Active fabric softener composition

FIELD: chemistry.

SUBSTANCE: invention relates to active fabric softener compositions. Described is an active fabric softener composition which contains a) not less than 50 wt % bis-(2-hydroxypropyl)-dimethylammonium methylsulphate ester of a fatty acid, having molar ratio of fatty acid moieties to amine moieties ranging from 1.5 to 1.99, average chain length of fatty acid moieties ranging from 16 to 18 carbon atoms, and iodine number of fatty acid moieties calculated for a free fatty acid ranging from 0.5 to 50, and b) 0.5-5 wt % fatty acid. Also described is a method of producing the fabric softener composition.

EFFECT: good softening capacity, good stability when stored in an aqueous dispersion, the softener composition can be used and processed in a liquid state without adding a flammable solvent.

15 cl, 2 tbl, 19 ex

 

The present invention relates to an active compositions, fabric softener, high softening ability, good stability when stored in aqueous compositions that can be processed in aqueous compositions without the use of volatile solvents.

Quaternary ammonium salt containing two hydrophobic long chain hydrocarbon fragment, are widely used as active substances of fabric softener. Quaternary ammonium salts alkanolamines, esterified on average, two fragments of fatty acids in terms of one molecule, usually called Quaternary esters, largely replaces the previous Quaternary ammonium alkyl derivatives, due to their Biodegradability.

For use in the rinse cycle softener active composition of the softener must comply with different and sometimes contradictory requirements:

"she must have good softening ability from the viewpoint of softness to the touch and re-wetting the cloth,

"she must have good stability when stored in water dispersion with a small change in the viscosity of the dispersion, and

it should be suitable for use and processing in the liquid state.

Quaternary complex is haunted esters, which are widely used in industry and which are now standards for softening abilities are methyltrichlorosilane diesters of fatty acids and dimethyldiallylammonium diesters of fatty acids. However, aqueous dispersions of these active components of the fabric softener which has limited stability and long shelf life at temperatures above 40°C, usually lead to an unacceptable increase in the viscosity of the dispersion or deposition of the active component softener. In addition, these active components fabric softener impossible to use and process in water dispersion without added solvent due to high melting points and melt viscosities and limited thermal and hydrolytic stability of the active components of fabric softner. Therefore, they usually deliver and process with the addition of from 5 to 15 wt.% ethanol or isopropanol, which requires additional precautions due to the volatility and Flammability of the solvent.

In EP 0293955 A2 and EP 0302567 A2 discloses aqueous dispersions of fabric softener with high storage stability and a small change in viscosity during storage, and method for producing such dispersions. These compositions contain bis-(2-hydroxypropyl)-dial lemmonii salt diapir fatty acid as an active ingredient of fabric softener in the form of particles of submicron size. However, these dispersions requires processing of the active component fabric softener mixed with 5-50 wt.% monatomic C1-C4-alcohol. In the examples of bis-(2-hydroxypropyl)-dimethylammoniumchloride fluids palmitic acid is used as the active component of fabric softner and isopropanol is used as solvent.

In DE 2430140 C3 disclosed bis-(2-hydroxypropyl)-dialkylammonium salts of diesters of fatty acids, designed to obtain a liquid active ingredients of fabric softner. Example 2 disclosed the receipt of bis-(2-hydroxypropyl)-dimethylaminomethylphenol diapir fatty acids by the reaction of bis-(2-hydroxypropyl)-methylamino diapir fatty acids with medium chain length, part 19 to 20 carbon atoms, and containing 90 wt.% fragments of unsaturated fatty acids with respect to the number of moles to the number of moles of dimethylsulfate equal to 1:1.

In EP 1018541 A1 discloses a transparent composition of fabric softener containing Quaternary ester and alkoxycarbonyl phenol or branched C3-C6-alcohol as a solvent. Example 6 is disclosed a composition comprising a bis-(2-hydroxypropyl)-dimethylaminomethylene ester of fatty acids having a ratio of the number of moles of fragments of fatty acids to the quantities of the moles of amine fragments, 1.8, derived from fatty acids with medium chain length, part 18 carbon atoms, and iodine number of approximately 150. Upon receipt of this composition, as disclosed in the paragraph [0026], active Quaternary ester is treated with the addition of 10 wt.% isopropanol.

In WO 00/06678 revealed incompletely esterified Quaternary esters of branched alkanolamines for whom stated that they have low melting and good hydrolytic stability, and proposed to leave in the middle one hydroxy-group of alkanolamine neeterificirovannah. In example 50 disclosed bis-(2-hydroxypropyl)-dimethylaminomethylene a fatty acid ester, obtained by quaternization bis-(2-hydroxypropyl)-methylamino fatty acid ester having a ratio of the number of moles of fragments of fatty acids to the number of moles of amine fragments, is 1.26 derived from fatty acids having a chain length factor of 12 to 14 carbon atoms.

In DE 3608093 A1 discloses concentrated aqueous composition of fabric softener containing Quaternary ester with two acyl groups, fatty acid or its salt of the alkali metal in the number of 1/70 to 1/3 of the amount of the Quaternary complex of ether, and a combination of solvents, including water, shall glycerin and additional organic solvent with the full content, of 1/6 to twice the amount of the Quaternary complex of ether. Example 4 disclosed a composition comprising 45 wt.% bis-(2-hydroxypropyl)-dimethylaminomethylphenol diapir oleic acid, 1 wt.% sodium salt of tall oil fatty acid, 11.5 wt.% water, 11.5 wt.% glycerin, 17.5 wt.% 2-propanol, 6 wt.% propylene glycol and 3 wt.% dipropyleneglycol.

Active Quaternary esters disclosed in DE 2430140 C3, EP 1018541 A1 and WO 00/06678, have low melting, but have insufficient softening capacity due to the high degree of unsaturation fragments fatty acids and high content of component - Quaternary complex monoether. On the other hand, similar Quaternary esters derived from bis-(2-hydroxypropyl)-methylamine and having a low content of Quaternary complex monoether derived from fatty acids with a low degree of unsaturation, as disclosed in EP 302567 A2, provide the necessary softening ability, but have high melting points and melt viscosities and therefore for use and processing require the addition of solvent.

Therefore, the necessary active composition of fabric softener, which can be used to process without solvent without compromising stability when stored in water, d is spersed with little change in the viscosity of the dispersion.

According to the invention it was found that the active composition of fabric softener based on bis-(2-hydroxypropyl)-dimethylaminomethylphenol fatty acid ester derived from fatty acids with a specific chain length and a certain degree of unsaturation and with a certain ratio of the number of moles of fragments of fatty acids to the number of moles of amine fragments, which contain a certain amount of free fatty acids, provide a high softening ability and good stability when stored in an aqueous dispersion and at the same time they can be used and processed in the liquid state without the addition of volatile solvent.

Therefore, the present invention relates to active composition of fabric softener, containing not less than 50 wt.% bis-(2-hydroxypropyl)-dimethylaminomethylphenol fatty acid ester having a ratio of the number of moles of fragments of fatty acids to the number of moles of amine fragments equal to from 1.5 to 1.99, medium chain length fragments of fatty acids comprising from 16 to 18 carbon atoms, and iodine number for fragments of fatty acids, calculated for the free fatty acid is from 0.5 to 50 and from 0.5 to 5 wt.% fatty acid.

The present invention also relates to a method for obtaining such compositions, vkluchaya is from the reaction of bis-(2-hydroxypropyl)-methylamine fatty acid, with an average chain length equal to 16 to 18 carbon atoms, and iodine number equal to from 0.5 to 50, with respect to the number of moles of fatty acid to the number of moles of the amine is 1,51 to 2.1, with removal of water until the acid number of the reaction mixture will not be in the range from 1 to 10 mg KOH/g and subsequent reaction with dimethylsulfate when the ratio of the number of moles of dimethylsulfate to the number of moles of the amine, equal from 0.90 to 0.97 and preferably from 0.92 to 0.95, while the amine number of the reaction mixture will not be in the range of from 1 to 8 mg KOH/g

Active composition of fabric softener proposed in the present invention contains at least 50 wt.% bis-(2-hydroxypropyl)-dimethylaminomethylphenol ether fatty acids. The composition preferably contains from 85 to 99 wt.% the specified ether. According to the invention unexpectedly found that the use of methyl sulfate simultaneously leads to a lower melting temperature of the composition and greater stability against hydrolysis of the aqueous dispersion of the composition in comparison with the use of a chloride, used in EP 0293955 A2 and EP 0302567 A2.

Bis-(2-hydroxypropyl)-dimethylaminomethylene the fatty acid ester is a mixture of at least one diapir formula (CH3)2N+(CH2CH(CH3)OC(=O)R)2CH3OSO3is the -and at least one monoether formula (CH3)2N+(CH2CH(CH3)OH)(CH2CH(CH3)OC(=O)R)CH3OSOO3-in which R denotes a fragment of a hydrocarbon group of a fatty acid RCOO. Bis-(2-hydroxypropyl)-dimethylaminomethylene the fatty acid ester has a ratio of the number of moles of fragments of fatty acids to the number of moles of amine fragments equal to from 1.5 to 1.99 and preferably from 1.85 to 1.99. The specified molar ratio, it is important to simultaneously ensure good softening ability and a low melting point composition. The ratio of the numbers of moles in the range from 1.85 to 1.99, provides a high softening ability in the absence of anionic surfactants or at low concentrations of these surfactants. Therefore, the active composition of fabric softener with respect to the numbers of moles applicable to obtain a softener to the rinse cycle, intended to be used for washing in the Laundry, where linen for washing repeatedly washed after washing before adding a softener to the rinse cycle. The ratio of the numbers of moles in the range from 1.5 to less than 1,85, provides a high softening ability in the presence of anionic surfactant is of exist. Therefore, the active composition of fabric softener with respect to the numbers of moles applicable to obtain a softener to the rinse cycle, intended to be used for washing in the Laundry, when the softener to the rinse cycle is added to the water for washing immediately after washing.

Fragment of fatty acid bis-(2-hydroxyethyl)-dimethylaminomethylphenol fatty acid ester prepared from a mixture of fatty acids of the formula RCOOH, in which R is a hydrocarbon group. The hydrocarbon group may be branched or unbranched and is preferably unbranched.

Fragment of a fatty acid has an average chain length comprising from 16 to 18 carbon atoms, and iodine number, calculated for the free fatty acid is from 0.5 to 50. The average chain length is preferably from 16.5 to 17.8 carbon atoms. Preferably, if the fragment fatty acid has an iodine number equal to from 1.0 to 50, more preferably equal to from 2 to 50, more preferably equal to from 5 to 40, and most preferably equal to from 15 to 35. The average length of a chain is calculated based on the mass fraction of individual fatty acids in the mixture of fatty acids. For fatty acids with branched chain chain length is considered the longest consecutive chain of carbon atoms. Iodine number means the code in the TES in grams amount of iodine, spent on reaction with double bonds 100 g fatty acids, determined by the method of ISO 3961. To provide the necessary average chain length and the iodine number of the fragment fatty acids can be obtained from a mixture of fatty acids containing saturated and unsaturated fatty acids. Unsaturated fatty acids are preferably monounsaturated fatty acids. Bis-(2-hydroxypropyl)-dimethylaminomethylene the fatty acid ester preferably contains less than 6 wt.% polyunsaturated fragments of fatty acids. Examples of suitable saturated fatty acids are palmitic acid and stearic acid. Examples of suitable monounsaturated fatty acids are oleic acid and elaidic acid. The ratio of CIS-TRANS-double bonds in unsaturated fragments of the fatty acid is preferably more than 55:45, and more preferably 65:35. The content of polyunsaturated fragments of fatty acids can be reduced by selective hydrogenation, which is a hydrogenation, which selectively hereroense one double bond substructure-CH=CH-CH2-CH=CH-, but not the double bond in monounsaturated hydrocarbon groups. Set the average chain length and iodine number necessary to simultaneously ensure a high softening methods for the activity and a low melting point composition. If the average chain length is less than 16 carbon atoms or an iodine number greater than 50, then softening ability is poor and the melting temperature of the composition may be too high if the average chain length is more than 18 carbon atoms.

Fragment of fatty acids can be obtained from fatty acids of natural or synthetic origin and preferably derived from fatty acids of natural origin, most preferably from fatty acids of vegetable origin. The necessary iodine number can be achieved by use of a mixture of fatty acids of natural origin, which already has such a iodine number, such as tall oil fatty acid. Alternatively, the necessary iodine number can be achieved by partial hydrogenation of a mixture of fatty acids or mixtures of triglycerides with greater iodine number. In another and preferred embodiment, the necessary iodine number provide by mixing a mixture of fatty acids with greater iodine number, with a mixture of saturated fatty acids. A mixture of saturated fatty acids can be obtained by hydrogenation of a mixture of fatty acids containing unsaturated fatty acids, or from gidrirovannoe mixture of triglycerides, such as gidrirovannoe plant is aslo.

Active composition of fabric softener proposed in the present invention, further comprises from 0.5 to 5 wt.% fatty acids in addition to bis-(2-hydroxypropyl)-dimethylaminomethylphenol ether fatty acids. The composition preferably contains from 1 to 5% and more preferably from 2 to 5 wt.% fatty acid. The fatty acid may be in the form of free fatty acids or as salts of fatty acids with equationsofinite bis-(2-hydroxypropyl)-metilenovyi esters. Active composition softener fabric preferably contains a mixture of fatty acids, which preferably has a natural origin, and most preferably of vegetable origin. In the most preferred embodiment, fragments of fatty acid bis-(2-hydroxypropyl)-dimethylaminomethylphenol fatty acid ester formed from the same mix of fatty acids contained in the composition in amounts of 0.5 to 5 wt.%. The specified number of fatty acids is important to ensure a low melting point composition without compromising stability when stored in water dispersion. If the composition contains less than 0.5 wt.% fatty acids, the melting temperature of the composition may become too high, while the content of more than 5 wt.% fatty acids in HDMI is tion will result in that the aqueous dispersion obtained from the composition, will have unacceptably high viscosities and low stability of the dispersion. By maintaining the content of fatty acids in the stated range can be obtained composition proposed in the present invention, which will have a low viscosity without the use of any solvent or diluent. Such compositions allow to obtain a dispersion softener to the rinse cycle the water does not contain solvent or containing the minimum amount of solvent.

Active composition of fabric softener proposed in the present invention, preferably contains 2 wt.% and more preferably less than 0.5 wt.% water. Composition having such a low water content, have improved storage stability in the molten state and therefore they can be stored and transported as liquids without compromising product quality. Compositions containing more water, have a much greater viscosity of the melt and therefore they are difficult to process in the aqueous dispersion.

Active composition of fabric softener proposed in the present invention, preferably contains less than 10 wt.% and more preferably less than 1 wt.% solvents having a flash point equal to below 20°C.

In a preferred is ariante implementation of the active composition of fabric softener, proposed in this invention contains up to 9.9 wt.% and preferably up to 5 wt.% at least one solvent selected from the group comprising glycerine, ethylene glycol, propylene glycol, dipropyleneglycol and C1-C4alkalemia monoether of ethylene glycol, propylene glycol and dipropyleneglycol. Examples of suitable C1-C4-alilovic of monoamino glycol is 2-methoxyethanol, 2-ethoxyethanol, 2-butoxyethanol, 1-methoxy-2-propanol, onomatology broadcast dipropyleneglycol and monobutyl broadcast dipropyleneglycol. In this embodiment, the compositions have the advantage that the low viscosity of the melt and close to Newtonian rheological characteristics of the melt, i.e. the viscosity varies little with changing shear forces.

In another preferred embodiment, the active composition of fabric softener proposed in the present invention contains from 2 to 8 wt.% the triglyceride fatty acids with medium chain length fragments of the fatty acid constituting from 10 to 14 carbon atoms, and iodine number, calculated for the free fatty acid equal to from 0 to 15. In this embodiment, the compositions also have the advantage that the low viscosity of the melt and close to Newtonian rheological x is the new melt, i.e. the viscosity varies little with changing shear forces.

In a preferred alternative embodiment, the amount of solvent contained in the active composition of fabric softener is less than 5 wt.% and more preferably less than 1 wt.%. In this embodiment, the composition can be further processed in the molten state and to obtain a dispersion containing no aqueous solvent.

In addition to bis-(2-hydroxypropyl)-dimethylaminomethylphenol ether, fatty acid, fatty acid and optionally a solvent, the active composition of fabric softener proposed in the present invention may preferably further comprise from 1.5 to 9 wt.% bis-(2-hydroxypropyl)-methylamino ester of a fatty acid containing the same fragments of fatty acids as bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acids. Bis-(2-hydroxypropyl)-metaluminous the fatty acid ester preferably is a mixture of at least one diapir formula (CH3)N(CH2CH(CH3)OS(=O)R)2and at least one monoether formula (CH3)N(CH2CH(CH3)IT)(CH2CH(CH3)OS(=O)R). At least part of bis-(2-hydroxypropyl)-methylamino fatty acid ester is contained in the form of a salt with a fatty acid Akti is Noah composition of fabric softener. Such salts have the structure HN+(CH3)(CH2CH(CH3)OC(=O)R)2RCOO-or HN+(CH3)(CH2CH(CH3)OH)(CH2CH(CH3)OC(=O)R)RCOO-. The presence of bis-(2-hydroxypropyl)-methylamino ether fatty acids in a given number further reduces the melting temperature of the composition without compromising mitigation and stability during storage in water dispersion.

Active composition of fabric softener proposed in the present invention can additionally contain a small amount (2-hydroxypropyl)-(1-methyl-2-hydroxyethyl)-dimethylaminomethylene esters of fatty acids, bis-(1-methyl-2-hydroxyethyl)-dimethylaminomethylene esters of fatty acid, (2-hydroxypropyl)-(1-methyl-2-hydroxyethyl)-methylamino esters of fatty acids and bis-(1-methyl-2-hydroxyethyl)-methylamino esters of fatty acids.

Active composition of fabric softener proposed in the present invention, can be obtained by mixing bis-(2-hydroxypropyl)-dimethylaminomethylphenol of fatty acid ester, fatty acid, and optional components such as a solvent or bis-(2-hydroxypropyl)-metaluminous ether fatty acids.

Active composition of fabric softener proposed in the present invention, preferably obtained by the method proposed in the us is oasam the invention, comprising the reaction of bis-(2-hydroxypropyl)-methylamine fatty acid having an average chain length equal to 16 to 18 carbon atoms, and iodine number equal to from 0.5 to 50, with respect to the number of moles of fatty acid to the number of moles of the amine is 1,51 to 2.1, with removal of water until the acid number of the reaction mixture will not be in the range from 1 to 10 mg KOH/g and subsequent reaction with dimethylsulfate when the ratio of the number of moles of dimethylsulfate to the number of moles of the amine, equal from 0.90 to 0.97 and preferably from 0.92 to 0.95, while the amine number of the reaction mixture will not be in the range of from 1 to 8 mg KOH/g

In the first stage of the method proposed in the present invention, bis-(2-hydroxypropyl)-methylamine is introduced into the reaction with the fatty acid at the ratio of the number of moles of fatty acid to the number of moles of the amine is 1,51 to 2.1, preferably of 1.86 to 2.1, with removal of water. The reaction is preferably carried out at a temperature equal to from 160 to 220°C. the Water is preferably removed from the reaction mixture using distillation. During the reaction the pressure is preferably reduced from ambient pressure up to being in the range from 100 to 5 mbar to improve the removal of water. The first stage can be done in the presence of a catalyst-acid, which is preferably used in amounts which, comprising from 0.05 to 0.2 wt.%. Suitable catalysts are acids are methansulfonate acid, p-toluensulfonate acid and gipofosforna acid. The reaction is carried out until the acid number of the reaction mixture will not be in the range from 1 to 10 mg KOH/g Acid number is determined by titration with a standardized solution of alkali in accordance with ISO 660 and calculated as the number of milligrams of KOH per 1 g of the sample. Then the reaction can be stopped by cooling to a temperature below 80°C, to prevent further reaction of the fatty acid and save unreacted fatty acid to provide an adequate amount of fatty acids in the final product.

In the second stage of the method proposed in the present invention, the reaction mixture in the first stage is introduced into the reaction dimethylsulfate when the ratio of the number of moles of dimethylsulfate to the number of moles of the amine, equal from 0.90 to 0.97 and preferably from 0.92 to 0.95. The reaction is preferably carried out at a temperature equal to from 60 to 100°C. the Reaction is carried out until the amine number of the reaction mixture will not be in the range of from 1 to 8 mg KOH/g amine Full number is determined by non-aqueous titration with perchloric acid according to the method Tf 2A-64 American society of chemists of petroleum and hope in the form of the number is TBA milligrams KOH per 1 g of the sample.

The method proposed in the present invention, has the advantage of giving the active composition of fabric softener proposed in the present invention, without the need for any stage in addition to the stages necessary to obtain bis-(2-hydroxypropyl)-dimethylaminomethylphenol ether fatty acids. This advantage is provided by appropriate selection of the ratio of the number of moles of fatty acid to the number of moles of the amine and carrying out the reaction of fatty acid with the amine in a given range of acid numbers, ensuring that a certain percentage of unreacted fatty acid.

The present invention is illustrated in the following examples, which are not intended for any limitation of the scope of the present invention.

Examples

General provisions

Table 1 shows the sources of the distribution chain fatty acids in length and iodine number of fatty acids A-G, which are used in the examples. Distribution chain fatty acids by lengths were determined using gas chromatography after receiving the derived fatty acids in the form of a methyl ester.

Active composition of fabric softener received by the following General method, if in some examples, unless otherwise noted. Fatty acid with 0.2 wt.% 50 wt.% hypophosphorous sour the s was placed in the reactor with electric heating, equipped with thermometer, mechanical stirrer and a distillation column, and with stirring was added bis-(2-hydroxypropyl)-methylamine. The resulting mixture with stirring, they were heated to 200°C and held at this temperature for 4 h under ambient pressure, fending off the water using a distillation column. Then the pressure was reduced to 10 mbar and the mixture was additionally stirred at 200°C, water was removed by a vacuum pump within the time specified in the specific example, while you have not installed the required acid number of the reaction mixture. Then the mixture was cooled to 75°C., was added dimethylsulfate and the resulting mixture was stirred for 2 h at a temperature equal to 70 to 90°C.

The content of free amine, amine salts and fatty acids in the active composition of fabric softener was determined using the non-aqueous potentiometric titration with tetrabutylammonium after adding an excess of HCl in 2-propanol.

C18 (3)
Table 1
The sources of the distribution chain fatty acids in length and iodine number of fatty acids
Fatty acidABC
SourceTall oil*Tall oil, partially gidrirovannoeRapeseed oil
C12 (0)
C14 (0)2,1
C15 (0)0,4
C16 (0)0,727,93,2
C16 (1)0,7
C17 (0)0,21,1
C18 (0)1,848,11,0
C18 (1)29,315,117,1
C18 (2)46,30,9a 12.7
0,97,3
C20 (0)0,20,90,7
C20 (1)0,47,9
C22 (0)0,7
C22 (1)45,9
C22 (2)0,7
C24 (0)0,2
C24 (1)0,8
The average chain length18,0the 17.320,1
Iodine number15020102

CX(y) denotes the linear fatty acid containing x carbon atoms which have double bonds.

* 20% of fatty acids was impossible, omelet and analyze.

Table 1 (continued)
Fatty acidDEFG
SourcePlant mixCoconut oil, gidrirovannoePlant mix, partially gidrirovannyVegetable mixture, gidrirovanny
C12 (0)46,4
C14 (0)0,253,60,82,6
C16 (0)19,245,346,4
C16 (1)0,5
C18 (0)of 21.2 the 13.4to 49.3
C18 (1)47,637,2
C18 (2)7,91,9

Fatty acidDEFG
SourcePlant mixCoconut oil, gidrirovannoePlant mix, partially gidrirovannyVegetable mixture, gidrirovanny
C18 (3)
C20 (0)0,21,9
C20 (1)0,3
C22 (0)0,2
C22 (1)
C22 (2)
C24 (0)
C24 (1)
The average chain length17,613,117,1of 17.0
Iodine number610,1370,7

The contents of fractions monoether and diapir in bis-(2-hydroxypropyl)-dimethylaminomethylphenol ether fatty acid was determined using HPLC (high performance liquid chromatography (column Waters Spherisorb SCX, the eluent methanol buffer of formic acid with triethylamine, detection in the infrared region).

The melting temperature was determined by capillary method, as the upper boundary values of the temperature in the melting range with the use of heat at a rate of 1°C/min the Samples were kondicionirovanie by melting the composition, homogenization of the melt, rapid solidification of the melt by pouring onto a cold metal plate and cooling rapidly solidified melt at -16°C for at least 4 h, followed by its transfer to the capillary to determine the melting temperature.

The melt viscosity was measured at 70°C by using a StressTech rheometer, manufactured by the firm REOLOGICA® instruments, using parallel plates with a size of 40 mm, the distance between the plates is equal to 0.5 m, and shear rates of 1, 10 and 100 s-1.

The storage stability was determined for 10 wt.% aqueous dispersions of the active compositions, fabric softener, which were stored for 6 weeks at 50°C in sealed glass vials. Dispersion was obtained by pre-dispersing a melt of the active composition of fabric softener, heated to the temperature at 5-10°C higher than the melting point of 0.05 wt.% aqueous HCl solution pre-heated at 5°C below the melting temperature of the composition, using a reactor IKA Super Dispax-Reactor® SD 41 operating at 8000 min" 1. Then under stirring was added a 25 wt.% an aqueous solution of CaCl and received the concentration of CaCl2equal to 0.025 wt.%. Acid number of the dispersions was determined before and after storage using acid-base titration by KOH or NaOH and led as the number of milligrams of KOH per 1 g of dispersion. The viscosity of the dispersions before and after storage was determined at 20°C using a Brookfield viscometer using spindle No. 1 for viscosities equal to 100 MPa·s, and spindle No. 2 for viscosities greater than 100 MPa·S.

Softening ability of the active composition of fabric softener was determined using the tactile test conducted by the test team using samples made of cotton towels treated with the aqueous dispersion composition. The pieces are made of cotton Terry towels size 80×50 cm double-washed effective powder detergent, washed twice and finally was wrung out, hung in the air and dried. Samples of 10 wt.% aqueous dispersions of the active compositions, fabric softener, prepared as described above was diluted with cold tap water and received 2 l of a solution for rinsing, containing 0.025 wt.% active composition of fabric softener. The washed pieces are made of cotton towels immersed in this solution for rinsing for 10 min, timely, were hung on the air and were dried at ambient temperature. Then the processed pieces made from cotton towels cut into 10 equal pieces 16×25 cm, which was distributed in a group of 9 test, which evaluated the softness on a scale ranging from 0 for hard and unpleasant to the touch for up to 5 soft and pleasant to the touch fabric. Indicators of softness in these examples are the sum of the 9 selected indicators and therefore ranges from 0 to 45. Using repeated comparative experiments it was determined that the difference of the indices of softness in excess of 4, was statistically significant.

Example 1 (comparative example corresponds to the component A5 in EP 1018541 A1)

644 g (of 2.25 mol) Fatty acids have atrificial using 182,5 g (1.25 mol) of bis-(2-hydroxypropyl)-methylamine at 190°C for 8 h the reaction under reduced pressure until the acid number of the reaction mixture does not become equal to 0.6 mg KOH/g, the Obtained mixture was introduced into a reaction with 151 g (1,20 mole) of dimethylsulfate at 60°C. the Obtained active composition of fabric softener was a brownish viscous liquid, containing 0.015 mmol/g (0.5 wt.%) fatty acids and 0,070 mmol/g aquatinting amine (0,041 mmol/g free amine and 0,029 mmol/g protonated amine). Analysis by HPLC showed that bis-(2-hydroxypropyl)-d is methylaminoethylcarbonyl ether fatty acid contains 8.2% of monoether and 91.8% of diapir (ratio of peak areas in %).

The composition has a melt viscosity equal to 685 MPa·s at a shear rate equal to 1-1, 488 MPa·s at 10-1and 431 MPa·s at 100 s1.

10% Aqueous dispersion has an acid number equal to 0.6 mg KOH/g, and a viscosity equal to 34 MPa·s, to storage and acid number equal to 1.2 mg KOH/g, and a viscosity equal to 265 MPa·s, after storage for 6 weeks at 50°C.

Figure softness using the composition equal to 12.

Example 2

Repeating example 1 using 954 g (3,49 mol) fatty acid, 283 g (1,94 mole) bis-(2-hydroxypropyl)-methylamine and 235 g (1,86 mole) of dimethylsulfate. Received active composition softener fabric was a white solid having a melting point equal to 42°C, containing 0.025 mmol/g (0.7 wt.%) fatty acids and 0,059 mmol/g aquatinting amine (0,033 mmol/g free amine and was 0.026 mmol/g protonated amine). Analysis by HPLC showed that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 8.8% of monoether and 91.2% of diapir (ratio of peak areas in %).

The composition has a melt viscosity equal 47200 MPa·s at a shear rate equal to 1-1, 9880 MPa·s at 10-1and 2960 MPa·s at 100 s-1.

10% Aqueous dispersion has an acid number of 0.5 mg KOH/g, and a viscosity of 18 MPa·s, to keep the value and acid number, equal to 1.1 mg KOH/g, and a viscosity of 18 MPa·s, after storage for 6 weeks at 50°C. the Rate of softness using the composition is equal to 32.

Example 3 (comparative example corresponds to example 2 of DE 2430140 C3)

744,5 g (2,38 mol) Fatty acid C was atrificial using 174,1 g (1,19 mole) bis-(2-hydroxypropyl)-methylamine for 15 h the reaction under reduced pressure until the acid number of the reaction mixture does not become equal to 1.5 mg KOH/g, the Obtained mixture was introduced into a reaction with 142,5 g (1,13 mole) of dimethylsulfate within 4 hours Received active composition of fabric softener was a yellowish gel to 0.032 mmol/g (1.0 wt.%) fatty acids and 0,113 mmol/g aquatinting amine (0,042 mmol/g free amine and 0,071 mmol/g protonated amine). The number of monoether and diapir in bis-(2-hydroxypropyl)-dimethylaminomethylphenol the fatty acid ester can be determined by analysis using HPLC.

The composition has a melt viscosity equal to 561 MPa·s at a shear rate equal to 1-1, 535 MPa·s at 10-1and 469 MPa·s at 100 s-1.

10 wt.% Aqueous dispersion obtained with the use of 0.025 wt.% CaCl2was very viscous. Therefore, the variance for stability studies were prepared using double the amount of CaCl2i.e. 0.1 wt.% CaCl2. The variance is Bladet acid number, equal to 0.7 mg KOH/g, and a viscosity equal to 160 MPa·s, to storage and acid number equal to 1.4 mg KOH/g, and a viscosity equal to 270 MPa·s, after storage for 6 weeks at 50°C.

Figure softness using the composition equal to 24.

Example 4

Repeating example 3 using 948 g (3,47 mol) fatty acid, 253,4 g (1,735 mole) bis-(2-hydroxypropyl)-methylamine and 208 g (of 1.65 mol) of dimethylsulfate for 15 h the reaction under reduced pressure until the acid number of the reaction mixture does not become equal to 1.4 mg KOH/g Obtained active composition softener fabric was a white solid having a melting point equal to 43°C, containing to 0.032 mmol/g (0.9 wt.%) fatty acids and 0,073 mmol/g aquatinting amine (0,043 mmol/g free amine and being 0.030 mmol/g protonated amine). Analysis by HPLC showed that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 3.1% of monoether and 96.9% of diapir (ratio of peak areas in %).

The composition has a melt viscosity equal 36200 MPa·s at a shear rate equal to 1-1, 7440 MPa·s at 10-1and 2160 MPa·s at 100 s-1.

10% Aqueous dispersion has an acid number equal to 0.6 mg KOH/g, and a viscosity equal to 16 MPa·s, to storage and acid number equal to 1.3 mg KOH/g, and a viscosity of 18 MPa·s, POS is f storage for 6 weeks at 50°C.

Figure softness using the composition is equal to 31.

Examples 1 and 4 and comparative examples 2 and 3 clearly show that the active composition of fabric softener proposed in the present invention, provide a much better softening ability from the point of view of the feeling of softness and better stability during storage 10% aqueous dispersion compared with the active compositions, fabric softener, known from EP 1018541 A1 and DE 2430140 C3.

Example 5

2780 g (10,18 mol) fatty acid was atrificial with 783 g (are 5.36 mol) bis-(2-hydroxypropyl)-methylamine for 3 h the reaction under reduced pressure until the acid number of the reaction mixture does not become equal to 5.2 mg KOH/g, the Obtained mixture was introduced into a reaction with 642 g (5,10 mole) of dimethylsulfate. Received active composition softener fabric was a white solid having a melting point equal to 41°C, containing 0.075 mmol/g (2.2 wt.%) fatty acids and 0,123 mmol/g aquatinting amine (0,068 mmol/g free amine and by 0.055 mmol/g protonated amine). Analysis by HPLC showed that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 5.5% monoether 94.5% diapir (ratio of peak areas in %). The composition has a melt viscosity equal 2360 MPa·s at a shear rate equal to 1-1, 190 MPa·s at 10 -1and 619 MPa·s at 100 s-1.

10% Aqueous dispersion has an acid number equal to 0.8 mg KOH/g, and a viscosity equal to 28 MPa·s, to storage and acid number equal to 2.8 mg KOH/g, and a viscosity of 12 MPa·s, after storage for 6 weeks at 50°C.

Figure softness using the composition is equal to 35.

Example 6

1365 g (5.0 mol) Fatty acid was atrificial using 384,2 g (2,63 mole) bis-(2-hydroxypropyl)-methylamine for 14 h the reaction under reduced pressure until the acid number of the reaction mixture does not become equal to 1.3 mg KOH/g, the Obtained mixture was introduced into a reaction with 315 g (2.5 mol) of dimethylsulfate. Received active composition softener fabric was a white solid having a melting point equal to 43°C, containing 0.025 mmol/g (0.7 wt.%) fatty acids and 0,113 mmol/g aquatinting Amin (of 0.081 mmol/g free amine and to 0.032 mmol/g protonated amine). Analysis by HPLC showed that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 5.7% monoether and 94.3% of diapir (ratio of peak areas in %). The composition has a melt viscosity equal 16200 MPa·s at a shear rate equal to 1-1, 4970 MPa·s at 10-1and 1530 MPa·s at 100 s-1.

10% Aqueous dispersion has an acid number of 0.5 mg KOH/g, and visco is thew, equal to 19 MPa·s, to storage and acid number equal to 1.9 mg KOH/g, and a viscosity equal to 13 MPa·s, after storage for 6 weeks at 50°C.

Figure softness using the composition is equal to 32.

Example 7

Stage of esterification of example 6 was repeated and 1021 g of the obtained reaction mixture was mixed with 45 g of fatty acids B. the resulting mixture was brought into reaction with 193 g (1,53 mole) of dimethylsulfate. Received active composition softener fabric was a white solid having a melting point equal to 41°C, containing 0,151 mmol/g (4,15 wt.%) fatty acids and rate £ 0.162 mmol/g aquatinting amine (0,070 mmol/g free amine and 0,092 mmol/g protonated amine). Analysis by HPLC showed that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 5.7% monoether and 94.3% of diapir (ratio of peak areas in %).

The composition has a melt viscosity equal 842 MPa·s at a shear rate equal to 1-1, 663 MPa·s at 10-1and 619 MPa·s at 100 s-1.

10% Aqueous dispersion has an acid number equal to 1.3 mg KOH/g, and a viscosity equal to 23 MPa·s, to storage and acid number equal to 3.9 mg KOH/g, and a viscosity of 8 MPa·s, after storage for 6 weeks at 50°C.

Figure softness using the composition is equal to 31. Examples 5-7 show that h is about the presence of fatty acids in the active compositions, fabric softener, proposed in the present invention, contributes to the low melt viscosity of the composition, provides a more near-Newtonian rheological properties of molten and has no adverse effect on the viscosity of the water dispersion of the composition during storage.

Example 8 (comparative, large iodine number)

970 g (3.5 mol) Fatty acids D was atrificial with 287 g (1,84 mole) bis-(2-hydroxypropyl)-methylamine for 3 h the reaction under reduced pressure until the acid number of the reaction mixture does not become equal to 5.6 mg KOH/g, the Obtained mixture was introduced into a reaction with 221 g (about 1.75 mole) of dimethylsulfate. Received active composition of fabric softener was a yellow viscous liquid containing 0,054 mmol/g (1.6 wt.%) fatty acids and 0,129 mmol/g aquatinting amine (0,068 mmol/g free amine and 0.061 mmol/g protonated amine). Analysis by HPLC showed that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 6.6% of monoether and 93.4% of diapir (ratio of peak areas in %).

The composition has a melt viscosity equal to 581 MPa·s at a shear rate equal to 1-1, 538 MPa·s at 10-1and 480 MPa·s at 100 s-1.

10% Aqueous dispersion has an acid number equal to 0.9 mg KOH/g, and a viscosity equal to 40 MPa·s, to storage and acid is Islom, equal to 2.6 mg KOH/g, and a viscosity equal to 36 MPa·s, after storage for 6 weeks at 50°C

Figure softness using the composition is equal to 23.

Example 8 shows that the active composition of fabric softener, which contains fragments of the fatty acid Quaternary ammonium salt with iodine number higher than that claimed, does not provide the same high softening ability, as an active composition of fabric softener proposed in the present invention.

Example 9 (comparative, shorter average chain length)

1125 (a 5.25 mol) Fatty acid E was atrificial with 403 g (was 2.76 mol) bis-(2-hydroxypropyl)-methylamine for 2 h the reaction under reduced pressure until the acid number of the reaction mixture does not become equal to 4.1 mg KOH/g, the Obtained mixture was introduced into a reaction with 330 g (2,62 mole) of dimethylsulfate. Received active composition softener fabric was a white gel containing 0,049 mmol/g (1.1 wt.%) fatty acids and 0,122 mmol/g aquatinting amine (0.079 in mmol/g of free amine and 0,043 mmol/g protonated amine). Analysis by HPLC showed that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 3.2% of monoether and 96.8% of diapir (ratio of peak areas in %).

The composition has a melt viscosity equal to 552 MPa·s when karasti shift, equal to 1-1, 550 MPa·s at 10-1and 497 MPa·s at 100 s-1.

10% Aqueous dispersion has an acid number equal to 0.8 mg KOH/g, and a viscosity of 30 MPa·s, to storage and acid number equal to 2.5 mg KOH/g, and a viscosity equal to 79 MPa·s, after storage for 6 weeks at 50°C.

Figure softness using the composition is equal to 16.

Example 9 shows that the active composition of fabric softener, which contains fragments of the fatty acid Quaternary ammonium salt having an average chain length that is less than stated, does not provide the same high softening ability, as an active composition of fabric softener proposed in the present invention.

Example 10

1032 g (of 3.78 mol) Fatty acid was atrificial using 313,3 g (2,16 mole) bis-(2-hydroxypropyl)-methylamine for 2 h the reaction under reduced pressure until the acid number of the reaction mixture does not become equal to 4.6 mg KOH/g, the Obtained mixture was introduced into a reaction with 258,8 g (2.05 mol) of dimethylsulfate. Received active composition softener fabric was a white solid having a melting point equal to 41°C, containing 0,047 mmol/g (1.3 wt.%) fatty acids and 0,134 mmol/g aquatinting amine (0,076 mmol/g free amine and 0,058 mmol/g protonated amine). Analysis by HPLC pok is provided, what bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 16.6%) of monoether and 83.4% of diapir (ratio of peak areas in %).

The composition has a melt viscosity equal 27100 MPa·s at a shear rate equal to 1-1, 6040 MPa·s at 10-1and 1870 MPa·s at 100 s-1.

10% Aqueous dispersion has an acid number equal to 0.9 mg KOH/g, and a viscosity equal to 19 MPa·s, to storage and acid number equal to 2.5 mg KOH/g, and a viscosity equal to 13 MPa·s, after storage for 6 weeks at 50°C.

Figure softness using the composition is equal to 27.

Example 10 shows that the active composition of fabric softener, which has a ratio of the number of moles of fragments of fatty acids to the number of moles of amine fragments smaller than stated, does not provide the same high softening ability, as an active composition of fabric softener proposed in the present invention.

Example 11

919 g (3,37 mol) Fatty acid was atrificial using 245,7 g (1,68 mole) bis-(2-hydroxypropyl)-methylamine within 7 h of reaction under reduced pressure until the acid number of the reaction mixture does not become equal to 5.5 mg KOH/g, the Obtained mixture was introduced into a reaction with 201,3 g (1,60 mole) of dimethylsulfate. Received active composition softener fabric was a white solid is emesto, having a melting point equal to 43°C, containing 0,076 mmol/g (2.2 wt.%) fatty acids and 0,141 mmol/g aquatinting amine (0,084 mmol/g free amine and 0,057 mmol/g protonated amine). Analysis by HPLC showed that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 0.9% monoether and 99,1% diapir (ratio of peak areas in %).

The composition has a melt viscosity equal to 1510 MPa·s at a shear rate equal to 1-1, 687 MPa·s at 10-1and 553 MPa·s at 100 s-1. 10% Aqueous dispersion has an acid number equal to 0.9 mg KOH/g, and a viscosity equal to 31 MPa·s, to storage and acid number equal to 3.3 mg KOH/g, and a viscosity of 12 MPa·s, after storage for 6 weeks at 50°C.

Figure softness using the composition is equal to 31.

Example 12

4823 g (17,68 mol) Fatty acid F was atrificial using 1337,4 g (9,16 mole) bis-(2-hydroxypropyl)-methylamine for 5 h reaction at ambient pressure and within 5 h of reaction under reduced pressure until the acid number of the reaction mixture does not become equal to 4.6 mg KOH/g, the Obtained mixture was introduced into a reaction with 1096,5 g (8,70 mole) of dimethylsulfate. Received active composition softener fabric was a white solid having a melting point equal to 38°C, with whom containing a series of 0,069 mmol/g (2.0 wt.%) fatty acids and 0,130 mmol/g aquatinting amine (0,071 mmol/g free amine and 0,059 mmol/g protonated amine). Analysis by HPLC showed that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 5.9% monoether and 94,1% diapir (ratio of peak areas in %).

The composition has a melt viscosity equal to 592 MPa·s at a shear rate equal to 1-1, 610 MPa·s at 10-1and 552 MPa·s at 100 s-1.

Figure softness using the composition is equal to 38.

Example 13

4088 g (to 14.9 mol) Fatty acids G was atrificial using 1129,5 g (7,74 mole) bis-(2-hydroxypropyl)-methylamine for 4 h the reaction under reduced pressure until the acid number of the reaction mixture does not become equal to 3.7 mg KOH/g, the Obtained mixture was introduced into a reaction with 926,5 g (7,4 mole) of dimethylsulfate. Received active composition softener fabric was a white solid having a melting point equal to 52°C, containing of 0.066 mmol/g (1.9 wt.%) fatty acids and 0,128 mmol/g aquatinting amine (0,073 mmol/g free amine and by 0.055 mmol/g protonated amine). Analysis by HPLC showed that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 6.8% monoether and 93.2% of diapir (ratio of peak areas in %).

The composition has a melt viscosity equal 34700 MPa·s at a shear rate equal to 1-1, 8100 MPa·s at 10-1and 2630 MPa·s at 100 sup> -1.

Figure softness using the composition is equal to 38.

Example 14

2520,4 g (9,23 mol) Fatty acid was atrificial using 692,5 g (4,75 mole) bis-(2-hydroxypropyl)-methylamine for 5 h the reaction under reduced pressure until the acid number of the reaction mixture does not become equal to 6.1 mg KOH/g, the Obtained mixture was introduced into a reaction with 568,6 g (4,51 mole) of dimethylsulfate for 1 h and Then added 180,8 g dipropyleneglycol and the mixture is homogenized by stirring. Received active composition softener fabric was a white solid having a melting point equal to 40°C, containing 0,083 mmol/g (2.4 wt.%) fatty acids and 0.119 mmol/g aquatinting amine (0,048 mmol/g free amine and 0,071 mmol/g protonated amine). Analysis by HPLC showed that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 6.8% monoether and 93.2% of diapir (ratio of peak areas in %).

The composition has a melt viscosity equal to 368 MPa·s at a shear rate equal to 1-1, 340 MPa·s at 10-1and 318 MPa·s at 100 s-1.

Example 15

3214 g (11,77 mol) Fatty acid was atrificial using 883,5 g (6,05 mole) bis-(2-hydroxypropyl)-methylamine for 4 h the reaction under reduced pressure until the acid number of the reaction mixture n which was equal to 3.3 mg KOH/g Then added 157 g of refined coconut oil and the resulting mixture was brought into reaction with 724,2 g (5,75 mole) of dimethylsulfate for 1 h and Then added 472 g of 2-propanol and the mixture is homogenized by stirring. Received active composition softener fabric was a white solid having a melting point equal to 36°C, containing 0,049 mmol/g (1.4 wt.%) fatty acid and 0.125 mmol/g aquatinting amine (0,067 mmol/g free amine and 0,058 mmol/g protonated amine). Analysis by HPLC showed that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 6.3% of monoether and 93.7% of diapir (ratio of peak areas in %).

The composition has a melt viscosity that is equal to 144 MPa·s at a shear rate equal to 1-1, 107 MPa·s at 10-1and 94 MPa·s at 100 s-1.

Figure softness using the composition is equal to 34.

Example 16 (comparative example corresponds to example 50, WO 00/06678)

250 g (to 1.15 mol) Radiacid® 600 fatty acids were atrificial using 176,3 g (1,21 mole) bis-(2-hydroxypropyl)-methylamine for 14 h at ambient pressure until the acid number of the reaction mixture does not become equal to 2.6 mg KOH/g, the Obtained mixture was introduced into a reaction with 137,0 g (1,09 mole) of dimethylsulfate. Received active softener composition TC is neither represented a yellowish wax, having a melting point equal to 35°C, containing 1.1 wt.% fatty acid. Analysis by HPLC showed that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 84.7% of monoether and 15.3% diapir (ratio of peak areas in %).

Figure softness using the composition is 13.

Example 17 (comparative, the smaller the ratio of the number of moles of fragments of fatty acids to the number of moles of amine fragments)

378,6 g (1,38 mol) Fatty acid was atrificial with the help of 211.5 g (1,45 mole) bis-(2-hydroxypropyl)-methylamine for 12 h at ambient pressure until the acid number of the reaction mixture does not become equal to 3.8 mg KOH/g, the Obtained mixture was introduced into a reaction with 164,5 g (1,60 mole) of dimethylsulfate. Received active composition of fabric softener was a yellowish wax having a melting point equal to 40°C, containing 1.7 wt.% fatty acid. Analysis by HPLC showed that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 80,7% monoether and 19.3% of diapir (ratio of peak areas in %).

Figure softness using the composition is 13.

Example 18

411,0 g (of 1.50 mol) Fatty acid was atrificial using 146,0 g (1.0 mole) of bis-(2-hydroxypropyl)-methylamine for 16 h at a pressure environment is the first environment, until the acid number of the reaction mixture does not become equal to 5.0 mg KOH/g, the Obtained mixture was introduced into a reaction with 113,5 g (0,9 mol) dimethylsulfate. Received active composition of fabric softener was a yellowish wax having a melting point equal to 38°C, containing 2.2 wt.% fatty acid. Analysis by HPLC showed that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 39.0% of monoether and 61,0% diapir (ratio of peak areas in %).

Figure softness using the composition equal to 25. Comparative examples 16 and 17 and example 18 shows that in order to ensure acceptable softening abilities required minimum ratio of the number of moles of fragments of fatty acids to the number of moles of amine fragments, equal to 1.5.

Example 19 (comparative, Quaternary salt with ammonium chloride)

2780 g (10,18 mol) Fatty acid was atrificial with 783 g (are 5.36 mol) bis-(2-hydroxypropyl)-methylamine for 3 h the reaction under reduced pressure until the acid number of the reaction mixture does not become equal to 5.2 mg KOH/g 469,2 g of the resulting mixture under stirring was injected into the autoclave were added 195 g of acetonitrile, and the autoclave was closed and heated at 75°C. In an autoclave with stirring at 75°C with speed, providing the pressure in the reactor equal to less than 4 BA is, introduced the 41.75 g (0,827 mole) of methyl chloride and the mixture was stirred for 90 hours at a temperature equal to 75 to 80°C. Then the pressure dropped solvents and unreacted methyl chloride and acetonitrile drove away. Received active composition softener fabric was a white solid having a melting point equal to 69°C, containing of 0.085 mmol/g (2.3 wt.%) fatty acids and 0,152 mmol/g aquatinting amine (0,103 mmol/g free amine and 0,049 mmol/g protonated amine). Analysis by HPLC showed that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains 1.0% monoether and 99.0% diapir (ratio of peak areas in %).

10% Aqueous dispersion has an acid number equal to 1.2 mg KOH/g, and a viscosity equal to 66 MPa·s to storage, but during storage for 6 weeks at 50°C was divided into two phases.

Comparative example 19 shows that the composition should contain Quaternary ammonianitrogen salt to have a low melting temperature and to ensure the stability of aqueous dispersions, whereas Quaternary ammoniacloridegas salt leads to high melting temperature 10 and insufficient stability of aqueous dispersions.

Table 2 shows the characteristics of active softener compositions fabrics obtained in examples 1-15 Otnoshenie the number of moles of fatty acid to the number of moles of the amine in table 2 means the ratio of the numbers of moles in bis-(2-hydroxypropyl)-dimethylaminomethylphenol ether 15 fatty acids, calculated according to the analysis by HPLC. The values of the acid number increase, and the change in viscosity during storage refers to 10 wt.% aqueous dispersions of the active compositions, fabric softener, which were stored for 6 weeks at 50°C.

Table 2
Characteristics of the active compositions of fabric softner
ExampleThe ratio of the number of moles of fatty acid to the number of moles of amineFatty acid, wt.%Melting point, °CThe melt viscosity at 1 s-1, MPa·sThe melt viscosity at 100 C-1MPa·sThe increase in acid number after storage, mg KOH/gThe change in viscosity after storage, MPa·sFigure softness
1*1,920,5<206854310,623112
2 1,910,7424720029600,6032
3*BUT1,0**5614690,711024
41,970,9433620021600,7231
51,952,24123606192,0-1635
61,940,7431620015301,4-632
7 1,944,15418426192,6-1531
8*1,931,6<205814801,7-423
9*1,971,1**5524971,74916
101,831,3412710018701,6-627
111,992,24315105532,4-1931
12 1,942,038592552BUTHOHO
131,931,952347002630BUTHOHO
141,932,440368318BUTHOHO
151,941,43614494HOHOHO
* Not proposed in this invention; ** gel; HO=not determined.

1. Active composition of fabric softener containing
a) at least 50 wt.% bis-(2-hydroxypropyl)-dimethylaminomethylphenol fatty acid ester with respect to the quantities of the moles of fragments of fatty acids to the number of moles of amine fragments, equal to from 1.5 to 1.99, where the average chain length fragments of the fatty acid is from 16 to 18 carbon atoms and an iodine number of fragments of fatty acids, calculated for the free fatty acid is from 0.5 to 50, and
b) from 0.5 to 5 wt.% fatty acid.

2. Active composition of fabric softener according to claim 1, characterized in that the ratio of the number of moles of fragments of fatty acids to the number of moles of amine fragments is from 1.85 to 1.99.

3. Active composition of fabric softener according to claim 1 or 2, characterized in that the iodine number of fragments of fatty acids, calculated for the free fatty acid is from 5 to 40, preferably from 15 to 35.

4. Active composition of fabric softener according to claim 1 or 2, characterized in that it contains from 1 to 5 wt.% and preferably from 2 to 5 wt.% fatty acid.

5. Active composition of fabric softener according to claim 1 or 2, characterized in that it contains from 85 to 99 wt.% bis-(2-hydroxypropyl)-dimethylaminomethylphenol ether fatty acids.

6. Active composition of fabric softener according to claim 1 or 2, characterized in that bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acid contains less than 6 wt.% polyunsaturated fragments of fatty acids.

7. Active composition of fabric softener according to claim 1 or 2, characterized in that the ratio of the amounts of CIS : TRANS double bonds in fragments Nena is yennai fatty acid bis-(2-hydroxypropyl)-dimethylaminomethylphenol the fatty acid ester is more than 55:45.

8. Active composition of fabric softener according to claim 1 or 2, characterized in that the fragments of fatty acid bis-(2-hydroxypropyl)-dimethylaminomethylphenol the fatty acid ester formed from a fatty acid component (b).

9. Active composition of fabric softener according to claim 1 or 2, containing less than 2 wt.% and preferably less than 0.5 wt.% water.

10. Active composition of fabric softener according to claim 1 or 2, containing less than 10 wt.% and preferably less than 1 wt.% solvents having a flash point equal to less than 20°C.

11. Active composition of fabric softener according to claim 1 or 2, additionally containing up to 9.9 wt.% at least one solvent selected from the group comprising glycerine, ethylene glycol, propylene glycol, dipropyleneglycol and C1-C4-alkalemia monoether of ethylene glycol, propylene glycol and dipropyleneglycol.

12. Active composition of fabric softener according to claim 1 or 2, additionally containing from 2 to 8 wt.% the triglyceride fatty acids with medium chain length fragments of the fatty acid constituting from 10 to 14 carbon atoms, and iodine number, calculated for the free fatty acid equal to from 0 to 15.

13. Active composition of fabric softener according to claim 1 or 2, additionally containing from 1.5 to 9 wt.% bis-(2-hydroxypropyl)-methylamino ester of a fatty acid containing the same fragments of the IRNA acid, as bis-(2-hydroxypropyl)-dimethylaminomethylene ether fatty acids.

14. A method of obtaining a composition of fabric softener according to claim 1, which includes stages
a) the reaction of bis-(2-hydroxypropyl)-methylamine fatty acid having an average chain length equal to 16 to 18 carbon atoms, and iodine number equal to from 0.5 to 50, with respect to the number of moles of fatty acid to the number of moles of the amine is 1,51 to 2.1, with removal of water until the acid number of the reaction mixture will not be in the range from 1 to 10 mg KOH/g and
b) reaction of the product obtained in stage a), with dimethylsulfate when the ratio of the number of moles of dimethylsulfate to the number of moles of the amine, equal from 0.90 to 0.97, and preferably from 0.92 to 0.95, while the amine number of the reaction mixture will not be in the range of from 1 to 8 mg KOH/g

15. The method according to 14, characterized in that the ratio of the number of moles of fatty acid to the number of moles of the amine is from of 1.86 to 2.1.



 

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9 cl, 5 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: described is a detergent which contains: an alkali metal hydroxide, sodium metasilicate, dye and water, and additionally oxyethylene diphosphonic acid, a tetrasodium salt of oxyethylene diphosphonic acid, a salt of ethylenediaminotetraacetic acid, citric acid, sodium silicate, a sodium salt of a copolymer of acrylic acid and maleic acid, alkylated polyglycoside with length of the alkyl chain of C6-C12, a mixture of anionic surfactants, with the following ratio of components, wt %: alkali metal hydroxide 4-12%, oxyethylene diphosphonic acid 0-8%, tetrasodium salt of oxyethylene diphosphonic acid 0-8%, salt of ethylenediaminotetraacetic acid 1-3%, citric acid 2-10%, sodium silicate 0,5-3%, sodium salt of a copolymer of acrylic acid and maleic acid 0-1%, alkylated polyglycoside with length of the alkyl chain of C6-C12, with respect to pure substance 1-6%, mixture of anionic surfactants, which includes a compound of the type RO-(CHR'CHR'-O)nSO3Na, where R is a linear or branched saturated or unsaturated alkyl substitute with backbone chain length of C10-C18, R'=H, CH3, n ranges from 0 to 4 and a compound of the type R"C6H4SO3X, where R" is a linear or branched saturated or unsaturated alkyl substitute with backbone chain length of C6-C12, X-Na, K, H with respect to pure substance 2-10%, dye 0.05-0.5%, water - the balance.

EFFECT: improved quality of contactless washing due to higher foaming capacity.

6 cl, 3 ex

FIELD: chemistry.

SUBSTANCE: described is a washing liquid which can be used to clean car windscreens. The washing liquid contains, as a freezing point lowering component, methyl ether of propylene glycol, as well as an anionic surfactant, a nonionic surfactant, trilon B, a dye, a deodorant, triethanolamine, phosphoric acid and water. The method of preparing the washing liquid involves preparing a highly concentrated solution of methyl ether of propylene glycol in deionised water by mixing 90% methyl ether of propylene glycol and 10% deionised water. An anionic surfactant, a nonionic surfactant, trilon B, triethanolamine, phosphoric acid, an antifoaming agent, a deodorant, a dye and, optionally, ethylene glycol are then added to the obtained solution while stirring. Deionised water is added to the solution while stirring continuously and stirring continues until complete homogeneity, followed by filtration.

EFFECT: reduced metal corrosion and swelling of rubber components and paint coat.

4 cl, 5 tbl

FIELD: chemistry.

SUBSTANCE: described is a compact liquid detergent composition containing less than 25% water by mass of the composition and a mixture of chelating agents, wherein the first chelating agent is selected from a group consisting of a sodium salt of ethylenediamine-N,N'-disuccinic acid, ethylenediamine-N,N'- disuccinic acid which is neutralised with 2-aminoethanol, and mixtures thereof, and the second chelating agent is a sodium salt of diethylene triamine pentaacetate.

EFFECT: high activity of the chelating agents, efficient stain removal.

8 cl, 1 tbl

Method of cleaning // 2519554

FIELD: process engineering.

SUBSTANCE: proposed method comprises placing the part into container that sustains a variable pressure. Foam composition is applied to the part including at least one foaming agent, at least one ferment and dissolved gas. Note here that said foam composition is redistributed over the part at application and/or after part cleaning. The part is cleaned by foam composition at application of variable pressure to container. Besides, said part is rinsed with appropriate fluid at pressure application to said container. Note here that pressure in said container is increased unless said foam composition behaves as a fluid.

EFFECT: better cleaning.

14 cl, 6 dwg, 5 tbl

Fabric softener // 2515236

FIELD: chemistry.

SUBSTANCE: invention relates to methods of producing a fabric softener. Disclosed are methods of producing a fabric softener composition, containing 1-49% bis-(2-hydroxyethyl)-diethylammonium chloride of a fatty acid ester by weight of the composition, which include a step of mixing water with an active composition (FSAC), wherein the FSAC contains 65-95% by weight of FSAC of bis-(2-hydroxyethyl)-diethylammonium chloride of a fatty acid ester, having molar ratio of fatty acid fragments and amine fragments of 1.80-1.96, average chain length of fatty acid fragments of 16-18 carbon atoms and iodine number, calculated for a free fatty acid, of 0-50, 2-8% by weight of FSAC of a fatty acid triglyceride, having average chain length of fatty acid fragments of 10-14 carbon atoms and iodine number, calculated for a free fatty acid, of 0-15, and 3-12% by weight of FSAC of alcohol, selected from ethanol, 1-propanol and 2-propanol.

EFFECT: preparing a fabric softener composition with low content of flammable solvents, low melt viscosity and high stability in molten state.

22 cl, 1 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to compositions for controlling foaming for liquid detergent systems. Disclosed is a composition for controlling foaming, which contains: (A) an organosilicon antifoaming agent containing (i) organopolysiloxane having at least one substitute of formula X-Ar linked to silicon, where X is a divalent aliphatic group linked to a silicon atom through a carbon atom, and Ar is an aromatic group, (ii) an organosilicon polymer of formula R1aSiO(4-a)/2, where R1 is a hydrocarbon group, hydrocarbon oxy or hydroxyl, and a has an average value from 0.5 to 2.4, and (iii) hydrophobic filler, and (B) organopolysiloxane resin containing at least one polyoxyalkylene group, as well as tetrafunctional siloxane links of formula SiO4/2 and monofunctional siloxane links of formula R23SiO1/2, wherein the total number of tetrafunctional siloxane links in the resin is not less than 50% of the total number of siloxane links, and R2 is a hydrocarbon group. Also disclosed is a liquid detergent containing one or more surfactants, weater and said composition for controlling foaming.

EFFECT: disclosed composition is safe and inert to detergent components, provides stability of the mixture in detergents and excellently control foaming.

4 cl, 1 dwg, 2 tbl, 8 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a liquid hand dishwashing detergent composition which contains: (a) 0.001-10 wt % cationic polymer and (b) 0.005-3 wt % active inorganic mother-of-pearl agent having particle size smaller than 50 mcm, and the cationic polymer is a carboxyethyl cellulose salt. The present invention relates to a method of cleaning dishes.

EFFECT: obtaining a dishwasher detergent which cares for skin, particularly correction of cysts and skin lustre.

22 cl, 12 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of reducing creases when washing a garment made from heavy fabric, which includes steps of washing the garment and applying a fabric softener, which contains a quaternary ammonium fatty ester and a hydrolysed protein and polysiloxane copolymer, where the average molecular weight of the protein component ranges from 500 to 500000 Da, to the garment made from fabric weighing at least 250 g/m2. The present invention also relates to a fabric softener for reducing creases on garments made from heavy fabric, which contains: a) 0.5-50 wt % cationic softener, which contains a fatty acid ester of quaternary ammonium, b) 0.02-0.5 wt % hydrolysed protein and siloxane copolymer, where the average molecular weight of the protein component ranges from 500 to 500000 Da, c) a fragrant and d) water.

EFFECT: obtaining an efficient and cheap agent for removing or reducing creases on clothes during washing and drying.

13 cl, 3 ex, 4 tbl

FIELD: chemistry.

SUBSTANCE: foaming composition contains (i) at least one component of formula (1)

,

where one of symbols B1, B2, B3 independently denotes an acyl group represented by -CO-R and the rest denote H, (ii) at least one component of formula (1), where two of symbols B1, B2, B3 independently denote an acyl group represented by -CO-R and the rest denote H, (iii) at least one component of formula (1), where each of symbols B1, B2, B3 independently denotes an acyl group represented by -CO-R, (iv) at least one component of formula (1), where each of B1, B2 and B3 denotes H. The weight ratio of components (i)/(ii)/(iii) is equal to 60-90/10-35/less than 10 in formula (1), where R' denotes H or CH3, each of m, n or l independently denotes a number from 0 to less than 9, where the sum of m, n and l ranges from more than 5 to less than 9, where in the acyl group represented by -CO-R, R denotes an alkyl or alkenyl group, linear or branched, containing 6 to 9 carbon atoms, and the weight ratio of (i)+(ii)+(iii)/(iv) ranges from 2.0:0.5 to 0.5:3.0. The invention also relates to use of the foaming composition as a foaming enhancing or stimulating agent in detergent compositions.

EFFECT: foaming composition enables to achieve maximum foam volume and increase the number of theoretical plates.

5 cl, 5 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: alkaline detergent for fabric hand washing contains a foaming surfactant, polyethylene imine defoamer having empirical formula (PEI)aEO)b(PO)c (I), where a assumes a value from 100 to 100000, b assumes a value from 5 to 60 and c assumes a value from 2 to 60; and a pH control system. When said detergent is diluted with water in weight ratio 1:350 in order to prepare a washing solution and during washing, the pH control system keeps pH of the washing solution at temperature 20°C higher than 8. The present invention relates to a method for hand washing fabric, involving steps for providing the laundry detergent, preparing the washing solution by diluting the detergent with water in weight ratio from 1:150 to 1:1000, keeping pH of the washing solution higher than 9, hand washing the fabric in the washing solution, keeping pH of the washing solution between 9 and 13 during the washing step, rinsing the linen in a rinsing bath, wherein pH of the rinsing bath is lower than 9. The invention also relates to a method of saving water, involving a step for washing fabric in accordance with the hand washing method.

EFFECT: reduced foaming after the first rinsing.

12 cl, 4 ex, 1 tbl

FIELD: chemistry.

SUBSTANCE: invention describes fabric softening compositions containing approximately from 0.01 to 50% cationic or nonionic softening compound; approximately from 0.01 to 5% fragrance component; and at least 0.001 wt % polymer material capable of holding ingredients of a volatile fragrance component, containing: at least approximately 0.001 wt % cross-linked polymer containing at least one vinyl monomer; and approximately from 5000 to 100000 ppm divinyl cross-linking agent. Also disclosed is a fabric softening method which involves bringing fabric into contact with the composition of a fabric softening agent in an effective amount, where contact takes place by sprinkling, rubbing or rinsing.

EFFECT: improved composition properties.

26 cl, 5 ex, 4 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to water-soluble hydroxyethyl cellulose and derivatives thereof. Hydroxyethyl cellulose and derivatives thereof are characterised by ratio of unsubstituted trimers less than approximately 0.21, hydroxyethyl molar substitution between approximately 0.7 and 1.3 and water-solubility of over 90%. Hydroxyethyl cellulose is obtained using a suspension method. Cellulose, water and alkali are mixed and react in an organic solvent. Molar ratio of water to anhydroglucose in the prepared alkaline cellulose mixture lies between approximately 5 and 35, and molar ratio of alkali to anhydroglucose is greater than approximately 1.6. Ethylene oxide is added. A sufficient amount of acid is continuously added so as to reduce the molar ratio of alkali to anyhydroglucose to at least approximately 0.4 and preferably higher than approximately 0.04 while simultaneously reacting ethylene oxide with alkaline cellulose. If needed, at least one deriving agent is added to obtain modified hydroxyethyl cellulose. A viscosity lowering agent is then added. This water-soluble hydroxyethyl cellulose and its derivatives are used in compositions for personal care agents, compositions for household care agents, pharmaceutical compositions, building compositions, emulsion polymerisation compositions, compositions of working fluids for oil fields, compositions of working fluids for civil engineering, compositions for coating paper, compositions for making paper, compositions for applying architectural coatings, compositions for applying industrial coatings, compositions for printing ink, adhesive compositions and compositions for processing and extracting minerals.

EFFECT: obtained hydroxyethyl cellulose and its derivatives is more efficient when concentrating aqueous systems than existing hydroxyethyl cellulose products, and demonstrates unique rheological properties in systems with low water activity.

34 cl, 8 ex, 16 tbl, 24 ex, 1 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to nonuniformly substituted (substituted in mass) hydroxyethyl cellulose and derivatives thereof. Hydroxyethyl cellulose contains groups which are nonuniformly distributed in the cellulose main chain. The fraction of unsubstituted trimmers is greater than 0.21 and hydroxyethyl molar substitution is greater than approximately 1.3 and less than approximately 5.0. Hydroxyethyl cellulose which is substituted in the mass is obtained and used in functional systems. The method involves mixing and reacting cellulose, water and ethylene oxide in an organic solvent for a sufficient period of time and sufficient temperature. A second mixture of the main cellulose reagent is then prepared by adding acid or a mixture of the main hydroxyethyl cellulose reagent by adding ethylene oxide followed by addition of the main reagent. Further, ethylene oxide is added to the second mixture of the main cellulose reagent or the cellulose mixture of the main hexaethyl cellulose reagent and the reaction is carried out at sufficient temperature for a sufficient period of time to obtain the hydroxyethyl cellulose end product.

EFFECT: mixture of hydroxyethyl cellulose and derivatives thereof have unique and high-demand rheological properties and are more efficient in thickening aqueous systems than existing hexaethyl cellulose products.

37 cl, 1 dwg, 16 tbl, 33 ex

Fabric softener // 2515236

FIELD: chemistry.

SUBSTANCE: invention relates to methods of producing a fabric softener. Disclosed are methods of producing a fabric softener composition, containing 1-49% bis-(2-hydroxyethyl)-diethylammonium chloride of a fatty acid ester by weight of the composition, which include a step of mixing water with an active composition (FSAC), wherein the FSAC contains 65-95% by weight of FSAC of bis-(2-hydroxyethyl)-diethylammonium chloride of a fatty acid ester, having molar ratio of fatty acid fragments and amine fragments of 1.80-1.96, average chain length of fatty acid fragments of 16-18 carbon atoms and iodine number, calculated for a free fatty acid, of 0-50, 2-8% by weight of FSAC of a fatty acid triglyceride, having average chain length of fatty acid fragments of 10-14 carbon atoms and iodine number, calculated for a free fatty acid, of 0-15, and 3-12% by weight of FSAC of alcohol, selected from ethanol, 1-propanol and 2-propanol.

EFFECT: preparing a fabric softener composition with low content of flammable solvents, low melt viscosity and high stability in molten state.

22 cl, 1 tbl

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