RU2259432C1 - Oiling agent for wool fiber - Google Patents

Abstract

FIELD: textile industry.

SUBSTANCE: oiling agent for preparing emulsion for treatment of wool fiber contains 4.5-5.5% oleic acid, 0.8-1.0% triethanolamine, 7.0-8.0% "syntanol", 3.0-4.0% "stearoks-6", transformer oil (balancing amount), and bactericidal additive, namely thiourea/phosphorus trichloride/formalin interaction product neutralized with soda ash used in amount 6.0-8.0% relative to 100% of above-indicated composition.

EFFECT: enhanced bactericidal properties.

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Description

The invention relates to the field of protection against biodefeat. It can be used in the textile industry, namely in the processing of wool fiber.

One of the stages of wool processing in the textile industry is the oiling stage, which is carried out using special fluids - oiling agents in order to increase the adhesion between the fibers and to obtain a more complete roving. Oiling protects the fiber bundle from damage and facilitates the drawing of fibers.

From (Schönfeld N. Surfactants based on ethylene oxide. Translated from German. / Under the editorship of N.N. Lebedev. Ed. 2nd. - M .: Chemistry, 1982, - p. 488) a sizing agent is known worsted wool, including neutral oils (peanut) and fatty acids (oleic), water-soluble lubricants including, for example, ethoxylated fatty acids, alcohols and similar compounds are also described therein. In (application 19847497 Germany, application. 15.10.1998, publ. 20.04.2000) describes a sizing based on coconut oil acids or oil palm seeds, or a mixture of fatty acids of coconut oil and palm oil. In (U.S. Patent 5269950, Dec. 12/12/1991, publ. 12/14/1993), a sizing agent is provided which comprises mineral, animal or vegetable oil, an oxyalkylated higher alcohol or a polyhydric alcohol ester. The composition of sizing agents based on esters of polyhydric alcohols, in particular, the compound of the general formula R ¹ - Y - (X) _n - (CH ₂ ) _m - COOR ² , where R ¹ is alkyl C _1-23 ; R ² is alkyl C _1-23 ; n is 3-15; m is 1-6; Y is a group —O— or —S—; X is a group of the formula —C ₂ H ₄ O— and / or —C ₃ H ₆ O— is known from (US Pat. No. 5,314,718, filed January 21, 1993, publ. May 24, 1994), and the compound of the general formula R ¹ is O ( X) _n - CH ₂ - COOR ² , where R ¹ is alkyl C _1-23 ; R ² is alkyl C _1-23 ; n is 3-15; X is a group of the formula —C ₂ H ₄ O— and / or —C ₃ H ₆ O— is known from (U.S. Pat.

Emulsions of mineral oils and water-soluble derivatives of ethylene and propylene oxides are known to be used for oiling wool in hardware spinning. An example of a water-soluble sizing agent is the patented (application 10020669 Germany, application 27.04.2000, publ. 24.01.2002) a copolymer of ethylene and propylene oxide with a molecular weight of 200 - 10,000 g / mol, viscosity at 50 ° C 50-1000 mm ² / s and pour point less than minus 30 ° C, obtained by copolymerization in the presence of C ₄ -C ₁₂ alcohol with 4-12 OH groups as an initiator.

In (Kozlova O. V., Smirnova OK, Odintsova O. I., Melnikov B. N. // 1. Regional interuniversity conference "Actual problems of chemistry, chemical technology and chemical education": "Chemistry-96", Ivanovo, 22 -26 April 1996: Abstract (Ivanovo, 1996, pp. 174-175) describes compositions of derivatives of paraffins, synthetic fatty acids and new effective surface-active substances (surfactants) that act as emulsifiers and stabilizers of emulsifiers of lubricants. From (Schoenfeld N. Surfactants based on ethylene oxide. Translated from German. / Under the editorship of N.N. Lebedev. Ed. 2nd. - M .: Chemistry, 1982, - p. 488) the application is known anionic surfactants mixed with non-inogenic ones.

In (Kozlova O.V., Ilyina O.V., Odintsova O.I.// International scientific and technical conference "Problems of the development of low-waste resource-saving environmentally friendly technologies in the textile and light industry" (Progress-95), Ivanovo, October 31 - November 3, 1995: Abstracts - Ivanovo, 1995, pp. 136-137) describes the composition of lubricants based on paraffins, chloroparaffins, synthetic fatty acids. Emulsifiers and stabilizers of emulsifiers of lubricants are surfactants: neonols, phenoxol, as well as oleox, syntanols.

Common features of the above technical solutions with the invention are the use of an oil base, anionic surfactants in a mixture with nonionic surfactants (hydroxyethylated fatty acids, esters of polyhydric alcohols, etc.) as emulsifiers and stabilizers of emulsifiers.

The main disadvantages of emulsions known lubricants is their susceptibility to biological damage during storage and use. The use of an infected emulsifier of the sizing leads to rotting of the coat, the appearance of an unpleasant odor, a decrease in the strength of the thread and the throttle response to uniform dyeing. Wool treated with fresh emulsion at the aging stage before staining is also susceptible to bactericidal damage. These disadvantages are partially eliminated at the stage of washing the wool fiber before dyeing, which leads to increased material and energy costs.

The closest (prototype) to the proposed sizing by technical nature and the achieved effect is "Sizing B-73" (TU 6-14-999-80), which is a composition comprising mineral oil and anionic and nonionic emulsifiers - oleic acid, sulfonated castor oil, triethanolamine, Oleox-5, Xylan O (glycerol monooleate). Known sizing is characterized by the following physico-chemical properties:

pH value of 10% aqueous emulsion 7.0-8.0 stability of 10% aqueous emulsion, days is stable during the day mass fraction of moisture,%, no more 6.0 conditional viscosity (VU) at 20 ° С, no more 16 mass fraction of fatty substances,%, not less than 92.5

Working concentration (wt.%) Sizing in the emulsion during processing:

- wool in hardware production - up to 20;

- wool blends in worsted production - up to 5.

A disadvantage of the known sizing is its biodegradability.

The objective of the invention is:

- giving the sizing agent bactericidal properties;

- increase the shelf life of the prepared emulsion sizing;

- improving the quality of wool fiber during its processing using the proposed sizing.

The technical result of the claimed invention is to prevent biodegradability of the sizing and, accordingly, prepared on its basis emulsion, increasing the shelf life of the emulsion.

The specified technical result is achieved by introducing into the composition of the sizing agent, including oleic acid, triethanolamine, syntanol, stearox-6, transformer oil, in the following ratio, wt.%:

oleic acid 4,5-5,5 triethanolamine 0.8-1.0 syntanol 7.0-8.0 stearox-6 3.0-4.0 transformer oil rest

a bactericidal additive, which is a product of the interaction of thiocarbamide, phosphorus trichloride and formalin neutralized by caustic soda in an amount of 6.0-8.0 wt.% per 100 wt.% of the above composition.

A comparative analysis of the prototype and the proposed invention shows that the use of oleic acid, triethanolamine as components of an emulsifier, mineral oil base, surfactants to relieve static stress during fiber production is common.

The difference between the invention and the prototype is the use of a surfactant composition in the lubricant, including syntanol and stearox-6 (according to GOST 8980-75 - a mixture of polyoxyethylene glycol esters of stearic acid), transformer oil as a mineral oil base, a bactericidal additive, which is a product of the interaction of caustic soda neutralized thiocarbamide, phosphorus trichloride and formalin.

Oleic acid and triethanolamine are components of an emulsifier which, when reacted with each other (during the production of a lubricant) form an oleic acid triethanolamine ester of the following formula:

,

,

being an emulsifier. Sintanol and stearox-6 form a surfactant composition, which allows to reduce friction and fluffing of wool during fiber production, to soften the neck of woolen fabric. Transformer hydrocracking oil is the mineral oil base of the sizing, characterized by a low content of aromatic carbon (less than 1.5 wt.%) And a paraffin-naphthenic composition.

The possibility of implementing the invention, namely: obtaining a bactericidal additive and a sizing agent, as well as determining the bactericidal properties of a sizing agent and emulsions prepared using it, are shown in the following examples.

Example 1. Preparation of a sizing.

As a result of the implementation of the invention receive a sizing containing, wt.%:

oleic acid 5,0 triethanolamine 0.9 syntanol 7.5 stearox-6 3,5 transformer oil rest

which additionally includes a bactericidal additive, which is a product of the interaction of thiocarbamide, phosphorus trichloride and formalin, neutralized by caustic soda, in an amount of 7.0 wt.% per 100 wt.% of the above composition.

Below is a description of the components used.

1. Technical triethanolamine (TU 6-02-916-79):

- Formula - C ₆ H ₁₅ O ₃ N;

- Molecular mass - 149.19;

Name of indicator Norm Brand a Brand b Brand B 1. Appearance Transparent liquid, opalescence is allowed, color from yellow to light brown Transparent liquid, opalescence allowed, brown Brown to Dark Brown Fluid 2. Density at 20 ° C, in the range, g / cm ³ 1,095-1,124 1,095-1,135 1,095-1,135 3. Fractional composition: at a residual pressure of (2.7 ± 0.2) kPa or (20 ± 1.5) mmHg distilled,%: a) at temperatures up to 170 ° C, no more 14.5 1 Not regulated b) at a temperature of 170 to 225 ° C, not less than 82.0 80.0 80.0 c) residue after distillation, not more than 3,5 6.0 20,0

2. Technical oleic acid (GOST 7580-91):

- Formula - C ₁₇ H ₃₃ COOH;

- Molecular mass - 282.198;

Name of indicator Norm Color number, mg of iodine, no more 70 Mass fraction of fatty acids in anhydrous product, wt.% Not less 97.4 Mass fraction of unsaponifiable and unsaponifiable substances, wt.% No more 2,5 Iodine number, g iodine / 100 g - for brand B14, 85-105 - for the OM brand 90-105 Acid number, mg KOH / g 185-200 Saponification number, mg KOH / g 185-200

3. Sintanol ACSE-12 (TU 6-14-819-86)

Name of indicator Norm Appearance at 20 ° C Pasta from white to slightly yellow The color of the molten product in units of iodine scale, mg I / 100 cm ³ No more than 2 The activity index of hydrogen ions (pH) of an aqueous solution of the drug with a mass fraction of the main substance of 10%, within 6.0-8.0 The cloud point of the product solution with a mass fraction of the main substance of 1% in an aqueous solution of sodium chloride with a mass fraction of 5%, ° C within 65-70 Mass fraction of polyethylene glycols,%, no more 2,5 Mass fraction of substances extracted with hexane,%, no more fifteen

4. Stearox-6 - a mixture of polyoxyethylene glycol esters of stearic acid (GOST 8980-75).

Name of indicator Norm for the premium OKP 24 8324 0120 Appearance at (20 ± 2) ° С Cream-colored Vaseline mass The appearance of the molten product Viscous mass of light brown color without mechanical impurities The stability of the aqueous dispersion with a mass fraction of 1% Must withstand Saponification number, mg KOH / g 80-88 Mass fraction of ash,%, no more 0.5 Mass fraction of iron,%, no more 0.003 pH of an aqueous dispersion with a mass fraction of 1% 7.0-9.0 Mass fraction of moisture,%, no more 0.30

5. Transformer oil GK (TU 38. 1011025-85):

Name of indicator Norm 1 2 Kinematic viscosity, mm ² / s, not more than: - at 50 ° C nine - at minus 30 ° С 1200 Acid number, mg KOH / g oil, not more than 0.01 1 2 Flash point, determined in a closed crucible, ° С, not lower 135 Pour point, ° C, not higher minus 45 Color on the colorimeter CNT, units CNT, no more 1 Stability against oxidation (at 150 ° С, 14 h, oxygen consumption 50 ml / min): - mass of volatile low molecular weight acids, mg KOH / g, not more than; 0.04 - mass fraction of sediment,%, no more; 0.015 - acid number of oxidized oil, mg KOH / g, not more than 0.1 Dielectric loss tangent at 90 ° С,%, no more 0.5 Density at 20 ° С kg / m ³ , no more 895

6. Bactericidal additive: crystalline powder from slightly colored to white, readily soluble in water, insoluble in alcohols and hydrocarbons, has a melting range of 330-355 ° C and a bulk density of 0.75 g / cm ³ .

A method of obtaining a sizing is as follows:

1. The entire amount of transformer oil is introduced into the contactor-mixer, then, with constant stirring, the entire amount of oleic acid is added to the oil. The mixture is stirred for 1 hour at a temperature not exceeding 25 ° C. Subsequent operations are carried out with constant stirring.

2. In the resulting mixture gradually, in small portions, add the entire amount of triethanolamine (stirring for 2-3 hours). At this stage, the synthesis of an emulsifier - triethanolamine oleic acid soap proceeds.

3. Then, the temperature in the contactor-mixer is gradually increased (at a speed of 15-20 ° С per hour) to 50 ° С and first the whole amount of syntanol and then stearox-6 are introduced into the resulting solution of triethanolamine soap of oleic acid in transformer oil, and then stirred for three hours. At this stage, the formation of a surfactant composition occurs.

4. After all components are completely dissolved, a bactericidal additive is added to the mixture, and the resulting mixture is stirred for one hour.

The resulting sizing has the following physico-chemical properties:

pH value of 10% aqueous emulsion 7.0-8.0 stability of 10% aqueous emulsion, days is stable during the day mass fraction of moisture,%, no more 1,0 conditional viscosity (VU) at 30 ° С, no more 7.0 mass fraction of fatty substances,%, not less than 98.0

Working concentration (wt.%) Sizing in the emulsion during processing:

- wool in hardware production - up to 20;

- wool blends in worsted production - up to 10.

Example 2. Synthesis of a bactericidal additive.

A method of obtaining a bactericidal additive is as follows. 25 ml of a 70% (wt.) Solution of thiocarbamide are charged into a reaction flask with a stirrer and reflux condenser, heated to 50 ° C, 36 ml of phosphorus trichloride are added and kept for 15 minutes. After the specified time, neutralize with caustic soda to a pH of 6.0. Then injected with 40 ml of 37% (wt.) Formalin, incubated for 120 minutes at 40-50 ° C. After this, the mixture is unloaded, add 250 ml of a 15% (wt.) Solution of caustic soda.

The precipitated flocculent precipitate was filtered under vacuum and dried at room temperature to constant weight. As a result, 50 g of the product, a bactericidal additive, are obtained. The structure of the substance is not clearly established.

Example 3. Determination of the bactericidal properties of the sizing.

The bactericidal properties of the sizing obtained in Example 1 and emulsions prepared on its basis were carried out according to the method described in (cutting lubricants for metal cutting: Handbook / Under the general editorship of S.G. Entelis, E.M. Berliner. - 2nd ed., Revised and enlarged M: Mechanical Engineering, 1995, 496 p.). The experiments were carried out as follows. In one test tube, 9 ml of a contaminated second-hand 10% (w / w) emulsion of a lubricant containing no bactericidal additive is placed. In a second test tube, 9 ml of a 10% (w / w) oil emulsion containing a bactericidal additive was used. Then, 1.0 ml of indicator, 0.5% (wt.) Aqueous solution of 2,3,5-triphenyltetrazolium chloride (TTX), is added to both tubes. The contents of the tubes are thoroughly mixed, the tubes are placed in a thermostat and kept at a temperature of 30 ± 5 ° C for the time necessary for the appearance of a characteristic color in the tested emulsions (1-5 days). Visually assess the presence and intensity of the color of the emulsion and determine the microbiological damage score of the emulsion. As a result of the tests, it was found that after the trial period the emulsion prepared from a sizing agent without a bactericidal additive has a limit IV biodefeat score on a V-scale from 0 to IV, which indicates that the emulsion is unsuitable for further use. An emulsion prepared from a sizing agent with a bactericidal additive has a score of 0-1, i.e. This emulsion is suitable for operation for a long time.

The presented examples show the feasibility of the invention and the achievement of the claimed technical result.

Claims (1)

A sizing agent for preparing an emulsion for processing wool fiber, comprising oleic acid, triethanolamine, syntanol, stearox-6, transformer oil, characterized in that the sizing composition contains, in wt.%: oleic acid 4,5-5,5 triethanolamine 0.8-1.0 syntanol 7.0-8.0 stearox-6 3.0-4.0 transformer oil rest, In addition, a bactericidal additive is introduced, which is a product of the interaction of thiocarbamide, phosphorus trichloride and formalin neutralized with caustic soda in an amount of 6.0-8.0 wt.% per 100 wt.% of the above composition.