Patent GB-710742-A (GB)
Title: Process of increasing the melting point of petrolatum
Inventor: SCHMERLING LOUIS
IPC: C10G73/38
Filed: 1952-05-02
Abstract: The melting point of petrolatum is increased by subjecting it to condensation with ethylene in the presence of an organic peroxide catalyst at a temperature at least as high as the decomposition temperature of the catalyst.  Ethylene from any source, particularly C2 cracking fractions may be used, the ratio of ethylene to petrolatum present by weight preferably being 1-6:1, and the ratio reacted 0.6-1.5:1.  Specified catalysts are peracetic acid, diacetyl peroxide, toluic acid peroxide, oleic peroxide, benzoyl peroxide, tertiary butyl perbenzoate, ditertiary butyl peroxide, hexyl peroxide, tertiary butyl hydroperoxide, and methylcyclohexyl hydroperoxide.  Preferably magnesium, zinc, cadmium or mercury are added as promoters, either as such or as compounds yielding the metals, preferably in finely divided form. The catalyst may be formed in situ by autoxidation of the petrolatum by passing air in the presence of a trace of peroxide from a previous reaction or an oxidation catalyst such as magnesium stearate.  Temperature is generally not more than 150 DEG C. higher than that of catalyst decomposition; and pressure is generally at least 15, preferably 30-100 atm.  Catalyst equivalent to about 0.1-5 per cent. of the ethylene is desirable but may be up to 15 per cent more.  Batch or continuous operation using either an unpacked reactor or one containing an absorbent on which the catalyst is deposited may be used or finely divided absorbent or promoter may be fluidized by the reactants.  In an example, a 43-45 DEG C. M.P. petrolatum and tart, butyl peroxide, are pressurized to 50 atm. with ethylene in a rotating autoclave, and reacted at 136 DEG C. for four hours.  A grease-like product, M.P. 74 DEG C., is obtained.  The products are of use for coating paper and fabrics and as pour point depressants.ALSO:The melting point of petrolatum is increased by subjecting it to condensation with ethylene in the presence of an organic peroxide catalyst at a temperature at least as high as the decomposition temperature of the catalyst.  Ethylene from any source, particularly C2 cracking fractions may be used, the ratio of ethylene to petrolatum present by weight preferably being 1-6 : 1, and the ratio reacted 0.6-1.5 : 1.  Specified catalysts are peracetic acid, diacetyl peroxide, toluic acid peroxide, oleic peroxide, benzoyl peroxide, tertiary butyl perbenzoate, ditertiary butyl peroxide, hexyl peroxide, tertiary butyl hydroperoxide, and methylcyclohexyl hydroperoxide.  Preferably magnesium, zinc, cadmium or mercury are added as promoters either as such or as compounds yielding the metals, preferably in finely-divided form. The catalyst may be formed in situ by autoxidation of the petrolatum by passing air in the presence of a trace of peroxide from a previous reaction or an oxidation catalyst such as magnesium stearate.  Temperature is generally not more than 150 DEG  C. higher than that of catalyst decomposition; and pressure is generally at least 15, preferably 30-100 atmos.  Catalyst equivalent to about 0.1-5 per cent of the ethylene is desirable but may be up to 15 per cent more.  Batch or continuous operation using either an unpacked reactor or one containing an adsorbent on which the catalyst is deposited may be used or finely divided adsorbent or promoter may be fluidized by the reactants.  In an example, a 43-45 DEG  C. melting point petrolatum and tert.-butyl peroxide are pressurized to 50 atmos. with ethylene in a rotating autoclave, and reacted at 136 DEG  C. for 4 hours.  A grease-like product, 74 DEG  C. melting point, is obtained.  The products are of use for coating paper and fabrics and as pour point depressants.