern and the sodium perchlorate that are loaded with potassium react, and are settled out potassium perchlorate.With switching method removal immediately, potassium dissociates potassium and muriate, vitriol, nitrate and INTER ALIA chemical combination then with sodium.
The object of the invention provides the compound method of a kind of food grade sodium bicarbonate and fertilizer grade vitriolate of tartar, also can be applicable to fertilizer technology.
The compound method of a kind of food grade sodium bicarbonate and vitriolate of tartar comprises the following steps:
A) provide the source of fluid sulphuric acid sodium;
B) be provided for being settled out the source of the bicarbonate of ammonia of sodium bicarbonate;
C) above-mentioned sodium sulfate is contacted with above-mentioned bicarbonate of ammonia;
D) be settled out sodium bicarbonate and form a kind of solution;
E) filter out above-mentioned sodium bicarbonate and obtain containing the solution of sodium sulfate;
F) make from the solution of step e) saturated with sodium sulfate;
G) above-mentioned solution is contacted with bicarbonate of ammonia, ammonia or carbonic acid gas, be settled out more sodium bicarbonate;
H) sodium bicarbonate that is settled out filtration step g);
I) will be from step e) and h) sodium bicarbonate combine, wash, become the sodium bicarbonate of food grade; And
J) will be from step I) solution be cooled to 0 ℃, guarantee to form the saltcake precipitation;
K) with sulfuric acid to from step j) solution handle, the carbonate inorganics is changed into the vitriol inorganics and discharges carbon dioxide;
L) will be from step k) solution be heated between 30 ℃ to 40 ℃;
M) will be from step l) solution contact with Repone K, be settled out vitriolate of tartar.
This method comprises that also the vitriolate of tartar that will be settled out separates, and the step of washing with Repone K.With lime to handling, to discharge the step of ammonia from the solution of above-mentioned vitriolate of tartar separating step.Above-mentioned ammonia is reclaimed, send into the step of step g).Described filtered liquid is carried out the step of evaporation process.Described sodium sulfate is between 1.30 to 1.34 at the proportion under 40 ℃.Solution proportion from step d) is 1.25, and this solution consisting of by weight: 10.4% sodium sulfate, 17.1% ammonium sulfate, 8% to 12% sodium bicarbonate and the bicarbonate of ammonia of excess.Sodium sulfate from step e) contains Na
2SO
410H
2O.The proportion of solution under 40 ℃ from step f) is 1.285.From step j) solution be the saturated solution of a kind of sodium sulfate, ammonium sulfate and sodium bicarbonate.Described vitriolate of tartar quantum of output is at least 80%, purity at least 98%.The compound method of a kind of food grade sodium bicarbonate and vitriolate of tartar comprises the following steps:
A) provide the source of fluid sulphuric acid sodium;
B) provide the source of bicarbonate of ammonia;
C) above-mentioned sodium sulfate is contacted with above-mentioned bicarbonate of ammonia;
D) be settled out sodium bicarbonate and form a kind of solution;
This liquid that e) will form in step d) contacts with sodium sulfate, is settled out sodium bicarbonate and forms a kind of solution;
F) make the solution that in step e), forms saturated with sodium sulfate;
G) filter out solid in the solution of step f);
H) solution from step f) is contacted with sulfonic acid, to be settled out carbonate;
I) will be from step h) solution be cooled to 0 ℃, form the saltcake precipitation;
J) will be from step I) solution be heated to 30 ℃ to 40 ℃; And
K) with Repone K to from step j) solution handle, to be settled out vitriolate of tartar;
L) to from step k) solution carry out evaporation process, recover the content value of potassium, and loop back step k again); And
M) dry above-mentioned vitriolate of tartar.
This method comprises that also lime and ammonium chloride are to from step l) the step handled of surplus solution.Discharge ammonia, and these ammonias are recycled.Used Klorvess Liquid is sent into step k), carry out recirculation.
Confirm, after sodium bicarbonate forms,, can from solution, remove very successfully with the form of sodium sulfate with saltcake and sodium bicarbonate by solution being cooled to 0 ℃.The solubleness of saltcake can be come out by ammonium sulfate-sodium sulfate calphad in this system.By increasing the recirculation of saltcake, improve the sodium sulfate in the supercarbonate loop, can reduce the solubleness of supercarbonate, improve the efficient of this technology.
Again initial reagent is converted into the vitriolate of tartar aspect, confirms, the mol ratio of potassium and ammonium ion is remained on 5 or higher, can obtain special success.This mol ratio can be guaranteed the high transformation efficiency in this technology subordinate phase.
Fig. 1 process flow sheet illustrates the first part that adopts a kind of technology of the present invention;
Fig. 1 a illustrates the second section of technology shown in Figure 1;
Fig. 1 b illustrates the third part of technology shown in Figure 1;
Fig. 2 is a process flow sheet, illustrates the first part that adopts a kind of process variations of the present invention;
Fig. 2 a illustrates the second section of technology shown in Figure 2;
Fig. 2 b illustrates the third part of technology shown in Figure 2.
In each figure, similar numeral refers to similar parts.
Fig. 1 illustrates the technology that adopts first kind of implementation method of the present invention to 1b.
The source of fluid sulphuric acid sodium 10% aqueous solution and centrifugal filtrate water 12 is discussed later.These solution are mixed in groove 14 than weighing 1.30 under 40 ℃.In strainer 16 this solution is filtered then, this strainer can be, for example, and one 5 microns strainer.Solid 18 is removed, and filtrate 20 then is admitted to first sodium bicarbonate crystallizer tank 27.
Feeding intake of water, ammonia and carbonic acid gas all indicates that with numeral 24 these raw materials react in groove 22, with carbonate synthesis hydrogen ammonium.Crystallizer tank 27 is sent into solid phase prod in the bicarbonate of ammonia centrifuge dehydration in whizzer 26 that generates then.Recirculation loop 28 is used for bicarbonate of ammonia and solution are sent into reactive tank 29, carries out recirculation.The combination product of groove 29 is sodium bicarbonate.Mixture filters and centrifuge dehydration with strainer 30.In groove 32, sodium bicarbonate is washed, centrifuge dehydration in whizzer 34 then, the solid that stays is the food grade sodium bicarbonate.Water for cleaning is return slot 14 then.
Proportion from the solution of strainer 30 is 1.25, and its composition comprises about 10.4% sodium sulfate, 17.1% ammonium sulfate and 8% bicarbonate of ammonia, and excessive bicarbonate of ammonia then is used for reacting with saltcake (discussing in the back).This solution under 40 ℃ the temperature, reacts with the saltcake (being discussed later) that forms at the cooling stages of this technology in groove 36, produces sodium bicarbonate to use from the excessive bicarbonate of ammonia of crystallizer tank 29.Another kind method is to add bicarbonate of ammonia solid, slurry or solution at second section (in groove 36).
In groove 40, add solid sodium sulfate for solution from groove 36, to constitute sodium sulfate/ammonium sulfate saturated solution from source 41.Complete reaction needs to have in the solution enough bicarbonate of ammonia to exist, and therefore, if content is supplied, then must add, and makes solution reach 1.285 proportion.Slurry from groove 40 filters with strainer 42.Sodium bicarbonate solid 48 is sent into groove 46 (Figure 1A), and 44 of solution turn back to groove 32 and further handle, to isolate more sodium bicarbonate.Then solution 44 is sent into groove 46 (Figure 1A).Can generate solid sodium sulfate by the pure sodium sulfate that drops into is carried out processed,, guarantee the saturation ratio in loop with the circuit volume of control from the sodium bicarbonate loop.
Shown in Figure 1A, groove 46 contains and enough makes the sedimentary acid of carbonate cpds.Will be through this acid-treated solution at water cooler 48 internal cooling to 0 ℃, to reclaim saltcake and at strainer 50 inner filtrations.Send the saltcake that reclaims back to sodium bicarbonate crystallizer tank 36.
It is that 25.25% ammonium sulfate and weight percent are up to 11% sodium sulfate that filtered liquid contains weight percent, and this filtered liquid is sent to groove 52, is heated between 30 ℃ to 40 ℃, then with solid 65 chemical combination from strainer 66.Bonded solution is admitted to groove 54, react with solid Repone K, generation contains the ammonium chloride solution of weight percent 20%, and this solution contains: by weight percentage, and about 20.2% ammonium chloride, 6.7% Repone K, 4.9% sodium-chlor, 2.3% (x)
2SO
4(x=Na, K and have the vitriolate of tartar solid mixed crystallization of 10% to 20% ammonium sulfate) herein.
This solution filters in strainer 56, and the solid part that leaches contains about by weight 5% Repone K, the vitriolate of tartar of 80%-85%, the ammonium sulfate of 10%-15%.This solid part carries out chemical combination in groove 58 with from the water and the Repone K bittern of groove 60.The vitriolate of tartar solid is carried out centrifuge dehydration, in strainer 62, filter, under 25 ℃, carry out crystallization again then with Klorvess Liquid.Remaining ammonium sulfate is changed into vitriolate of tartar.Promptly obtain to be higher than the vitriolate of tartar of 98% specification.
In the unit operation in future, from vitriolate of tartar handle, also promptly filtered liquid will be with the unit operation method processing shown in Fig. 1 c in other words from the solution of strainer 56.Solution evaporates in vaporizer, improves the concentration of ammonium chloride solution, so that when cooling, reduces Repone K in the solution and residual vitriol as far as possible.This solution uses strainer 67 to filter, and solid material reclaims in groove 54.The filtered liquid that comprises about 22% to 30% ammonium chloride reacts at reactor 68 and calcium oxide, and the ammonia that discharges is reclaimed.The calcium chloride of reaction output can be sent into settling vessel 70 or washer 72 according to use needs subsequently.
After determining technology according to first kind of implementation method of the present invention, an example that can form this technology is as follows:
Example 1
Before the vitriolate of tartar operation, carry out the supercarbonate precipitation
Feed intake-1 liter; Proportion 1.3
350g/l Na
2SO
4
Fs
Output NaHCO
3
Bittern current after reaction finishes contain:
The Na of 130g
2SO
410.4% Na
2 SO
440 ℃
213.8g (NH
4)
2SO
40.95 liter of 17.1% proportion 1.250 is molten
Liquid
The NaHCO of 100g
38.0%
The H of 907g
2
O
1359.8
The NaHCO of output 172g
3Solid
The subordinate phase estimation
Consume: 544gNH
3A) 25.07gNH
3+ 64.9gCO
2
142.5gCO
2 B)51.2gNH
3+132.6gCO
2
The bittern that subordinate phase is 0.95 liter will dissolve following material:
A) 2 gram molecular weights 1 gram molecular weight B)
Na
2SO
410H
2O Na
2SO
410H
2O
(332g) (664g)
272gNa
2SO
4 16.2％Na
2SO
4 414gNa
2SO
4 20.7％Na
2SO
4
213.8g(NH
4)
2SO
4 18.9％(NH
4)
2SO
4 213.8g(NH
4)
2SO
4 10.7％(NH
4)
2SO
4
100gNaHCO
3 5.9％NaHCO
3 100gNaHCO
3 5.0％NaHCO
3
1087gH 2 O 65.1％H
2O
1267gH 2 O 63.4％H
2O
1672.8 1999
1.275 1.5 liters of bittern of 1.313 liters of bittern of proportion, 1.300 proportions
The composition of subordinate phase final solution:
A) B)
167.3gNa
2SO
4 10％Na
2SO
4 200gNa
2SO
4 10％Na
2SO
4
311g(NH
4)
2SO
4 18.9％(NH
4)
2SO
4 412g(NH
4)
2SO
4 20.2％(NH
4)
2SO
4
1087gH 2 O 63.1％H
2O
1267gH 2 O 61.8％H
2O
1644.5g solution 2039g solution
Output NaHCO
392.9g output NaHCO
3193.2g
Proportion 1.265,1.31 liters of bittern proportions 1.300 of output, 1.61 liters of solution of output
The supercarbonate precipitation
412g(NH
4)
2SO
4
200gNaSO
4 + 160×98＝93.3gH
2SO
4
160gNaHCO
3 84(2)
1267gH
2O
2039g (1.6 liters)
Proportion 1.285
Become at this:
412g(NH
4)
2SO
4
335gNa
2SO
4
1267gH
2
O
2014g (1.6 liters)
Proportion 1.265
Must add Na
2SO
4To reach proportion is 1.30 saturation ratio
A) 1.61 liters * 1.30=2080
Therefore:
412g(NH
4)
2SO
4
400gNa
2SO
4
1267gH
2
O
Add up to 2079g, 1.6 liters
Cooling
412g(NH
4)
2SO
4 28.7％
116gNa
2SO
4 8.0％
907gH 2 O 63％
1435g solution
Send into vaporizer
NH
4Cl 330.8g 21.9％
KCl 130g 8.6％
NaCl 94.7g 6.3％
x-SO4 50 3.3％
H 2 O 907g 60.0
1512g
Contain 33% NH
4After the Cl :-2.8%KCl
Afterwards :-2.0%K
2SO
4
Therefore: 330.8=1002g
.33
Evaporation load=907-623=284g
0.79t/t Na
2SO
4
Add the 0.5t that is used to clean
1.29t H
2O/t Na
2SO
4
K
2SO
4Reaction
A) from (NH
4)
2SO
4K
2SO
4=
412* 174=543g
132
B) from Na
2SO
4K
2SO
4=
116* 174=142g
142
C) loss of K2SO4=
-43g
K
2SO
4Total amount=642g
KCl reclaims
A) the KCl transport reaction=
685* 2 * 74=582g
174
B) KCl=50g of loss in the tailing
C) therefore, required KCl=632g
K
2SO
4Output=
642* 100=93.7%
685
The KCl efficiency of conversion=
582* 100=92.1%
632
Benchmark: 1 ton Na
2SO
4Feed intake
| Drop into | Product |
| Fs 0.153 ton of NH 30.396 ton CO 32.52 ton H 2O | 0.48 ton NaHCO 3 |
| Subordinate phase 644 gram Na 2SO 4 10H 20.142 ton of NH of O 30.368 ton CO 2 | 0.53 ton NaHCO 3 |
| Supercarbonate precipitation+Na 2SO 4Saturated | Filter the clarifying bittern of output |
| 0.26 ton H 2SO 40.18 ton Na 2SO 4 | |
| At water cooler internal cooling to 0 ℃-BTU ' s | 1.8 ton Na 2SO 4 10H 2O |
| Bittern in the water cooler | 1.14 ton (NH 4) 2SO 428.7% 0.32 ton of Na 2SO 48.0% 2.52 ton of H 2Totally 3.99 tons of O 63% |
| The KCl=1.76 ton | 1.78 ton K 2SO 4 |
| Be evaporated to 33% NH 4Cl, 1.29 tons/Na per ton 2SO 4 | 0.92 ton NH 40.05 ton of K of 0.08 ton of KCl solid of Cl bittern 2SO 40.28 1.73 tons of H of ton KCl 20.08 ton of K of O 2SO 4Totally 2.78 tons are reclaimed 0.36 ton |
| It with CaO content 0.57 ton of lime treatment of 85% | 0.29 ton NH, bittern: 0.995CaCl 20.08 0.05 ton of K of ton KCl 2SO 41.73 ton H 2O is at 75 to 90 ℃ following 2.815 tons |
Fig. 2 has described a substituting reaction scheme to Fig. 2 b with graphic.In this reaction scheme, before producing salt of wormwood, make solution saturated with anhydrite.
In this implementation method, sodium bicarbonate is to produce in the crystallization apparatus 22, operation and Fig. 1 of process basic identical to the described operation of Fig. 1 b.In groove 36, make bittern or filtrate saturated, at strainer 38 inner filtrations, remove and abandon insolubles then with anhydrous sodium sulphate.The filtrate of this operation is reacted with bicarbonate of ammonia in groove 80.A kind of alternative method is also can allow filtrate and ammonia or carbonic acid gas react, to be settled out sodium bicarbonate.In strainer 82, solution is filtered then, leach sodium bicarbonate.Then with these sodium bicarbonates with wash from the sodium bicarbonate of strainer 30, centrifuge dehydration and drying.These operations do not show in figure.
The component of the filtrate that stays is approximately by weight: 10% sodium sulfate, 24% ammonium sulfate and 8% sodium bicarbonate.The proportion of this solution under 40 ℃ is 1.285.
From then on section beginning is cooled to about O ℃ with filtrate solution in water cooler 84, contain so that filtrate component is by weight changed into approximately: 5% sodium sulfate, 28% ammonium sulfate and 6% sodium bicarbonate.Filter this solution with strainer 86, the sodium bicarbonate and the sodium sulfate that are settled out are recovered, and send supercarbonate crystallizer tank 32 back to, and filtrate is then reacted with Repone K in groove 88, the vitriolate of tartar of synthetic fs, the purity range of these vitriolate of tartar is approximately 75% to 90%.Solid sulphuric acid potassium then in groove 94, is used from the Repone K bittern of groove 92 and is changed slurry once more.Its product is exactly high quality, high level vitriolate of tartar.This product carries out repeatedly washing in the traditional washing section of round-robin 96 with groove 94 at one.
(Fig. 2 evaporates in a), improves the concentration of the solution of ammonium chloride, so that after cooling, makes the concentration of Repone K and vitriol drop to minimum at vaporizer 98 from the solution of strainer 90.This solution filters with strainer 100, Repone K that is settled out and (x) SO
4(x=K Na), sends into groove 88 and carries out recirculation herein.
Filtrate from strainer 100 contains ammonium chloride, Repone K and vitriolate of tartar, and this filtrate is admitted to vaporizer 102.React with sodium bicarbonate afterwards, discharge ammonia and carbonic acid gas.With suitable technique these gases are washed/handle then.Afterwards, the calcium chloride with output abandons or sells.
Example 2
Do not carry out the supercarbonate precipitation
Feed intake-1 liter; Proportion 1.3
350g/l Na
2SO
4
Fs
Output NaHCO
3
Bittern current after reaction finishes contain:
The Na of 130g
2SO
410.4% Na
2SO
440 ℃
213.8g (NH
4)
2SO
417.1% (NH
4)
2SO
40.95 liter of proportion 1.250 is molten
Liquid
The NaHCO of 100g
38.0% NaHCO
3
The H of 907g
2
O
1359.8
The NaHCO of output 172g
3Solid
Consume: 544gNH
3
142.5gCO
2
Use Na
2SO
4Make solution saturated again, bittern will contain the Na of 150g
2SO
4, this bittern filtered sends into second section NaHCO then
3Crystallizer.
The effusive bittern product of reaction feeds intake
280gNa
2SO
4 35.9gNH
3 130gNa
2SO
4 177gNaHCO
3
213.8g(NH
4)
2SO
4 92.9gCO
2 353g(NH
4)
2SO
4
100gNaHCO
3 100gNaHCO
3
907gH
2
O
907gH
2
O
1490.8g 1490g proportion 1.285
1.15 liters in 1.15 liters of bittern of proportion 1.32
Contain 237% (NH
4)
2SO
4
Then effusive bittern is cooled to O ℃
The component of bittern is: the Na of 5.O%
2SO
4, this means the Na of 60g
2SO
4With Na
2SO
410H
2The sedimentary form of O is precipitated out, and other has the H of 76g
2O separates out.
Therefore: 907-76=831gH
2O
At O ℃ of following proportion is that 1.26 bittern composition is:
70gNaSO
4
353g(NH
4)
2SO
4
100gNaHCO
3
831gH
2
O
Amount to 1354g
About 1 liter of bittern
K
2SO
4
a) 70gN
2SO
4×174＝85.8
142
b)353g(NH
4)
2SO
4×174＝
465.3g
132
Flow out bittern:
| 283gNH 4Cl 21.9％ 57gNaCl 4.8％ |
| 119g(KNaHCO 3) 9.2％ 831g H 2O 1290 |
Evaporate, make NH
4The content of Cl reaches 33.0%
Discharge NH in the vaporizer
3And CO
2, NH
4The salt that Cl forms is KCl but not NaCl.KCl presses
The method identical with example 1 carried out recirculation.
Benchmark: 1 ton Na
2SO
4Feed intake
| Drop into | Product |
| Fs 0.15 ton of NH 30.396 ton CO 32.52 ton H 2O | 0.48 ton NaHCO 3 |
| 0.10 ton of NH of subordinate phase 30.26 ton CO 30.42 ton Na 2SO 4 | 0.49 ton NaHCO 3 |
| Water cooler internal cooling to 0 ℃- | 0.4 ton Na 2SO 410H 2O |
| Bittern in the water cooler | 0.19 ton Na 2SO 45% 0.98 ton of (NH 4) 2SO 426% 0.28 ton of NaHCO 37.4% 2.31 ton of H 2Totally 3.76 tons of O 61.4% |
| The KCl=1.62 ton | 1.8 ton K 2SO 4 |
| Be evaporated to 33% NH 4Cl loop control=0.71 ton H 2The O washing is sent to 1.2 tons of H of vaporizer for=0.5 ton 2O/ Na per ton 2SO 4 | 0.98 ton of NH of bittern solid 40.08 ton of K of 0.08 ton of KCl of 0.28 ton of KCl of Cl 2SO 40.15 0.36 ton 0.19 ton of NaCl of ton is from CO 31.57 tons of H of NaCl 22.97 tons of O |
| It with CaO content 0.61 ton of lime treatment of 85% | 1.01 1.57 tons of H of ton 0.34 ton of NaCl of 0.08 ton of KCl of CaCl2 2O is at 75 to 90 ℃ following 3.0 tons |
Example 3
Carrying out supercarbonate precipitate-does not evaporate ammonium chloride
The solution that feeds intake is from No. 1 input-412g (NH
4)
2SO
4
335gNa
2SO
4
1267gH
2O
2014g; 1.265,1.60 liters of proportions
Be cooled to 0 ℃, the filtering solution of the process that draws is:
(the NH of 412g
4)
2SO
428.7%
The Na of 116g
2SO
48.0%
907gH
2O
The solution of 1435g
Then this bittern is heated to 25 ℃, is added into KCl with output K
2SO
4From K
2SO
4The effusive bittern in loop is composed as follows:
NH
4Cl 330.8g 21.9％
KCl 130g 8.6％
NaCl 94.7 6.3％
x-SO
4 50g 3.3％ x＝Na/K
H
2O 907g 60
1512g
Again this bittern is heated afterwards, itself and lime are reacted, reclaim ammonia, and walk around vaporizer.KCl is sent back to CaCl again
2Bittern, but not in vaporizer, reclaim.This means CaCl
2The K loss 15% to 20% of bittern.Can pass through to CaCl
2/ KCl bittern adds Na
2SO
4Make KaCl
2KCl in the bittern is reduced to 1.0%.In 0 to 100 ℃ scope, all can pass through syngenite (CaSO
4K
2SO
4XH
2O) coprecipitation mode is effectively collected potassium, but optimum temperature is 20 to 30 ℃, SO under this temperature
4The solubleness minimum, chemical reaction also reasonably speed carry out.
KaCl
2The composition of bittern:
343.3g KaCl
222.5%
The KCl 8.0% of 130g
94.7gNaCl 6.3％
50gxSO
4 32％(Na/K)
907g'sH
2O
59.5%
1525g 100％
Be added into 140gNa
2SO
4The back:
The filter cake that the bittern that comes out comes out
234.8g CaCl
217.8%
15.25g KCl 1.1% 310gCaSO
4K
2SO
4
NaCl 15.9%+100gH of 209g
2O
50gxSO
4 3.8％
807 61.3％
More than the bittern of Pai Chuing can be handled with deep well method.Filter cake can be used as tackiness agent and mixes K
2SO
4Product is perhaps further handled, and removes CaSO
4
Filter cake can with from NaHCO
3(the NH that processing feeds intake
4)
2HCO
3React CaSO wherein
4To react very soon, generate (NH)
2SO
4And K
2SO
4Bittern, and the CaCl that can filter out
3Precipitation, this throw out can abandon.With (NH)
2SO
4/ K
2SO
4Bittern is sent into first section K
2SO
4Crystallizer carries out recirculation.
Claims (15)
1, the compound method of a kind of food grade sodium bicarbonate and vitriolate of tartar comprises the following steps:
A) provide the source of fluid sulphuric acid sodium;
B) be provided for being settled out the source of the bicarbonate of ammonia of sodium bicarbonate;
C) above-mentioned sodium sulfate is contacted with above-mentioned bicarbonate of ammonia;
D) be settled out sodium bicarbonate and form a kind of solution;
E) filter out above-mentioned sodium bicarbonate and obtain containing the solution of sodium sulfate;
F) make from the solution of step e) saturated with sodium sulfate;
G) above-mentioned solution is contacted with bicarbonate of ammonia, ammonia or carbonic acid gas, be settled out more sodium bicarbonate;
H) sodium bicarbonate that is settled out filtration step g);
I) will be from step e) and h) sodium bicarbonate combine, wash, become the sodium bicarbonate of food grade; And
J) will be from step I) solution be cooled to 0 ℃, guarantee to form the saltcake precipitation;
K) with sulfuric acid to from step j) solution handle, the carbonate inorganics is changed into the vitriol inorganics and discharges carbon dioxide;
L) will be from step k) solution be heated between 30 ℃ to 40 ℃;
M) will be from step l) solution contact with Repone K, be settled out vitriolate of tartar.
2, the compound method of sodium bicarbonate according to claim 1 and vitriolate of tartar is characterized in that comprising that the vitriolate of tartar with being settled out separates, and the step of washing with Klorvess Liquid.
3,, it is characterized in that comprising with lime to handling, to discharge the step of ammonia from the solution of above-mentioned vitriolate of tartar separating step according to the compound method of sodium bicarbonate described in the claim 2 and vitriolate of tartar.
4, the compound method of sodium bicarbonate according to claim 3 and vitriolate of tartar is characterized in that comprising that the ammonia with above-mentioned reclaims, and sends into the step of step g).
5, the compound method of sodium bicarbonate according to claim 4 and vitriolate of tartar is characterized in that comprising to carry out the step of evaporation process from the described filtered liquid of claim 4.
6, the compound method of sodium bicarbonate according to claim 1 and vitriolate of tartar is characterized in that described sodium sulfate is between 1.30 to 1.34 at the proportion under 40 ℃.
7, the compound method of sodium bicarbonate according to claim 1 and vitriolate of tartar is characterized in that the solution proportion from step d) is 1.25, and this solution consisting of by weight:
10.4% sodium sulfate, 17.1% ammonium sulfate, 8% to 12% sodium bicarbonate and the bicarbonate of ammonia of excess.
8, the compound method of sodium bicarbonate according to claim 1 and vitriolate of tartar is characterized in that described sodium sulfate from step e) contains Na
2SO
410H
2O.
9, the compound method of sodium bicarbonate according to claim 1 and vitriolate of tartar is characterized in that the described proportion of solution under 40 ℃ from step f) is 1.285.
10, the compound method of sodium bicarbonate according to claim 1 and vitriolate of tartar is characterized in that described from step j) solution be the saturated solution of a kind of sodium sulfate, ammonium sulfate and sodium bicarbonate.
11,, it is characterized in that described vitriolate of tartar quantum of output is at least 80%, purity at least 98% according to the compound method of sodium bicarbonate described in the claim 1 and vitriolate of tartar.
12, the compound method of a kind of food grade sodium bicarbonate and vitriolate of tartar comprises the following steps:
A) provide the source of fluid sulphuric acid sodium;
B) provide the source of bicarbonate of ammonia;
C) above-mentioned sodium sulfate is contacted with above-mentioned bicarbonate of ammonia;
D) be settled out sodium bicarbonate and form a kind of solution;
This liquid that e) will form in step d) contacts with sodium sulfate, is settled out sodium bicarbonate and forms a kind of solution;
F) make the solution that in step e), forms saturated with sodium sulfate;
G) filter out solid in the solution of step f);
H) solution from step f) is contacted with sulfonic acid, to be settled out carbonate;
I) will be from step h) solution be cooled to 0 ℃, form the saltcake precipitation;
J) will be from step I) solution be heated to 30 ℃ to 40 ℃; And
K) with Repone K to from step j) solution handle, to be settled out vitriolate of tartar;
L) to from step k) solution carry out evaporation process, recover the content value of potassium, and loop back step k again); And
M) dry above-mentioned vitriolate of tartar.
13,, it is characterized in that comprising with lime and ammonium chloride to from step l according to the compound method of sodium bicarbonate described in the claim 12 and vitriolate of tartar) the step handled of surplus solution.
14,, it is characterized in that discharging ammonia, and these ammonias are recycled according to the compound method of sodium bicarbonate described in the claim 13 and vitriolate of tartar.
15, the compound method of sodium bicarbonate according to claim 12 and vitriolate of tartar is characterized in that used Klorvess Liquid is sent into step k), carry out recirculation.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US10396998P | 1998-10-13 | 1998-10-13 | |
| US60/103,969 | 1998-10-13 |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA021462313A Division CN1515491A (en) | 1998-10-13 | 1999-09-30 | Process for preparing alkali metal salt |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1330612A CN1330612A (en) | 2002-01-09 |
| CN1156397C true CN1156397C (en) | 2004-07-07 |
Family
ID=22297990
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA021462313A Pending CN1515491A (en) | 1998-10-13 | 1999-09-30 | Process for preparing alkali metal salt |
| CNB998143782A Expired - Fee Related CN1156397C (en) | 1998-10-13 | 1999-09-30 | Method of formulating alkali metal salts |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA021462313A Pending CN1515491A (en) | 1998-10-13 | 1999-09-30 | Process for preparing alkali metal salt |
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| Country | Link |
|---|---|
| EP (1) | EP1121327A1 (en) |
| JP (1) | JP2002527330A (en) |
| KR (1) | KR20010088870A (en) |
| CN (2) | CN1515491A (en) |
| AU (1) | AU751236B2 (en) |
| BR (1) | BR9914543A (en) |
| CA (1) | CA2284967A1 (en) |
| CZ (1) | CZ20011176A3 (en) |
| EA (1) | EA002709B1 (en) |
| HR (1) | HRP20000125A2 (en) |
| HU (1) | HUP0104062A3 (en) |
| ID (1) | ID28729A (en) |
| NO (1) | NO20011851L (en) |
| NZ (1) | NZ510786A (en) |
| PL (1) | PL347098A1 (en) |
| SI (1) | SI20636A (en) |
| SK (1) | SK5002001A3 (en) |
| TR (1) | TR200100960T2 (en) |
| UA (1) | UA73096C2 (en) |
| WO (1) | WO2000021887A1 (en) |
| YU (1) | YU27101A (en) |
| ZA (1) | ZA200001142B (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6365122B1 (en) * | 1998-06-22 | 2002-04-02 | William J. Rigby | Process for manufacturing potassium sulfate fertilizer and other metal sulfates |
| US6475458B1 (en) | 1999-10-25 | 2002-11-05 | Airborne Industrial Minerals Inc. | Method for formulating food grade sodium bicarbonate |
| JP4812253B2 (en) * | 2001-08-29 | 2011-11-09 | リグビィ、ウィリアム、ジェイ． | Method for producing potassium sulfate fertilizer and other metal sulfates |
| US7393378B2 (en) * | 2003-02-11 | 2008-07-01 | Airborne Industrial Minerals Inc. | Method for recovering purified sodium bicarbonate and ammonium sulfate |
| JP5404180B2 (en) * | 2009-05-22 | 2014-01-29 | 日立造船株式会社 | Sodium extraction device |
| CN102503636A (en) * | 2011-10-27 | 2012-06-20 | 山西师范大学 | Ammonium chloride agglomerating prilling method |
| FR3007753A1 (en) * | 2013-06-26 | 2015-01-02 | Solvay | PROCESS FOR THE PREPARATION OF ALKALI METAL BICARBONATE PARTICLES |
| CN104556154B (en) * | 2014-12-30 | 2017-04-12 | 东莞市英硫净水服务有限公司 | Comprehensive utilization technology of residual liquid after evaporation of heavy salt water |
| CN109052434B (en) * | 2018-10-19 | 2021-06-04 | 四川金象赛瑞化工股份有限公司 | Method for jointly producing soda ash and composite nitrogen fertilizer by taking mirabilite and ammonium bicarbonate as raw materials |
| CN111895722B (en) * | 2020-09-04 | 2024-03-01 | 江西智联塑化科技有限公司 | Conduction oil cooling device for pentaerythritol stearate preparation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CA2032627C (en) * | 1990-12-18 | 1997-01-14 | Jack S. Thompson | Process for producing sodium carbonate and ammonium sulphate from sodium sulphate |
| CN1044222C (en) * | 1991-12-28 | 1999-07-21 | 邓绍齐 | Comprehensive utilization method of chromium-containing sodium sulfate |
| CN1089235A (en) * | 1993-12-29 | 1994-07-13 | 张祥林 | The method of the single-phase decomposition system sodium bicarbonate of sodium sulfate and bicarbonate of ammonia |
| CN1041401C (en) * | 1994-11-01 | 1998-12-30 | 何永汉 | Method for production of Lemery salt |
| SK279011B6 (en) * | 1995-04-05 | 1998-05-06 | Považské Chemické Závody | Method for conversion of ammonium sulphate to potassium sulphate |
| US5830422A (en) * | 1995-06-23 | 1998-11-03 | Ormiston Mining And Smelting Co. Ltd. | Method for production of sodium bicarbonate, sodium carbonate and ammonium sulfate from sodium sulfate |
-
1999
- 1999-09-29 CA CA002284967A patent/CA2284967A1/en not_active Abandoned
- 1999-09-30 UA UA2001042328A patent/UA73096C2/en unknown
- 1999-09-30 AU AU58457/99A patent/AU751236B2/en not_active Ceased
- 1999-09-30 CN CNA021462313A patent/CN1515491A/en active Pending
- 1999-09-30 EA EA200100340A patent/EA002709B1/en not_active IP Right Cessation
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- 1999-09-30 JP JP2000575800A patent/JP2002527330A/en active Pending
- 1999-09-30 HU HU0104062A patent/HUP0104062A3/en unknown
- 1999-09-30 SK SK500-2001A patent/SK5002001A3/en unknown
- 1999-09-30 TR TR2001/00960T patent/TR200100960T2/en unknown
- 1999-09-30 BR BR9914543-0A patent/BR9914543A/en not_active Application Discontinuation
- 1999-09-30 CZ CZ20011176A patent/CZ20011176A3/en unknown
- 1999-09-30 CN CNB998143782A patent/CN1156397C/en not_active Expired - Fee Related
- 1999-09-30 ID IDW00200101051A patent/ID28729A/en unknown
- 1999-09-30 KR KR1020017004656A patent/KR20010088870A/en not_active Application Discontinuation
- 1999-09-30 WO PCT/CA1999/000905 patent/WO2000021887A1/en not_active Application Discontinuation
- 1999-09-30 EP EP99945817A patent/EP1121327A1/en not_active Withdrawn
- 1999-09-30 NZ NZ510786A patent/NZ510786A/en unknown
- 1999-09-30 YU YU27101A patent/YU27101A/en unknown
-
2000
- 2000-03-07 HR HR20000125A patent/HRP20000125A2/en not_active Application Discontinuation
- 2000-03-07 ZA ZA200001142A patent/ZA200001142B/en unknown
-
2001
- 2001-04-10 NO NO20011851A patent/NO20011851L/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| JP2002527330A (en) | 2002-08-27 |
| KR20010088870A (en) | 2001-09-28 |
| PL347098A1 (en) | 2002-03-25 |
| ID28729A (en) | 2001-06-28 |
| HUP0104062A3 (en) | 2003-03-28 |
| SK5002001A3 (en) | 2001-10-08 |
| AU751236B2 (en) | 2002-08-08 |
| CZ20011176A3 (en) | 2001-09-12 |
| HRP20000125A2 (en) | 2001-02-28 |
| CN1515491A (en) | 2004-07-28 |
| TR200100960T2 (en) | 2001-08-21 |
| NO20011851L (en) | 2001-06-12 |
| NO20011851D0 (en) | 2001-04-10 |
| YU27101A (en) | 2003-10-31 |
| HUP0104062A2 (en) | 2002-04-29 |
| EA002709B1 (en) | 2002-08-29 |
| NZ510786A (en) | 2002-05-31 |
| EA200100340A1 (en) | 2001-10-22 |
| ZA200001142B (en) | 2000-10-23 |
| EP1121327A1 (en) | 2001-08-08 |
| CA2284967A1 (en) | 2000-04-13 |
| CN1330612A (en) | 2002-01-09 |
| BR9914543A (en) | 2001-06-26 |
| SI20636A (en) | 2002-02-28 |
| AU5845799A (en) | 2000-05-01 |
| UA73096C2 (en) | 2005-06-15 |
| WO2000021887A1 (en) | 2000-04-20 |
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