US1975171A - Process of purifying tetra alkyl lead - Google Patents
Process of purifying tetra alkyl lead Download PDFInfo
- Publication number
- US1975171A US1975171A US526141A US52614131A US1975171A US 1975171 A US1975171 A US 1975171A US 526141 A US526141 A US 526141A US 52614131 A US52614131 A US 52614131A US 1975171 A US1975171 A US 1975171A
- Authority
- US
- United States
- Prior art keywords
- lead
- tetra
- tetra alkyl
- alkyl lead
- aqueous solution
- 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
- 125000000217 alkyl group Chemical group 0.000 title description 23
- 238000000034 method Methods 0.000 title description 11
- MRMOZBOQVYRSEM-UHFFFAOYSA-N tetraethyllead Chemical compound CC[Pb](CC)(CC)CC MRMOZBOQVYRSEM-UHFFFAOYSA-N 0.000 description 42
- 239000007864 aqueous solution Substances 0.000 description 13
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 9
- 239000001488 sodium phosphate Substances 0.000 description 7
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 7
- 235000019801 trisodium phosphate Nutrition 0.000 description 7
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 7
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 239000007859 condensation product Substances 0.000 description 4
- 239000003599 detergent Substances 0.000 description 4
- 238000009736 wetting Methods 0.000 description 4
- 229910021538 borax Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- PSZYNBSKGUBXEH-UHFFFAOYSA-N naphthalene-1-sulfonic acid Chemical class C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-N 0.000 description 3
- 159000000000 sodium salts Chemical class 0.000 description 3
- 235000010265 sodium sulphite Nutrition 0.000 description 3
- 235000010339 sodium tetraborate Nutrition 0.000 description 3
- 239000004328 sodium tetraborate Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 2
- -1 alkyl lead compounds Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 235000017550 sodium carbonate Nutrition 0.000 description 2
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 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
- 239000005909 Kieselgur Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- XTFHTDANPJKKNI-UHFFFAOYSA-N butyllead Chemical compound CCCC[Pb] XTFHTDANPJKKNI-UHFFFAOYSA-N 0.000 description 1
- 239000008395 clarifying agent Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000015424 sodium Nutrition 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 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
- NMYKPZSMIQTTPB-UHFFFAOYSA-M sodium;4,7-di(propan-2-yl)naphthalene-2-sulfonate Chemical compound [Na+].CC(C)C1=CC(S([O-])(=O)=O)=CC2=CC(C(C)C)=CC=C21 NMYKPZSMIQTTPB-UHFFFAOYSA-M 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- XOOGZRUBTYCLHG-UHFFFAOYSA-N tetramethyllead Chemical compound C[Pb](C)(C)C XOOGZRUBTYCLHG-UHFFFAOYSA-N 0.000 description 1
- SMHNCYOTIYFOKL-UHFFFAOYSA-N tetrapropylplumbane Chemical compound CCC[Pb](CCC)(CCC)CCC SMHNCYOTIYFOKL-UHFFFAOYSA-N 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/24—Lead compounds
Definitions
- This invention relates to the process of producing tetra alkyl lead and more particularly to the process of removing sludge in such processes.
- An object of my invention is to overcome the difficulties heretofore experienced in the manufacture of tetra alkyl lead, and particularly tetra ethyl lead.
- a further object of my invention is the removal of suspended matter in tetra alkyl lead processes.
- Nekal A which is the sodium salt of the condensation product of naphthalene sulfonic acids and isopropyl alcohol. Other similar condensation products may also be used.
- sludge as used herein is to be understood as applied to the finely divided lead, etc., in suspension in the tetra ethyl lead, or like compounds.
- the process of removing suspended matter from tetra alkyl lead which comprises agitating the tetra alkyl lead with an aqueous solution of a compound of the group consisting of borax, sodium carbonate, trisodium phosphate, sodium sulfite, sodium bisulfite, and the sodium salt of the condensation product of naphthalene sulfonic acid and isopropyl alcohol, permitting the tetra alkyl lead to separate from the aqueous solution, and then drawing off the purified tetra alkyl lead.
- a compound of the group consisting of borax, sodium carbonate, trisodium phosphate, sodium sulfite, sodium bisulfite, and the sodium salt of the condensation product of naphthalene sulfonic acid and isopropyl alcohol permitting the tetra alkyl lead to separate from the aqueous solution, and then drawing off the purified tetra alkyl lead.
- the step which comprises distilling off the tetra alkyl lead from a reaction mass containing the same, treating the distilled tetra alkyl lead with an aqueous solution of a compound having pronounced wetting and detergent properties, permitting the tetra alkyl lead to separate from the from tetra ethyl lead which comprises agitatingv the tetra ethyl lead with an aqueous solution of .a-
- the process of removing suspended matter from tetra ethyl lead which comprises agitating the tetra ethyl lead with an aqueous solution of trisodium phosphate, permitting the tetra ethyl lead to separate from the aqueous solution, and
- v 1 8.
- the step which comprises distilling off the tetra ethyl lead from a reaction mass containing the saine, treating the distilled tetra ethyl lead with an aqueous solution of a compound having pronounced wetting and detergent properties, permitting the tetra ethyl lead to separate from the aqueous solution, and then drawing oil the purified tetraethyl lead; ALFRED E. PARMELEE.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Detergent Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Patented Oct. 2, 1934 u irs Alfred EfP armelee, Carneys loinflli. .I assi 'gn or: v Q
i to E. I. du Pont de Nemours &Gompany,-;W ilmingto'm D eL, a corporation of Delaware p c h arcli. 2 .5 931; Serial No. 5.2 .14; 21,231;
No Draw n 8 Claims. (Cl. 260-11) This invention relates to the process of producing tetra alkyl lead and more particularly to the process of removing sludge in such processes.
When tetra alkyl lead is recovered by steam distillation from the reaction mass in which it is formed, there is carried over a very appreciable amount of finely divided metallic lead and also organic derivatives of lead which are solids. These solid materials remain suspended in the tetra alkyl lead and are so fine that they are not readily removed by any common means of filtration. The ordinary clarifying agents such as diatomaceous earth and charcoals may not be used with ease or safety for clarifying because the tetra alkyl lead which is absorbed upon their surface will catch fire spontaneously on exposure to air.
An object of my invention is to overcome the difficulties heretofore experienced in the manufacture of tetra alkyl lead, and particularly tetra ethyl lead. A further object of my invention is the removal of suspended matter in tetra alkyl lead processes. Other and further objects will appear hereinafter.
These objects are accomplished by the following invention in which I have found that the solid particles which are suspended in tetra ethyl lead may be coagulated and caused to separate by floating to the interfacial layer if the tetra ethyl lead is washed with relatively dilute solutions of one of several inorganic compounds and organic compounds, or mixtures of such compounds, Those compounds which possess strong detergent and wetting properties have been found especially efi'icacious for my purpose. Such compounds comprise trisodium phosphate, borax, sodium car- 'bonate, sodium sulfite, sodium metasilicate, so-
dium bisulfite and commercial wetting agents known as Nekal A, which is the sodium salt of the condensation product of naphthalene sulfonic acids and isopropyl alcohol. Other similar condensation products may also be used.
With the View of more clearly disclosing my invention the following illustrative example of one specific embodiment thereof is given.
Ewample 30,000 to 40,000 pounds of crude tetra ethyl lead are placed in a suitable washer which is provided with an agitator. 500 gallons of water in which have been dissolved 10 to 20 pounds of trisodium phosphate are then added and the mixture is agitated for 10 minutes to 1 hours. The agitation is then stopped and the charge allowed to settle for one or more hours. When the settling period has been completed it will be found that the solids which were suspended in the tetra ethyl lead have been wetted by the water solution of trisodium phosphate and will have collected at the interfacial layer between the two liquids. This makes it possible to draw off, from the bottom, the tetra ethyl lead in a purified condition and free from suspended sludges.
While my invention is illustrated specifically as applied to the manufacture of tetra ethyl lead, it will be understood that it may be applied in a similar manner in the manufacture of any of the tetra alkyl lead compounds, such as tetra methyl lead, tetra butyl lead, tetra propyl lead, etc.
The term sludge as used herein is to be understood as applied to the finely divided lead, etc., in suspension in the tetra ethyl lead, or like compounds.
As many apparently widely difierent embodiments of this invention may be made without departing from the spirit thereof, it is to be under-' stood that I do not limit myself to the foregoing examples or descriptions except as indicated in the following patent claims.
I claim:
1. The process of removing suspended matter from tetra alkyl lead which comprises agitating the tetra alkyl lead with an aqueous solution of a compound having pronounced wetting and detergent properties, permitting the tetra alkyl lead to separate from the aqueous solution, and then drawing off the purified tetra alkyl lead.
2. The process of removing suspended matter from tetra alkyl lead which comprises agitating the tetra alkyl lead with an aqueous solution of a compound of the group consisting of borax, sodium carbonate, trisodium phosphate, sodium sulfite, sodium bisulfite, and the sodium salt of the condensation product of naphthalene sulfonic acid and isopropyl alcohol, permitting the tetra alkyl lead to separate from the aqueous solution, and then drawing off the purified tetra alkyl lead.
3. The process of removing suspended matter from tetra alkyl lead which comprises agitating the tetra alkyl lead with an aqueous solution of trisodium phosphate, permitting the tetra alkyl lead to separate from the aqueous solution, and then drawing off the purified tetra alkyl lead.
4. In the process of producing tetra alkyl lead, the step which comprises distilling off the tetra alkyl lead from a reaction mass containing the same, treating the distilled tetra alkyl lead with an aqueous solution of a compound having pronounced wetting and detergent properties, permitting the tetra alkyl lead to separate from the from tetra ethyl lead which comprises agitatingv the tetra ethyl lead with an aqueous solution of .a-
compound of the group consisting of borax,
sodium carbonate, trisodium phosphate, sodium sulfite, sodium bisulfite, and the sodium salt of the condensation product of naphthalene sulfonic acid and isopropyl alcohol, permittingthe tetra ethyl lead to separate from the aqueous solution, and then drawing off the purified tetra ethyl lead.
'7. The process of removing suspended matter from tetra ethyl lead which comprises agitating the tetra ethyl lead with an aqueous solution of trisodium phosphate, permitting the tetra ethyl lead to separate from the aqueous solution, and
' then drawing ofi the purified tetra ethyl lead.
v 1 8. In the process of producing tetra ethyl lead, the step which comprises distilling off the tetra ethyl lead from a reaction mass containing the saine, treating the distilled tetra ethyl lead with an aqueous solution of a compound having pronounced wetting and detergent properties, permitting the tetra ethyl lead to separate from the aqueous solution, and then drawing oil the purified tetraethyl lead; ALFRED E. PARMELEE.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US526141A US1975171A (en) | 1931-03-28 | 1931-03-28 | Process of purifying tetra alkyl lead |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US526141A US1975171A (en) | 1931-03-28 | 1931-03-28 | Process of purifying tetra alkyl lead |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US1975171A true US1975171A (en) | 1934-10-02 |
Family
ID=24096087
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US526141A Expired - Lifetime US1975171A (en) | 1931-03-28 | 1931-03-28 | Process of purifying tetra alkyl lead |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US1975171A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2440810A (en) * | 1943-05-29 | 1948-05-04 | Du Pont | Purification of tetraethyl lead |
| US2622093A (en) * | 1951-05-23 | 1952-12-16 | Ethyl Corp | Recovery of tetraalkyllead compounds |
| US3088920A (en) * | 1960-04-26 | 1963-05-07 | Du Pont | Process for treating tetraalkyllead compositions |
| US3384559A (en) * | 1964-08-04 | 1968-05-21 | Ethyl Corp | Tetraalkyllead recovery from an anhydrous reaction mass |
| US3452069A (en) * | 1966-07-29 | 1969-06-24 | Ethyl Corp | Process for manufacture of tetraalkyllead and reclamation of by-product lead |
-
1931
- 1931-03-28 US US526141A patent/US1975171A/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2440810A (en) * | 1943-05-29 | 1948-05-04 | Du Pont | Purification of tetraethyl lead |
| US2622093A (en) * | 1951-05-23 | 1952-12-16 | Ethyl Corp | Recovery of tetraalkyllead compounds |
| US3088920A (en) * | 1960-04-26 | 1963-05-07 | Du Pont | Process for treating tetraalkyllead compositions |
| US3384559A (en) * | 1964-08-04 | 1968-05-21 | Ethyl Corp | Tetraalkyllead recovery from an anhydrous reaction mass |
| US3452069A (en) * | 1966-07-29 | 1969-06-24 | Ethyl Corp | Process for manufacture of tetraalkyllead and reclamation of by-product lead |
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