PL77840B2 - - Google Patents
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- Publication number
- PL77840B2 PL77840B2 PL15577572A PL15577572A PL77840B2 PL 77840 B2 PL77840 B2 PL 77840B2 PL 15577572 A PL15577572 A PL 15577572A PL 15577572 A PL15577572 A PL 15577572A PL 77840 B2 PL77840 B2 PL 77840B2
- Authority
- PL
- Poland
- Prior art keywords
- exceed
- lead
- content
- oxygen
- water
- Prior art date
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- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims description 5
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 235000005985 organic acids Nutrition 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000008187 granular material Substances 0.000 claims 1
- 238000000034 method Methods 0.000 claims 1
- 235000006408 oxalic acid Nutrition 0.000 claims 1
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- AYPZCTCULRIASE-ZVGUSBNCSA-L [Pb+2].C([C@H](O)[C@@H](O)C(=O)[O-])(=O)[O-] Chemical group [Pb+2].C([C@H](O)[C@@H](O)C(=O)[O-])(=O)[O-] AYPZCTCULRIASE-ZVGUSBNCSA-L 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- MVWDJLOUEUAWIE-UHFFFAOYSA-N O=C=O.O=C=O Chemical compound O=C=O.O=C=O MVWDJLOUEUAWIE-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- -1 for example Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 235000015243 ice cream Nutrition 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
Description
W tej temperaturze utrzymuje sie piec przez okolo 15 minut, po czym wlacza sie ogrzewanie pieca i zwieksza sie przeplyw C02. Gdy temperatura spadnie do okolo 300°C otwiera sie piec i stopniowo, bardzo powoli przesuwa sie lódke grafitowa w kierunku wylotu. Zbyt szybkie przesuwanie lódki moze spowodowac zniszczenie pieca.Material ceramiczny, z którego wykonana jest rura nie wytrzymuje duzych róznic temperatur. Ponowny cykl rozkladu szczawianu olowiu mozna powtórzyc nie czekajac na calkowite wystygniecie pieca. Ziarna grafitu, które przyczepily sie do powierzchni metalicznego olowiu, usuwa sie pocierajac o siebie prety olowiane. W celu usuniecia powierzchniowych zanieczyszczen, prety olowiane trawi sie najpierw w rozcienczonym roztworze HN03 w stosunku 1 objetosc stezonego HN03 i 5 objetosci H20 w temperaturze okolo 60°C przez 30 minut, a nastepnie kolejno plucze sie woda jonitowa, alkoholem metylowym i chloroformem. Te ostatnie oczyszcza sie przez destylacje w aparaturze szklanej.Podobne wyniki uzyskuje sie przy zastosowaniu soli innych kwasów organicznych, jak np. kwas winowy.W wyniku termicznego rozkladu winianu olowiu otrzymuje sie metaliczny olów z domieszka drobno sproszko¬ wanego wegla. Dodatek niewielkiej ilosci winianu olowiu nie przekraczajacej 10% w szczawianie olowiu, zmniejsza korozje lódek grafitowych.Granulowanie olowiu przeprowadza sie w specjalnym piecu wykonanym z grafitu. Stopiony olów wlewa sie powoli do chloroformu, który zostal oczyszczony na drodze destylacji. Co pewien czas po wlaniu okolo 20 kg metalicznego olowiu, chloroform destyluje sie. W celu usuniecia resztek chloroformu olów suszy sie w temperaturze pokojowej.Przy zastosowaniu spektrochemicznej i spektrofotometrycznyeh metod kontroli analitycznej stwierdzono, ze w otrzymanym preparacie: zawartosc arsenu zawartosc bizmutu zawartosc chromu zawartosc cynku zawartosc glinu zawartosc kadmu zawartosc magnezu nie przekracza 2.10~5% nie przekracza 5.10~6% nie przekracza 5.10~6% nie przekracza 1.10_5% nie przekracza 5.10~5% nie przekracza 1.10~5% nie przekracza 5.10~5% zawartosc manganu nie przekracza 1.10_5% zawartosc miedzi nie przekracza 2.10_6% nie przekracza 5.10~6% nie przekracza 2.10-6% nie przekracza 5.10_5% nie przekracza 3.10_5% nie przekracza 5.10~5% zawartosc riiklu zawartosc srebra zawartosc talu zawartosc wapnia zawartosc zelaza PL PLThe stove is kept at this temperature for about 15 minutes, then the stove is heated and the CO 2 flow is increased. When the temperature drops to around 300 ° C, the furnace opens and the graphite ice cream is gradually moved very slowly towards the outlet. Moving the ice tray too quickly can damage the stove. The ceramic material of the pipe does not withstand high temperature fluctuations. The lead oxalate decomposition cycle can be repeated without waiting for the furnace to cool completely. The graphite grains that adhere to the metallic lead surface are removed by rubbing the lead rods together. In order to remove surface contamination, lead rods are first digested in a dilute HNO3 solution in the ratio of 1 volume of concentrated HNO 3 and 5 volumes of H 2 O at a temperature of about 60 ° C for 30 minutes, and then successively rinsed with ion exchange water, methyl alcohol and chloroform. The latter are purified by distillation in a glass apparatus. Similar results are obtained with the use of salts of other organic acids, such as, for example, tartaric acid. As a result of thermal decomposition of lead tartrate, metallic lead is obtained in admixture with finely powdered carbon. The addition of a small amount of lead tartrate, not exceeding 10%, in lead oxalation reduces corrosion of graphite ice cubes. Lead granulation is performed in a special furnace made of graphite. The molten lead is poured slowly into the chloroform, which has been purified by distillation. Every now and then, after pouring about 20 kg of metallic lead, the chloroform is distilled. In order to remove residual chloroform, the leads are dried at room temperature. Using the spectrochemical and spectrophotometric methods of analytical control, it was found that the preparation obtained: arsenic content bismuth content chromium content zinc content aluminum content cadmium content does not exceed 2.10 ~ 5% magnesium content does not exceed 5.10 ~ 6% does not exceed 5.10 ~ 6% does not exceed 1.10_5% does not exceed 5.10 ~ 5% does not exceed 1.10 ~ 5% does not exceed 5.10 ~ 5% manganese content does not exceed 1.10_5% copper content does not exceed 2.10_6% does not exceed 5.10 ~ 6% does not exceed 2.10-6% does not exceed 5.10_5% does not exceed 3.10_5% does not exceed 5.10 ~ 5% riikel content silver content thallium content calcium content iron content PL PL
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PL15577572A PL77840B2 (en) | 1972-06-03 | 1972-06-03 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PL15577572A PL77840B2 (en) | 1972-06-03 | 1972-06-03 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| PL77840B2 true PL77840B2 (en) | 1975-04-30 |
Family
ID=19958806
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PL15577572A PL77840B2 (en) | 1972-06-03 | 1972-06-03 |
Country Status (1)
| Country | Link |
|---|---|
| PL (1) | PL77840B2 (en) |
-
1972
- 1972-06-03 PL PL15577572A patent/PL77840B2/pl unknown
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