US2012061A - Process for the preparation of monochromates and dichromates - Google Patents
Process for the preparation of monochromates and dichromates Download PDFInfo
- Publication number
- US2012061A US2012061A US672904A US67290433A US2012061A US 2012061 A US2012061 A US 2012061A US 672904 A US672904 A US 672904A US 67290433 A US67290433 A US 67290433A US 2012061 A US2012061 A US 2012061A
- Authority
- US
- United States
- Prior art keywords
- parts
- oxidizing
- monochromates
- reaction
- under
- 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 - Lifetime
Links
- 238000000034 method Methods 0.000 title description 11
- 238000002360 preparation method Methods 0.000 title description 2
- 239000000126 substance Substances 0.000 description 21
- 238000006243 chemical reaction Methods 0.000 description 20
- 230000001590 oxidative effect Effects 0.000 description 20
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 17
- 229910000423 chromium oxide Inorganic materials 0.000 description 17
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 16
- 150000001768 cations Chemical class 0.000 description 13
- 229910052804 chromium Inorganic materials 0.000 description 13
- 239000011651 chromium Substances 0.000 description 13
- 239000003795 chemical substances by application Substances 0.000 description 12
- 238000000354 decomposition reaction Methods 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 11
- 239000002585 base Substances 0.000 description 11
- 239000001301 oxygen Substances 0.000 description 11
- 229910052760 oxygen Inorganic materials 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 8
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 8
- 239000012736 aqueous medium Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000000243 solution Substances 0.000 description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 5
- 239000001488 sodium phosphate Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 150000001450 anions Chemical class 0.000 description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 description 4
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 4
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 4
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 4
- 239000007800 oxidant agent Substances 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 3
- 150000004679 hydroxides Chemical class 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- KIEOKOFEPABQKJ-UHFFFAOYSA-N sodium dichromate Chemical compound [Na+].[Na+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KIEOKOFEPABQKJ-UHFFFAOYSA-N 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical class OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 2
- 239000001175 calcium sulphate Substances 0.000 description 2
- 235000011132 calcium sulphate Nutrition 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 2
- 229910000397 disodium phosphate Inorganic materials 0.000 description 2
- 235000019800 disodium phosphate Nutrition 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 2
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 2
- 235000019801 trisodium phosphate Nutrition 0.000 description 2
- QLOKJRIVRGCVIM-UHFFFAOYSA-N 1-[(4-methylsulfanylphenyl)methyl]piperazine Chemical compound C1=CC(SC)=CC=C1CN1CCNCC1 QLOKJRIVRGCVIM-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 241000861718 Chloris <Aves> Species 0.000 description 1
- 241001600451 Chromis Species 0.000 description 1
- 241001649081 Dina Species 0.000 description 1
- 229910000604 Ferrochrome Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- ZEASXVYVFFXULL-UHFFFAOYSA-N amezinium metilsulfate Chemical compound COS([O-])(=O)=O.COC1=CC(N)=CN=[N+]1C1=CC=CC=C1 ZEASXVYVFFXULL-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- VQWFNAGFNGABOH-UHFFFAOYSA-K chromium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Cr+3] VQWFNAGFNGABOH-UHFFFAOYSA-K 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
- 235000019799 monosodium phosphate Nutrition 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- SOBHUZYZLFQYFK-UHFFFAOYSA-K trisodium;hydroxy-[[phosphonatomethyl(phosphonomethyl)amino]methyl]phosphinate Chemical compound [Na+].[Na+].[Na+].OP(O)(=O)CN(CP(O)([O-])=O)CP([O-])([O-])=O SOBHUZYZLFQYFK-UHFFFAOYSA-K 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G37/00—Compounds of chromium
- C01G37/14—Chromates; Bichromates
Definitions
- alkaline-' or alkaline earth hydroxides carbonates or .bicarbonates or monochromate's'in an aqueous medium, the quantity of alkaline agent employed being such that it remains below that required for the formationfof monochromates.
- a solution of an acid contains :hydrogenions (cationsland non-metallic ions (anions) -j.a solution of" a base contains hydr'oxyl ions (anions) and metallic 'ions (cations); and a solution ofa alt "contains nonrmeta-llic (anions) andfmetallic an acid thefanions are the active elements which combine witlrthe attacked metal, forming chlorides, sulphates, phosphates, nitrates, etc.-,'
- the yield is 22.16%.
- the concentration of the sulphuric acid in the solution is about 0.5%. It may be remarked that the reaction does not progress beyond a decomposition corresponding to about 0.5% H2504.
- the yield of bichromate is 93.3%. l If instead of trisodium phosphate an equiva lent quantity of disodium phosphate is employed The yield can be considerably increased by a further dilution in order to the same time as oxidizing agents and when de- 1 composed as alkaline agents.
- the product obtained is a solution of bichromate'with a residue of silicic acid. .
- the yield is .'95.3,% of sodium bichromate.
- the product of the reaction is composed of a liquorcontainingsodium nionochromate and disodium phosphate; yield 90-95%.
- the productof the reaction is filtered from a small quantity of magnesia andchromium substance which are not attacked.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
CE? PROCESS ron THE PREPARATloN F t MONOOHBOMATES A D: DVICHROMATVES I. :meSEmisnai-a, c sarmaamnce, as l signer to Bd'zel-Maletra,SocitIndustrielle de 7 a I a i I Produits Chimiques, Paris, l lrance a c j z ai tion of France a 1, in; Drawing. ,xppisafioiiivia'y; "25, 1933, Serial No. 72,904. 'In France MayZG, 1932 *8 Claims. (ems-c) I The present invention relates tothe manufacture of monochromates and dichromates.
In my prior Patent No. 1,955,326, dated April 1-7, 1934,,1 have described and claimed a process for manufacturing, monochromates anddichromates with oxidizing ferro-chrome or a substance containing metallic chromium, as starting ma 'terials, in the presence of waterand an alkaline agent by means of an oxidizing gas underpressure; lhave already proposed to prepare monochromates by subjecting at temperatures above 100 C., chromium hydroxide, hydrated chromium oxide, chromium oxide or chrome ore, or substances containing .the same, to an oxidizing decomposition in the presence of alkaline: or alkaby subjecting at temperatures above 100'C.;chromium hydroxide, hydrated chromium oxide, chro- V mium oxide orsubstancescontaining the same or chrome ore, to an. oxidizing decomposition inthe presence of alkaline-' or alkaline earth hydroxides, carbonates or .bicarbonates or monochromate's'in an aqueous medium, the quantity of alkaline agent employed being such that it remains below that required for the formationfof monochromates.
In accordancewith'the present invention-ithas been 'found that for .thev formation of nionochromates orrdichromates, theipresence of alkalineor alkalineearth hydroxides, carbonates or bicarbonates or of monochromates is not abso'r lutely necessary. rAccording'to the invention it is possible to employlin'stead of ortogether with these alkalineor alkaline earth agents and in the case of the'preparation of dichromates instead ofor together with alkaline-or alkaline earth agents or monochromates, in general all compoundscapable of yielding their alkaline prin-.'
ciple underioxidizing conditions in the course of the process. 1
an oxygen-yielding? reagenttlike, potassium "chlorate; U
The tendency ofchromium, to be converted into hexavalent chromium-is so markedithat-inthe course of the'oxidation-fprocess the'substance's added undergo a splitting-'-up :which; causes them ions (cations) .fjf-
um. ,a qor'dina to, the quantity of the alkaline xprinciple entering into reaction it isfpossible to to igiveupjtheir alkalineprinciple tothe chromi In ordento 'proper1y;. distinguish between an .falkaline agent?.per seand a substance which in this- .case' underproper oxidizing conditions will it is well to remember that:
A solution of an acid contains :hydrogenions (cationsland non-metallic ions (anions) -j.a solution of" a base contains hydr'oxyl ions (anions) and metallic 'ions (cations); and a solution ofa alt "contains nonrmeta-llic (anions) andfmetallic an acid thefanions are the active elements which combine witlrthe attacked metal, forming chlorides, sulphates, phosphates, nitrates, etc.-,'
freeing" the hydrogen. In a base or alkaline ,agentiit is the cation'which isthe active 'element, while-in aisalt solution the anions and cations bind and'neutrali'ze each Otheryas long as no decomposition"takesplacei Onlywhn and after such decomposition is efiected under' special circumstances, free acting cations are liberated and a: chemical reaction isrealized. Thus a substance which" normally cannot be classified as base, can become an alkalineagent'.
While an'alka'line agent contains its-cation in afiree state," the substances employed according toj the present' inventionsare those capable of liberatingth'eirjcations generally under the oxiidi'zing 'actioncf the reaction. V Ido not claim as lily-present invention the use of .oxides, hydroxides of: alkali or alkali earth metals" taken alone. Nor do Iclaim the use of carbonates of alkalior alkaliearth metals taken alone. Neither do I claim as'qa part of my'presentinvention the use of monochromates per se as "a substance capable of giving up free 'a'ctingications to the substance containing chromium oxide under the influence a of the Ioxidizing reaction.
As compounds which in themselves are not bases, but in s the presence of an -'oxidizing reac- "tionare capable of, giving up their alkaline principle to jthechromium it is possible to em'ploy "the most varied saltsof strong or weakinorganic F or organic acids oralsooxygen"containingicompounds of a salt like character for example alkalineor alkaline earth sulphates, 'chlori'des,"'ph'osphatsac'etates, monochromates, silicates, aluminates, nitrates, chlorates, per-salts, manganates,
permanganates' and; thei -like. It may be rej marked that these latter 'compoundsjcan act at If for example organic derivatives are employed the organic principle is ingeneraloxidized to carbon dioxide which can conveniently be elimi-' 1 nated during the operation. Certain compounds capable of giving up their alkaline principle can be used alone, while in the case of certain others it is to be recommended that they should be used in conjunction with substances acting as neutralizing agents as for example the oxides or carbon ates of the alkaline earths. By way of example which is in no way limiting of the present process the following examples are given and it may be remarked that Example 1 illustrates the splitting upof sodium sulphate under-the action of the oxidizing decomposition of trivalent chromium. r I I As a matterof fact, the salts-just indicated above are not basesbut are capable of giving up their cations under the action of the oxidizing reaction. Said characteristic is clearly exemplified by the following Examples 1, 2, 7, and 8.
Examples (1) 9.38 parts of'hydrated chromium oxide (containing 81% of CrzO3),--7.1,partsof anhydrous sodium sulphate and 200 parts of water are heated to 280-290 C. for 6 hoursin a stirring autoclave. Before commencing the heating of the apparatus it is filled with oxygen under 15 atmospheres. I
By removing the contents of the'apparatus it is found that a large part of the hydrated chromium oxide is converted into sodium bichromate together with free mineral acid.
The yield is 22.16%. The concentration of the sulphuric acid in the solution is about 0.5%. It may be remarked that the reaction does not progress beyond a decomposition corresponding to about 0.5% H2504.
avoid exceeding this limiting acidity.
( 9.38 parts of hydrated chromium, oxide (containing 81% of Cr203), 7.1 parts of sodium sulphate, 5 parts of calcium carbonate and 200 parts of water are heated to 280290 C. for about 10-15 hours in the presence of oxygen under 15 atmospheres in a stirring autoclave.
After cooling a bichromate liquoris withdrawn from the apparatus leaving a residue consisting for the mostipart of calcium sulphate.
The yield is -97% bichromate.
(3) 9.38 parts of hydrated chromium ox ide (containing 81% of CrzOs), 17.42partsofcrystallized trisodium phosphate (10"mo1ecules .of water) and 225 parts of-waterare heated to 280-290 C. for about 9 hours in thepresence of oxygen under 15 atmospheres in a stirringautoclave. i r r Sodium bichromate and mono-sodium phosphate are formed according to the reaction;
V Na2C r20'I+NaI I2PO4.
The yield of bichromate is 93.3%. l If instead of trisodium phosphate an equiva lent quantity of disodium phosphate is employed The yield can be considerably increased by a further dilution in order to the same time as oxidizing agents and when de- 1 composed as alkaline agents.
the oxidation likewise takes place with good yield.
(4) 9.38 parts of hydrated chromium oxide (containing 81% of CrzOz) 11.73 parts of sodium silicate (containing 34.1% or sodium hydroxide) and 225 parts of water are-heated to 280-290 C. for about 9 hours under 15 atmospheres of oxygen ina stirring autoclave.
The product obtained is a solution of bichromate'with a residue of silicic acid. .The yield is .'95.3,% of sodium bichromate.
(5 9.38. parts of hydrated chromium oxide i (containing 81% of CI'zOs), 10.11 parts of potassium nitrate, 5 parts of calcium carbonate and 225 parts ofwater are heated to 280-290 C. for about10-15 hours under 15 atmospheres of oxygen in a stirring autoclave.
The product obtained is potassium bichromate together with calcium nitrate. The yield'of hexavalent chromium is 90%. V v a (6) 9.38 parts of hydrated chromium oxide (containing 81%of Cr2O3), 12.25 parts of potassium chlorate, 5 parts of calcium carbonate and 200 parts of water are-heated at 280-290" C. for about 10-15 hours and'without the presence of oxygen in a stirring autoclave. The reaction is as follows: 1
After cooling there is found in the apparatus free oxygen under pressure. The yield of bi- 'chromate is about8890%.
If double the quantity of hydrated chromium oxide-and an equivalent quantity of alkali are employed the oxygen formed will serve for the conversion of this additional quantity of hydrated chromium oxide according to the reaction 7) 9.38 parts of hydrated-chromium oxide conthan that of the vapour tension.
Whenthe reaction is complete the residue of calcium sulphate is filtered and the monochromate-is separated by known means. The yield is practicallyquantitative; Instead of calcium car- "bonate it is likewise possible:v toemploy caustic lime. I
(8) 7.6 parts of chromimn oxide 90-95%.(11'203, 14.5 parts of anhydrous sodium sulphate, 10 parts of calcium carbonate, 200 parts of water, are heated for about 15 hours with good agitation in an autoclave to BOO-350 C. A current of oxygen or.v air under pressure is caused to pass through. The progress of the reaction can be followed by the content of carbonic acid of the gas escaping from the apparatus.
At the end of the reaction residual calcium sulphateis filtered and the monochromateobtained in anexcellent yield is separated by any known *means." vJ
(9) 9.38 parts of hydrated chromium oxide,
81% C12O3,'-'7O parts'of trisodium phoshate 10 Aq., 225 parts of water are heated in an atmosphere of oxygen or in a current of air under. pressure for 10-15 hours at -300? C. V
The product of the reaction is composed of a liquorcontainingsodium nionochromate and disodium phosphate; yield 90-95%.
' reaction.
. under pressure and in an aqueous medium, in the presence of a substance beingnot normally classified as base, but other than a monochromateand (10) 9.5 parts of hydrated chromium oxide of CrzOs, 24.5 parts of potassium chlorate, 4.19 parts of magnesium oxide of 96.3% MgO, 200 parts of water are heated for 10-15 hours at 290-300 C.
At the end of thereaction free oxygen under pressure is present in the apparatus.
The productof the reaction is filtered from a small quantity of magnesia andchromium substance which are not attacked.
The potassium chromate obtained is separated by crystallization. I v
Oxidation yield 80-90%.
I claim:
1. Process for the manufacture of monochromates or dichromates consisting in subjecting a substance containing chromium oxide to oxidizing decomposition at temperatures above C. un-
der pressure and in an aqueous medium, in the presence of a substance being not normally classiffied as base,.but other than a monochromate and capable of giving up free acting cations to the chromium under the influence ofthe oxidizing 2.;Processfor the manufacture of monochromates or dichromates consisting in subjecting a substance containing chromium oxide to oxidizing decomposition at temperatures above 100C. un-
.der pressure and in an aqueous medium, in the a presence of a substance being not normally classified as base, but other than a monochromate and capable of giving up free acting cations tothe chromium under the influence of the oxidizing re action and in the presence of an alkaline agent.
3. Process for the manufacture of monochromates or dichromates consisting in subjecting a substance containing chromium oxide to oxidizing decomposition at temperatures above 100 C. un-.;
der pressure and in an aqueous medium, inthe presence of a substance being not normally classified as base, but other than a monochromate and capable of giving up free acting cations to the chromium under the influence of the oxidizing re action, andacting at the same time as oxidizing agent.
4. Process for the manufacture of monochro I mates or dichromates consisting in subjecting a substance containing chromium oxide to oxidizing decomposition at temperatures above 100 C.
capable of giving upfree acting cations to the chromium under the influence of the oxidizing reaction and acting at the same time as oxidizing agent, and inthe presence of an alkaline agent.
5. Process for the manufacture of monochromates or dichromatesconsisting in subjecting chrome ore to oxidizing decomposition at temperatures above 100 C. under pressure and in an aqueous medium, in the presence of a substance being not normally classified as base, but other than a monochromateand'oapable of giving up free acting cations tothe chromium under the influence of theoxidizing'reaction. V
6. Process for the manufacture of monochromates and dichromates consisting in subjecting chrome ore to oxidizing decomposition at temperatures above 100 C. under pressure and in an aqueous medium, in the presence of a substance being not normally classified as base, but other than a monochromate'and capable of giving up free acting cations to the chromium under themfluence of the oxidizing reaction, and in the presence of an alkaline agent.
7. Process for the manufacture of monochroperatures above 100 C. under pressure and in an aqueous medium, in the presence of a substance beingnot normally classified as base, but other than a monochromate and capable of givingup 'free'acting cations to the chromium under the in-. I fluence of the oxidizing reaction and acting at the same time as oxidizing agent, and in the presence of an alkaline agent. 7 I
1 JULES. EMILE DEMAN'I'.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR2012061X | 1932-05-26 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2012061A true US2012061A (en) | 1935-08-20 |
Family
ID=9683009
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US672904A Expired - Lifetime US2012061A (en) | 1932-05-26 | 1933-05-25 | Process for the preparation of monochromates and dichromates |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US2012061A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3369861A (en) * | 1964-10-09 | 1968-02-20 | Marathon Oil Co | Method for producing ammonium chromate |
| US3393972A (en) * | 1964-06-09 | 1968-07-23 | Marathon Oil Co | Method for preparing ammonium chromate |
| US3963824A (en) * | 1972-06-14 | 1976-06-15 | Produits Chimiques Ugine Kuhlmann | Process for extracting chromium from chromium ores |
| US9738131B2 (en) | 2015-05-11 | 2017-08-22 | Hendrickson Usa, L.L.C. | Air spring with damping characteristics for heavy-duty vehicles |
-
1933
- 1933-05-25 US US672904A patent/US2012061A/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3393972A (en) * | 1964-06-09 | 1968-07-23 | Marathon Oil Co | Method for preparing ammonium chromate |
| US3369861A (en) * | 1964-10-09 | 1968-02-20 | Marathon Oil Co | Method for producing ammonium chromate |
| US3963824A (en) * | 1972-06-14 | 1976-06-15 | Produits Chimiques Ugine Kuhlmann | Process for extracting chromium from chromium ores |
| US9738131B2 (en) | 2015-05-11 | 2017-08-22 | Hendrickson Usa, L.L.C. | Air spring with damping characteristics for heavy-duty vehicles |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US2376935A (en) | Chlorine dioxide manufacture | |
| US4193970A (en) | Process for the precipitation of iron as jarosite | |
| US2012061A (en) | Process for the preparation of monochromates and dichromates | |
| GB1008676A (en) | Improvements in and relating to the manufacture of titanium dioxide | |
| US1494029A (en) | Process of separating the constituents of mineral silicates | |
| US3034853A (en) | Process for the removal of lower oxides of nitrogen from gaseous mixtures containing them | |
| US2196584A (en) | Manufacture of ferric sulphate | |
| US3343910A (en) | Water-soluble lithium compounds | |
| US2402103A (en) | Production of chromium compounds | |
| US2431075A (en) | Production of chromium hydroxide | |
| US3314747A (en) | Recovery of chromate from chrome mud wastes | |
| US2384010A (en) | Method of producing magnesium sulphate | |
| US3734709A (en) | Process for the production of chlorine, sodium bicarbonate and ammonium-sodium nitrate | |
| US544366A (en) | Process of recovering glycerin from soap-underlye | |
| US1536619A (en) | Process for the recovery of zinc compounds from zinc-chloride solutions | |
| US2012062A (en) | Process for the preparation of monochromates and dichromates | |
| CA1093277A (en) | Process of producing aqueous solution of magnesium chloride | |
| US1797655A (en) | Process for the production of aluminum oxide or products containing aluminum oxide out of material containing aluminum sulphide | |
| US234595A (en) | Juan f | |
| US2013334A (en) | Method of producing magnesium chloride from calcium chloride | |
| GB748610A (en) | Improvements in or relating to a method for treating alkali metal chromates | |
| US2921838A (en) | Process of preparing chromic oxide | |
| US1978403A (en) | Process of separating calcium and magnesium chlorides | |
| US1300417A (en) | Process of preparing alumina. | |
| US1529435A (en) | Process for the production of soluble barium salts |