US 2246085 A
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Patented June 11, 1941 COMPOSITION AND PROCESS FOR SOF- TENING LEATHER, PAPER,
MATERIALS Luther B. Arnold, Jr., Wilmington, DeL,
to E. I. du Pont de Nemours & Company,
AND TEXTILE assignor Wilmington, Del., a corporation of Delaware No Drawing. Application February 23, 1938, Serial No. 192,162
This invention relates to treating agents for fibrous materials and to processes of treating such materials. More particularly it relates to compositions for softening leather, paper and textile materials and to processes therefor. Still more particularly it relates to textile treating compositions which contain high molecular weight sulfuric acid esters and urea. The invention also relates to processes of preparing such compositions.
This invention has for an object the production of chemical compositions which are useful in softening leather, paper, textile and related materials. A further object is the production of chemical compositions which have good softening action upon leather, paper and textile materials and render the same soft and pliable to the touch. A still further object is the preparation of softening compositions which render textile, leather and paper materials treated therewith pleasing in appearance, of good odor, and unchanged in color. Other objects include new leather, paper and textile treating processes and a general advancement in the art.
I have found that when urea is used in combination with long chain alcohol sulfate ester salts in certain proportions and incorporated in aqueous solutions for treating leather, paper and textile materials, they impart a novel finish to the same. The alcohol sulfate ester compositions containing certain proportions of urea when used in solution for treating fibrous materials such as cotton, hemp, jute, linen, wool, silk, regenerated cellulose, cellulose derivatives, e. g. cellulose acetate and wood pulp render the same when in filament, thread, skein, yarn or sheet form, soft and smooth to the touch and in general more pleasing cycloaliphatic hydrocarbons such as the hydrov carbons derived from petroleum.
The long-chain alcohol sulfate ester salts used according to the present invention may contain from 8 to 20 carbon atoms in the chain. They may be prepared by partially or completely sulfating long chain aliphatic alcohols and neutralizing the sulfuric acid esters with alkali metal bases. The preparation of these products is described in the chemical literature and is well known to the art. Suitable .salts of the alcohol sulfuric acid esters and their preparation are described in Bertsch Patents Nos. 1,968,794, 1,968,797 and 1,993,431. The products may also comprise the mixtures obtained by treating unsaturated long-chain alcohols with acid anhydrides, such as acetic anhydride prior to sulfation.
The invention will be further illustrated but is not intended to be limited by the following examples:
Example I An aqueous solution is prepared containing 0.2% of sodium cetyl sulfate and 0.4% of urea. It is heated to C. and applied to fabrics made from regenerated cellulose or cotton by passing them through the solution. After drying the fabrics are found to have a very smooth soft surface in addition to being pliable.
Example II A solution is prepared containing 0.5% by weight of the sodium salt of the product obtained by the conjoint sulfation of stearyl alcohol and petrolatum and 0.5% by weight of urea. Taffeta fabrics woven from regenerated cellulose and broadcloth fabrics woven from cotton after being treated in this solution at 40-60 C. and dried are found to possess a very smooth velvety surface as well as being soft and pliable. Many other types of fabrics from all known textile fibers, synthetic or natural, may be treated in a similar manner. For example, crepe fabrics from artificial silk, crepe fabric from artificial silk and cotton, printed dress fabrics from cotton and draperies from artificial silk and from cotton may be treated with urea and alcohol sulfate esters or softening agents based on alcohol sulfate esters in order to enhance their finish.
Example III Paper is treated by padding onto it a solution containing 0.1% by weight of sodium cetyl sulfate and 2.0% by weight of urea. After drying the paper has a soft, smooth surface.
The following examples illustrate the preparation of alcohol sulfate ester salts and softening agents containing urea:
Example IV Fifty parts by weight of urea are then added, theis stirred until it is homogeneous.
The product is a homogeneous, white paste in appearance. It emulsifies readily in warm water with simple agitation.
The sulfation may be also carried out to obtain still less complete sulfation of the aliphatic alcohol in order to change the finishing eifect of the product. Textiles, leatherand paper may be treated with this product following the procedure of Examples I, II and III.
Example V Nineteen and three-tenths parts by weight of stearyl alcohol and 12.8 pa ts by weight of refined petrolatum (M. P. range 40-50" 0.; Iodine No. 10-20) are melted together and 7.6 parts of chlor sulionic acid (92%-by theory on weight of stearyl alcohol) are added during agitation of the mass over a period of 30-40 minutes with a temperature maintained at 55-65 C. The mass is then stirred for 3 to 4 minutes to allow the reaction to come to an end. Sixty and three-tenths parts by weight of 5.4% sodium hydroxide at 30 C. are added to the reaction mass slowly during stirring. One hunderdand thirty-three parts by weight of urea are added. The temperature is brought to 50-60 C. and the mass is stirred until homogeneous.
The product is a homogeneous, white paste in appearance. It emulsifies readily in warm water with simple agitation and dilute emulsions even up to 5% will not separate after -20 minutes boiling or even while cooling from the boiling point.
In place of the specific alcohols of Example V, other alcohols having from 8 to 20 carbon atoms, preferably normal straight chain alcohols or mixtures, may be used. Thus, dodecy'l, myristyl, cetyl, oleyl or mixtures of the same may be substituted for the stearyl alcohol. The alcohols may be pure or of the crude or technical type, or may be mixtures.
Likewise, other hydrocarbon materials may be substituted for the refined petrolatum of Example V. Light mineral oils of 50 to 100 Baybolt units of viscosity at 100 F., heavy mineral oils oi 100 to 300 saybolt units of viscosity at 100 R,
petrolatum wax, paraflln wax or mixtures of these materials may be used. Mixtures of petrolatum with the mineral oils and/or paraflln wax give excellent results. I
Dry products which represent an important embodiment of this invention may be Pr pared in various ways. A sulfation product may be dried immediately after neutralization and the dry material ground with crystalline urea. The neutralized product resulting from the sulfation may be dried after. the addition of urea and then ground to a stable powder or it may be dried upon a drum dryer to form a flake product.
Products which have been prepared by sulrating fatty alcohols with sulfuric acid contain ing up to 30% of its weight of urea do not have any greater softening power than the product after removing the urea therefrom-does. I have found that if a material amount of urea is added to such products so that the urea is present in 1 to 50 parts per part of alcohol sulfateand preferably from 3 to 10 parts, the softening power oi the product is greatly increased and a novel finishing eflect is produced upon fibrous materials treated therewith. The urea may be added 2,246,085 temperature is raised to 45-50" C. and the mass The products (e. g., illustrated amplesIVandV) maybeappliedto paper or textiles at concentrations a wide range. Ocncentraflons Hydroscopic agents such as glycerine and glycols may be employed in conjunction with my compositions.
The compositions may be used in the dyebath asaand softening agentforusein' dyeing with a wide range of types of dyestufi's.
They are not compatible with the basic colors; with bleach-' ureaandlpartofamixtureobtainedbythe' conjoint sulfation of crude octadecyl alcohol and petrolatum and neutralization with a water soluble base.
2. The process which comprises treating fibrous materials in an aqueous bath consisting of water andasmallamountofamixtureofi to50partsofureaand1partofamixmreobtained by the conjoint sulfation of a normal primary aliphatic alcohol of at least 8 carbon atoms and a higher petroleum hydrocarbon.
3. An aqueous textile treating solution containingasmallamoimtofamixtureconsistingofi to5opartsofureaandlpartofamixtureobtained by the conjoint sulfation of a normal primary aliphatic alcohol of at least 8 carbon atoms and a higher petroleum hydrocarbon.
4.Anaqueouspastecomprising 1 to50parts ofureaandlpartofamixtureobtainedbythe conjoint sulfation of a normal primary aliphatic alcohol of at least 8 carbon atoms and a higher petroleum hydrocarbon.
5.Anaqueouspastecomprising1to50parts ofureaandlpartofamixtureobtainedbythe conjoint sulfation of stearyl alcohol and refined LUTHER B. ARNOLD, Jl.