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    Clay grease compositions and process of preparation therefor
    2.
    发明授权
    Clay grease compositions and process of preparation therefor 失效
    粘土润滑脂组合物及其制备方法

    公开(公告)号：US2886524A

    公开(公告)日：1959-05-12

    申请号：US56192256

    申请日：1956-01-27

    Applicant: SHELL DEV

    Inventor： ARMSTRONG JACK W ,  PREISS DONALD M

    IPC: B01J19/06 ,  C04B33/13

    CPC classification number: C04B33/1305 ,  C04B33/13 ,  C10M5/00 ,  C10M7/00 ,  C10M2201/08 ,  C10M2201/081 ,  C10M2201/082 ,  C10M2201/084 ,  C10M2201/085 ,  C10M2201/14 ,  C10M2205/00 ,  C10M2207/282 ,  C10M2207/34 ,  C10M2211/02 ,  C10M2211/06 ,  C10M2213/02 ,  C10M2213/062 ,  C10M2215/06 ,  C10M2215/062 ,  C10M2215/064 ,  C10M2215/066 ,  C10M2215/068 ,  C10M2215/086 ,  C10M2215/14 ,  C10M2215/22 ,  C10M2215/221 ,  C10M2215/225 ,  C10M2215/226 ,  C10M2215/28 ,  C10M2215/30 ,  C10M2217/00 ,  C10M2217/02 ,  C10M2217/04 ,  C10M2223/04 ,  C10M2223/041 ,  C10M2223/042 ,  C10M2227/02 ,  C10M2229/02 ,  C10M2229/04 ,  C10M2229/041 ,  C10M2229/043 ,  C10M2229/044 ,  C10M2229/05 ,  C10N2220/02 ,  C10N2230/08 ,  C10N2240/02 ,  C10N2240/12 ,  C10N2240/121 ,  C10N2250/10 ,  C10N2270/00 ,  C10N2270/02

    Abstract: A process for the preparation of grease-forming compositions comprises adding an aniline compound to a fluid clay hydrogel, mechanically separating water, displacing the remaining water with a water-soluble organic liquid, adding a lubricating oil to the resultant organogel in a proportion sufficient to prevent collapse of the gel structure but insufficient to form a grease, evaporating the water-soluble organic liquid, and heating the mixture in an oxidizing atmosphere to oxidize the aniline compound. The lubricating oil may be a refined, unrefined or semi-refined paraffinic, naphthenic or asphaltic base mineral oil (50 to 4000 SUS/100 DEG F.) or blend thereof or a synthetic oil such as the esters of phosphorus- and/or silicon-containing and aliphatic dicarboxylic acids, e.g. tritolyl phosphate, tetrakis-(2-ethylhexyl)-silicate, dioctyl phthalate, and bis-(2-ethylhexyl) and bis-(3,5,5 - trimethylhexyl) - sebacates, halocarbon oils, e.g. fluorocarbons, and liquid organosilicone polymers, e.g. dimethyl and methyl phenyl silicone polymers which are extensively described and exemplified. The aniline compounds include aniline itself and nuclear amino, methyl and hydroxyl substitution products thereof, e.g. the phenylene diamines, amino phenols, toluidines and xylidenes. When heated in the oxidizing atmosphere, i.e. air with or without added oxygen, the ultimate oxidation product of aniline is aniline black, and although intermediate products such as emeraldine, nigraniline, and pernigraniline are effective it is preferred that at least 50% of the aniline be completely oxidized. The clays are preferably high-based exchange clays such as Wyoming bentonite or hectorite, though low-base exchange clays, e.g. Georgia clay, attapulgite, may be used. The clay hydrogel is preferably treated with a mineral acid, e.g. H2SO4, HCl, H3PO4. Suitable water-soluble organic liquids include alcohols, ketones and esters, e.g. methyl, ethyl and isopropyl alcohols, acetone, methylethyl ketone and ethyl acetate. The oil used to prepare greases from these concentrates is preferably the same as that already incorporated therein. Examples comprise hectorite clay treated with 85% H3PO4, aniline, alcohol as volatile solvent, and a silicone oil. The compositions were heated in a forced draught oven at 300 DEG F. for 2 days and then milled with more silicone oil to form greases. Specification 736,270 is referred to.ALSO:A process for the preparation of greaseforming compositions (see Group III) comprises adding an aniline compound to a fluid clay hydrogel, mechanically separating water, displacing the water from the remaining concentrated clay hydrogel with a water-soluble organic liquid, adding a lubricating oil to the organogel in amount sufficient to preserve the gel structure during subsequent evaporation of the organic liquid but insufficient to form a grease structure, evaporating the water-soluble organic liquid and heating in an oxidizing atmosphere to oxidize the aniline compound. A silicone oil may subsequently be added to form a grease containing 1 to 8% wt. of clay. In an example 1 kg. of 2% wt. Hectorite clay in an aqueous slurry is acidified with 1.4 g. 85% H3PO4. 40 g. aniline are added, the water removed by filtration, and the filter coke washed with ethanol. The aniline coated clay is then dispersed in 1000 ml. ethanol and 100 g. commercial silicone oil and the alcohol evaporated off. The composition is then heated in a forced draught oven at 300 DEG F. for 2 days to oxidize to aniline. On milling the resulting composition with 100 g. silicone oil a smooth black grease is obtained. Specification 736,270, [Group III], is referred to.

    Process for the preparation of greases gelled with polymer coated clays
    4.
    发明授权
    Process for the preparation of greases gelled with polymer coated clays 失效
    用聚合物涂层粘土凝胶化的润滑脂的制备方法

    公开(公告)号：US2829100A

    公开(公告)日：1958-04-01

    申请号：US55227155

    申请日：1955-12-12

    Applicant: SHELL DEV

    Inventor： ARMSTRONG JACK W ,  PREISS DONALD M ,  EDGAR JOHN A

    IPC: C04B33/13

    CPC classification number: C04B33/1305 ,  C04B33/13 ,  C10M5/00 ,  C10M7/00 ,  C10M2201/08 ,  C10M2201/081 ,  C10M2201/082 ,  C10M2201/084 ,  C10M2201/085 ,  C10M2201/103 ,  C10M2201/14 ,  C10M2207/282 ,  C10M2207/34 ,  C10M2209/101 ,  C10M2211/02 ,  C10M2211/022 ,  C10M2211/024 ,  C10M2211/06 ,  C10M2213/00 ,  C10M2213/02 ,  C10M2213/04 ,  C10M2213/06 ,  C10M2213/062 ,  C10M2215/04 ,  C10M2215/06 ,  C10M2215/10 ,  C10M2215/102 ,  C10M2215/16 ,  C10M2215/22 ,  C10M2215/221 ,  C10M2215/222 ,  C10M2215/225 ,  C10M2215/226 ,  C10M2215/26 ,  C10M2215/30 ,  C10M2217/022 ,  C10M2217/042 ,  C10M2217/043 ,  C10M2217/046 ,  C10M2217/06 ,  C10M2219/044 ,  C10M2219/064 ,  C10M2221/02 ,  C10M2223/04 ,  C10M2223/041 ,  C10M2223/042 ,  C10M2227/02 ,  C10M2229/02 ,  C10M2229/04 ,  C10M2229/041 ,  C10M2229/043 ,  C10M2229/044 ,  C10M2229/05 ,  C10M2229/051 ,  C10N2220/02 ,  C10N2230/08 ,  C10N2240/02 ,  C10N2240/12 ,  C10N2240/121 ,  C10N2250/10 ,  C10N2270/00

    Abstract: A process for the preparation of lubricating grease compositions comprises adding an aminoplast-forming amino compound or hexamethylenetetramine to a fluid clay hydrogel, mechanically separating a substantial proportion of water from the hydrogel, displacing the remaining water by a volatile water-miscible organic liquid, adding a water-insoluble lubricating oil and evaporating the water-miscible organic liquid. The lubricating oil may be a paraffinic, naphthenic or asphaltic base lubricating oil or blend thereof or a synthetic oil such as the esters of phosphorus or silicon-containing acids and esters of aliphatic dicarboxylic acids with monohydric alcohols, e.g. tritolyl phosphate, dioctyl phthalate, bis-(2-ethyl hexyl) and bis-(3,5,5-trimethylhexyl) sebacates and tetrakis (2-ethyl hexyl) silicate. Suitable base oils for high temperature greases are the halocarbon oils such as the fluorocarbons and the organisilicone liquids such as polymers of dimethyl silicone which are extensively described and exemplified. The clay is preferably a high base exchange clay such as Wyoming bentonite or hectorite, though low base exchange clays such as Georgia clay and attapulgite may be used. Suitable amino compounds include those with at least 2 amino groups per molecule, each being attached to an unsaturated carbon atom, e.g. urea, thio-urea, guanidine, melamine, and dicyandiamide and the compounds obtained by replacing one hydrogen atom in such compounds by an alkyl group, e.g. methyl, ethyl and propyl urea, thioureas and guanidines; aryl primary amines, e.g. aniline and its alkyl derivatives; and alkyl sulphonamides, e.g. benzene, toluene, and other alkaryl sulphonamides. In all these compounds at least one amino group is attached to an unsaturated carbon or sulphur atom. Volatile water-miscible organic liquids are those which are more volatile than the lubricating oil and preferably have a relatively low boiling point such as alcohols and ketones, e.g. methanol, ethanol, isopropyl alcohol, acetone and methyl ethyl ketone, esters, e.g. ethyl acetate, and mixtures of the above. An optional feature of the invention is to treat the clay hydrogel with a mineral acid, e.g. phosphoric (which is preferred), hydrochloric or sulphuric, preferably before adding the amino compound. A further optional feature of the invention is to use the process to prepare the aminoplast-coated clay greases of Specification 793,092 by subsequently adding an aldehyde, preferably with the lubricating oil, to react with the amine already present. Suitable aldehydes include saturated and unsaturated aliphatic aldehydes or cyclic derivatives thereof, e.g. formaldehyde, acrolein, furfural, crotonaldehyde and acetaldehyde. When hexamethylene tetramine is used, it may be decomposed to formaldehyde by heating the clay hydrogel and a phenoplast resin formed by adding a phenol, e.g. phenol, resorcinol, the cresols and alkyl phenols such as t-butyl phenol and t-amyl phenol. Alternatively the amino compound added initially may not, or may only partially be used, to form the resin, which may be formed by subsequently adding an aldehyde and an amine or phenol, e.g. with the lubricating oil. In several examples, the amino compounds used are aniline, melamine, hexamethylene tetramine, and benzidine and the oil in each is a dimethyl silicone fluid, the aldehydes used are paraformaldehyde and furfural and, where hexamethylene tetramine is decomposed, phenol is used to form a phenoplast resin. Specification 736,270 also is referred to.ALSO:A process for the preparation of lubricating grease compositions (see Group III), comprises adding an aminoplast-forming amino compound or hexamethylene tetramine to a fluid clay hydrogel, mechanically separating a substantial proportion of water from the hydrogel, displacing the remaining water by a volatile water-miscible organic liquid, adding a water-insoluble lubricating oil and evaporating the water-miscible organic liquid. An optional feature of the invention is to use the process to prepare the aminoplast coated clay greases of Specification 793,092 by subsequently adding an aldehyde, preferably with the lubricating oil, to react with the amine and form an aminoplast resin in situ on the clay. The clay is preferably a high base exchange clay such as Wyoming bentonite or Hectorite, though low base exchange clays such as Georgia clay and Attapulgite may be used. The clay may be treated with a mineral acid, e.g. phosphoric, hydrochloric or sulphuric before adding the amino compound. Suitable amino compounds include those with at least two amino groups per molecule, each being attached to an unsaturated carbon atom, e.g. urea, thiourea, guanidine, melamine and dicyandiamide and the compounds obtained by replacing an hydrogen atom in such compounds by an alkyl group, e.g. methyl, ethyl and propyl urea, thioureas and guanidines; aryl primary amines, e.g. aniline, its alkyl derivatives and benzidine; and alkyl sulphonamides, e.g. benzene and toluene and other alkaryl sulphonamides. In all these compounds at least one amino group is attached to an unsaturated carbon or sulphur atom. Aldehydes which may be added to form the aminoplast resin include saturated and unsaturated aliphatic aldehydes or cyclic derivatives thereof, e.g. formaldehyde, acrolein, furfural, crotonaldehyde and acetaldehyde. When hexamethylene tetramine is used it may be decomposed to formaldehyde by heating the clay hydrogel and a phenoplast resin formed in situ by adding a phenol, e.g. phenol, resorcinol, the cresols, and alkyl phenols such as t-butyl phenol and t-amyl phenol. The lubricating oil used as the basis for the greases may be paraffinic, naphthenic, asphaltic, halocarbon (e.g. fluorocarbon), synthetic (e.g. tritolyl phosphate, tetrakis (2-ethyl hexyl) silicate, dioctylphthalate, bis(2-ethyl hexyl) sebacate, bis(3,5,5-trimethylhexyl) sebacate); or silicones which may be prepared by the hydrolysis and condensation of compounds of the average formula R4-zSiXz wherein 2.25 \sF z \s0 1.5, R is a lower alkyl radical and X is a hydrolysable halogen or alkoxy group. In the examples, the oil is a dimethyl silicone fluid and the clay is Hectorite in a 2 per cent slurry acidified with H3PO4; the resins are as follows, the amines being added first: (1) and (2) aniline-paraformaldehyde, (3) aniline-formalin, (4) anilinemelamine-paraformaldehyde, (5) hexamethylene tetramine-phenol-paraformaldehyde, (6) hexamethylene tetramine-phenol, (7) aniline-furfural, (8) melamine-paraformaldehyde, and (9) benzidine-paraformaldehyde. Specification 736,270, [Group III], also is referred to.

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