Patent GB-681033-A (GB)
Title: Improvements in or relating to lubricating compositions for cellulose derivative yarns and filaments
Filed: 1950-04-14
Abstract: In the manufacture of a conditioning agent for use in lubricants for cellulose derivatives (see Group III), a mixture of a long-chain fatty acid, a vegetable oil and a mineral oil is reacted with oleum and the product is treated with alkali to neutralize sulphuric acid and a major portion of the fatty acid and then de-salted and dehydrated as described in Specification 649,148.  The oleum is used at a temperature not above 20 DEG  C., whereby at least part of the fatty acid and vegetable oil are sulphated or sulphonated.  Following the reaction with oleum there is normally added an alkylated phenol, e.g. dibutyl or diamyl phenol, as a stabilizer, anti-oxidant and penetrant.  Starting materials mentioned are oleic, ricinoleic and palmitoleic acids and olive, rice and peanut oils.  In an example, a mixture of white oil, oleic acid and peanut oil is reacted with oleum, diamyl phenol added to the product and then sufficient aqueous sodium hydroxide to neutralize; the product is de-salted by addition of anhydrous isopropanol followed by filtration and dehydrated by distilling off the isopropanol as an azeotrope with the water present.ALSO:A conditioning composition for filaments of cellulose acetate and other organic derivatives of cellulose comprises a mineral oil, an aryl phosphate, a long-chain fatty acid, an alkylolamine, and a mixture obtained by desalting and dehydrating the alkali - neutralized reaction product of oleum on a mixture of a long-chain fatty acid, a vegetable oil and a mineral oil.  The term "long chain" is defined as containing a chain of at least 12 carbon atoms united by carbon-to-carbon linkages.  The aryl phosphate is preferably tricresyl phosphate.  The long-chain fatty acid is preferably oleic acid and is preferably present in the amount required to produce the amine salt with the alkylolamine. A blending agent such as oleyl alcohol, lauryl alcohol or other long-chain fatty alcohol may also be present.  The mixture preferably contains also from 0.5 to 2 per cent by weight of water so that it is substantially in equilibrium with the atmosphere. The desalted and dehydrated reaction product may contain an alkyl phenol (dibutyl phenol, diamyl phenol) as an antioxidan and may advantageously be diluted with mineral oil preparatory to incorporation in the composition.  In its preparation 20 per cent oleum may be reacted with mineral oil, olive oil, rice oil, peanut oil or other vegetable oil and a long-chain fatty acid such as oleic, ricinoleic or palmitoleic acid, at a temperature not above 20 DEG  C.  At the completion of the reaction an alkylated phenol is added and the mixture neutralized by the addition of alkali metal hydroxide.  The mixture is then desalted and dehydrated as described in Specification 649,148 and diluted with mineral oil, about 60 parts by weight of mineral oil being added to about 40 parts by weight of the salt-free, dehydrated product.  The final composition may contain 50 to 60 parts mineral oil, 4 to 12 parts triaryl phosphate, 5 to 14 parts long-chain fatty acid, 2.5 to 7 parts alkylolamine, 0.25 to 0.75 parts long-chain fatty alcohol, and 20 to 30 parts mineral oil-diluted, desalted, dehydrated, sulphated and/or sulphonated reaction product, all parts being by weight.  About 1.3 to 1.6 per cent of water may be added when the composition is to be employed at a relative humidity of 55 to 65 per cent, and about 0.5 to 0.7 per cent for a relative humidity of 30 to 40 per cent.  About 4 per cent by weight of the dressing is applied to the running filaments.  Filaments of cellulose propionate, butyrate, acetate-propionate, acetate-butyrate and ethyl and benzyl cellulose may be treated.  In an example (all parts by weight) 52.2 parts of paraffin base acid-refined mineral oil (50 S.U.S. at 100 DEG F.), 9.4 parts oleic acid, 4.7 parts triethanolamine, 8.4 parts tri-cresyl phosphate, 0.5 parts oleyl alcohol, and 24.8 parts of the mineral oil-diluted, desalted and dehydrated reaction product of 20 per cent oleum on a mixture of oleic acid, raw peanut oil and mineral oil (50 seconds Saybolt at 100 DEG  F.) are mixed, (for preparation of the reaction product see Group IV (b)), whereafter 1.4 parts by weight of water are added and the final composition filtered for use. Specification 539,333 also is referred to.ALSO:A lubricating composition for filaments of cellulose acetate and other organic derivatives of cellulose, comprises a mineral oil, an aryl phosphate, a long chain fatty acid, an alkylolamine, and a mixture obtained by desalting and dehydrating the alkali-neutralised reaction product of oleum on a mixture of long chain fatty acid, a vegetable oil and a mineral oil.  The term "long chain" is defined as containing a chain of at least 12 carbon atoms united by carbon-to-carbon linkages.  The aryl phosphate is preferably tricresyl phosphate.  The long chain fatty acid is preferably oleic acid and is preferably present in the amount required to produce the amine salt with the alkylolamine.  A blending agent such as oleyl alcohol, lauryl alcohol or other long chain fatty alcohol may also be present. The mixture preferably contains also from 0.5 to 2 per cent by weight of water so that it is substantially in equilibrium with the atmosphere.  The desalted and dehydrated reaction product may contain an alkyl phenol (dibutyl phenol, diamyl phenol) as an anti-oxidant, and may be diluted with mineral oil preparatory to incorporation in the composition.  In its preparation 20 per cent oleum may be reacted with mineral oil, olive oil, rice oil, peanut oil or other vegetable oil and a long chain fatty acid such as oleic, ricinoleic or palmitoleic acid, at a temperature not above 20 DEG C.  At the completion of the reaction an alkylated phenol is added and the mixture neutralized by the addition of alkali metal hydroxide.  The mixture is then desalted and dehydrated as described in Specification 649,148 and diluted with mineral oil, about 60 parts by weight of mineral oil being added to about 40 parts by weight of the salt-free, dehydrated product.  The final composition may contain 50-60 parts mineral oil, 4-12 parts triaryl phosphate, 5-14 parts long chain fatty acid, 2.5-7 parts alkylolamine, 0.25-0.75 parts long chain fatty alcohol, and 20-30 parts mineral oil-diluted, desalted, dehydrated sulphated and/or sulphonated reaction product, all parts being by weight.  About 1.3 to 1.6 per cent of water may be added when the composition is to be employed at a relative humidity of 55-65 per cent, and about 0.5-0.7 per cent for a relative humidity of 30-40 per cent.  About 4 per cent by weight of the dressing is applied to the running filaments. Filaments of cellulose propionate, butyrate, acetate - propionate, acetate-butyrate and ethyl and benzyl cellulose may be treated.  In an example (all parts by weight) 52.2 parts of paraffin base acid-refined mineral oil (50 S.U.S. at 100 DEG F), 9.4 parts oleic acid, 4.7 parts triethanolamine, 8.4 parts tri-crisyl phosphate, 0.5 parts oleyl alcohol, and 24.8 parts of the mineral oil-diluted, desalted and dehydrated reaction product of 20 per cent oleum on a mixture of oleic acid, raw peanut oil and mineral oil (50 seconds Saybolt at 100 DEG F) are mixed (for preparation of the reaction product see Group IVb), whereafter 1.4 parts by weight of water are added and the final composition filtered for use.  Specification 539,333 also is referred to.