US1611695A - Manufacture of lead alkyl compounds - Google Patents

Description

Patented Dec. 1926.

.A-UNITED v sT rEs PATENT fol-rice.

rnnnnnrox w. SULLIVAN, .13., AND LYMAN' CHALKLEY, .13., or wnrrme, IN IANA, nssreuons 'ro smunann OIL COMPANY, or WRITING, INDIANA, A CORPORATION OF INDIANA.

MANUFACTURE or. LEAD 'ALKYL' controuuns.

' No Drawing.

pounds, "and more particularly of 'lead.

. contain from 3 to 317aof sodium, 'it being,

\ the desired extent.

or may be heated tetraethyl, and will be fully understood from the 'followin description thereof. r

The invention will be specifically dccribed in connection with the manufacture of lead tetra'ethyl, although, as hereinafter pointed out, other lead alkyl compounds maybe manufactured under the process of thls invention. I l r ln'carrying out the invention for the for .mation of lead tetra/ethyl, a sodium lead alloy is subjected tothe action ofethyl sulfate, preferably vii -the presence of a halogen containing ganic halide. Thesodium' lead alloy may preferred that its sodi-liih contents be within the range'of from "li to 20%. The alloy containing 10% of s odiu'm has been found; to be particularly suitable; The amount of dietliyl sulfate employed is preferably not in excess of the calculaped equivalent 'required for reaction with the lead alloy, only one ethyl group being considered as reactive, Thus for .100 parts of sodiumlead alloy containing 10% of sodium, the cal-- (lulated equivalent quantity 'of diethyl sulfate is about 67 parts. The use of rts has been found to be particularlya vantageous, although lower. or higher proporene-r-j' tions may be employed. It is not allydesirable thatthe proportion of diethyl sulfate employed be less than 50% of the calculated equivalent. Anon-aqueous solventsu'ch as benzol, toluol or the like may be employed, serving primarilyjto control the rate of reaction. -It is also desirable that a, slight trace of Water be present;

The reactlonco i s tituents are admixed, pref-o I erabl-y with the solvent, the proportion of- .which, *whenused 'amount equal in, weightflto the amount of ethyl sulfate to from 50toj100% more and 'a tracefiof water, aytwklifto three reps may be added. mixture is then' heated to boiling under al refluxcondenser under pressure while hemg stirred until reaction 1 is completed to small amount of a ed. Thus chlorine,

It is preferred that halogen catalyst be ad vcompound, preferably .an inorparts oflead tetraethyl, a yield of approx- ,,may vary from an Application filed October 6, 1924. Serial No. 742,063.

bromine, iodine, or their salts, such as the alkali metal, alkaline earth metal, and zinc halides and the like may be employed. The

proportion required is very small, in general from one-halftothre'e per cent based on the diethyl sulfate con sufi'icient. With potassium iodide as a catalyst, highly satisfactory results have been obtained employing 1%..-

tent of the mixture being The following specific instance of a proc ess carried out under this invention illus trates'satisfactory conditions for operation.

100 parts of' ing 10% of sodium, 50 parts of ethyl sulsodium lead alloy containfate and about {parts of toluol are thoroughly mixed, 0.5 parts potassium iodide and-a. traze of water (two or three drops) being added. The mixture is boiled under a reflux column while being stirred, the"- heating being continued until'the reaction is carried to substantial completiom h'om 4 to 6 hours being required. In order to separate the lead tetraethyl produced, the re action mixture is treated with Water, and distilled or the lead tetraethyl otherwise re-' The separation may be or I vacuum distillation,

imately of theoretical, arejobtamecl. Th

which potassium iodide isan. example,

. P- pears greatly accelerate the rate of re I action and increase the yield. 7 The reaction may be carried out; however, without such facturing other lead alkyl compounds, 'sub-. stituting for the diethyl sulfate other alkyl sulfates' such as dimethyl sulfate, dipropyl sulfate,

ethylmethyl sulfate,

ethyl propyl sulfate, dibutyl sulfate and the like, the proportion of the various constituents 'of the as indicated with th man ufacture reaction mixture being varied above in connection of'lead tetraethyl. K .lVe claim: 3

1. The method of manufacturing lead alkyl compounds comprising the intermixe presence of a halide catalyst, 'ofw as chlorin, bromin,

T 1e invention mav be employedsin ma'nucomprising admixing a. so im lead alloyiodine compound ture of a sodium lead allo and a dialkyl sulfate, and the subsequent eating of the mixture. a

2. The method pounds comprising admixing a sodium lead alloy and a dialkyl sulfate in the presence of a halogen compound derived from the group including the elemental halogens and the soluble metallic halides and heating the mixture. x

3. The method of forming a lead alkyl comprising admixing a sodium lead alloy and a dialkyl sulfate in theresence of a halogen compound derived rom the group including the elemental halogens and the soluble metallic halides and a trace of Water, and heatin the mixture.

4. The method forming lead tetraethyl comprising admixing and heating together a sodium lead alloy and diethyl sulfate.

5'. The method of forming lead tetraethyl comprising admixing a sodium lead alloy and diethyl sulfate in the presence of a halogen compound derived from the group including the elemental halogens and the soluble metallic halides and heatingthe mixture.

6. The method of forming lead tetraethyl comprising admixing a sodium lead alloy and diethyl sulfatein' the presence of an derived from the group including iodine and the soluble metallic iodides and a trace of water and'heating the mixture.

Y 7. The method of forinin lead tetraethyl of forming lead alkyl com-- with diethyl sulfate in the presence'of an anhydrous solvent and a halogen catalyst derived from the group including the elemental halogens and the soluble metallic halides, and heating the mixture. 8. The method of forming lead tetraethyl comprising admixing a-sodium lead alloy with diethyl sulfate in amounts not in excess of the monomolecular equivalent, incorporating in the mixture a halogen catalyst derived from the group including the elemental halogens and the soluble metallic halides and heating'themixture.

9". The method of forming lead tetraethyl comprising admixing a sodium-lead alloy containing 3 to 31% of sodium with at least 50% .of the monomolecular' equivalent of diethyl sulfate and heating the mixture.

10. The method of forming lead tetraethyl compi'ising admixing? a sodium lead alloy containing 3 to 31% of sodium With at vleast 50% of the monomolecular equivalent of diethyl sulfate in the presence of a halogen body derived'from the group includingthe elemental halogensand the soluble metallic halides and'a tr'a'ce of water, and heating the mixture. 5 j

11. The method of forming lead tetraethyl comprising admixing 100 parts of a sodium lead alloy containing 1( of sodium, 50 parts of diethyl sulfate, 'pa1-t of potassium iodide, about 65 parts of toluol and a trace of water an'd heating the mixture un reflux condenser. 7

Y FREDERICK w. SULLIVAN, JR;- Li M N enAnm. 1 a r ..-IR.-

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