Fibre active (reactionable) azo dyes, obtaining and application thereof

FIELD: chemistry.

SUBSTANCE: invention relates to novel active dyes, methods of their obtaining and their application in dyeing or printing textile fibrous materials. An active dye of formula in which B represents a radical of formula -CH2-CH(R12)- or -(R12)CH-CH2-, in which R12 represents C1-C4alkyl, R5 represents hydrogen or sulpho, Z1 represents a fibre-reactionable group of formula -SO2-Y (3a) or -NH-CO-(CH2)l-SO2-Y (3b), R7 represents amino, R8 represents C2-C4alkanoylamino or ureido, X1 and X2 represent, each independently on the other, fluorine or chlorine, k equals a number 2 or 3, l equals a number 2 or 3 and Y represents vinyl or β-sulphatoethyl.

EFFECT: invention makes it possible to obtain the improved active dyes with high reaction ability, chemical affinity, as well as with good dyeability with a high degree of fixation.

8 cl, 2 tbl, 8 ex

 

The present invention relates to new active dyes, processes for their preparation and their use for dyeing or printing fibrous textile materials.

The practice of dyeing with the use of active dyes has recently led to higher requirements, which are as dyeing and profitability of the method of dyeing. As a result of this there is still a need for new active dyes having improved properties, especially in regard to their application.

Dyeing currently requires the use of active dyes, which have sufficient chemical affinity and at the same time have good washability unfixed dye. They should also have a good nakruchivaet and high reactivity, and the goal is especially ensuring krasheny with a high degree of fixation. Known dyes do not meet these requirements for all properties.

Asymmetric dyes known from US-A-5395925 and US-A-5552532, still have some drawbacks in respect of the above properties.

Therefore, the problem underlying the present invention is to develop for dyeing and printing fiber materials new and improved active dyes, which have the above described properties to a high degree. New the like should especially be highly narasimhamurthy and high stability of the connection fiber-dye. The dyes must also ensure the durability of the paints that have good properties of strength on all indicators, such as light fastness properties and moisture resistance.

It is shown that this problem mostly resolved with new dyes, the following.

The present invention accordingly relates to the active dye of the formula

in which

In represents an aliphatic bridge member,

G is a group of sulfonation or group of sulfobenzoic formula

or

the pyridone radical of the formula

R1, R2, R3and R4represent, each independently of the other hydrogen or unsubstituted or substituted C1-C4alkyl,

(R5)hmeans h is identical or different substituents selected from sulfopropyl,1-C4the alkyl and C1-C4alkoxy,

R6represents hydrogen, sulfo, halogen, carboxy, C1-C4alkyl, C1-C4alkoxy or active fiber group Z1formula

-SO2-Y
-NH-CO-(CH2)l-SO2-Y
-CONH-(CH2)m-SO2-Y
-NH-CO-CH(Hal)-CH2-Hal
-NH-CO-C(Hal)=CH 2
(3a)
(3b)
(3c)
(3d) or
(3rd)

R7represents amino, C1-C4alkyl or active fiber group Z2formula

-NH-(CH2)n-SO2-Y (3a)

(R8)jmeans j is identical or different substituents selected from sulfopropyl,2-C4alkanolamine, ureido,1-C4the alkyl and C1-C4alkoxy,

R9represents hydrogen, C1-C4alkyl or C1-C4alkoxy,

R10represents hydrogen or C1-C4alkyl,

R11represents hydrogen, cyano, carbarnoyl or sulfoethyl and

R12represents hydrogen, C1-C4alkyl or phenyl, which is unsubstituted or substituted With1-C4the alkyl, C1-C4alkoxy, C2-C4alkanolamine, ureido, halogen or sulfo,

X1and X2represent the atoms of halogen,

Hal represents chlorine or bromine,

h and j are each independently equal to the number 0, 1 or 2,

k is equal to the number 1, 2 or 3,

l, m and n are, each independently from each other equal to the number 2, 3 or 4, and

Y is vinyl or a radical-CH2-CH2-U and U is a group removable in alkaline conditions, with the proviso that the dye of formula (1) which holds at least one active fiber group Z 1or Z2.

The dyes of formula (1) contain at least two, preferably from 2 to 5 and especially 4-or 5-sulfo -, each of which is present either in the form of free acid or preferably in salt form. Suitable salts are, for example, alkali metal salts, alkaline earth metal or ammonium salts, organic amine or a mixture thereof. Examples of salts that can be specified are the salts of sodium, lithium, potassium or ammonium salt of mono-, di - or triethanolamine or mixed salts of Na/Li or Na/Li/NH4.

In another embodiment, R6represents the active fiber group Z1formula (3A), (3b), (3c), (3d) or (3E), above, and

R7represents amino or1-C4alkyl, especially amino.

In another embodiment of the present invention, the active dye of formula (1) corresponds to the formula

,

in which

In represents an aliphatic bridge member,

G is a group of sulfonation or group of sulfobenzoic formula (2A), in which K has the values listed above,

R1, R2, R3and R4represent, each independently of the other hydrogen or unsubstituted or substituted C1-C4alkyl,

(R5)h means h is identical or different substituents selected from sulfopropyl,1-C4the alkyl and C1-C4alkoxy,

R6represents the active fiber group Z1formula

-SO2-Y
-NH-CO-(CH2)l-SO2-Y
-CONH-(CH2)m-SO2-Y
-NH-CO-CH(Hal)-CH2-Hal
-NH-CO-C(Hal)=CH2
(3a)
(3b)
(3c)
(3d) or
(3rd)

R7represents amino or1-C4alkyl

(R8)jmeans j is identical or different substituents selected from the group2-C4alkanolamine, ureido,1-C4the alkyl and C1-C4alkoxy,

R9represents hydrogen, C1-C4alkyl or C1-C4alkoxy,

X1and X2represent the atoms of halogen,

Hal represents chlorine or bromine,

h and j are each independently equal to the number 0, 1 or 2,

k is equal to the number 1, 2 or 3,

l and m, each independently from each other equal to the number 2, 3 or 4, and

Y is vinyl or a radical-CH2-CH2-U and U is a group removable in alkaline conditions.

The radicals R1, R2, R3and R4in the active dye of formula (1) are alkyl Radik the crystals, which are unbranched or branched. The alkyl radicals can be further substituted, for example, hydroxy, sulfo, sulfate, cyano or carboxy. As examples, you can specify the following radicals: methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, tert-butyl or isobutyl, and the corresponding radicals substituted by hydroxy, sulfo, sulfate, cyano or carboxy. Preferred substituents are hydroxy, sulfo or sulphate, particularly hydroxy or sulphate, particularly hydroxy or sulfate, and more particularly hydroxy.

R1and R4represent, each independently, hydrogen or C1-C4alkyl, especially hydrogen.

R2and R3preferably represent, each independently, hydrogen or C1-C4alkyl, which is unsubstituted or substituted by hydroxy, sulfo, sulfate, cyano or carboxy. In an interesting embodiment, one of the radicals R2and R3represents a C1-C4alkyl, which is substituted by hydroxy, sulfo, sulfate, cyano or carboxy, and the other of the radicals R2and R3represents hydrogen or C1-C4alkyl, especially hydrogen.

R2and R3especially represent, each independently, hydrogen or C1-C4 alkyl, especially hydrogen.

In an important embodiment of the present invention R1, R2, R3and R4each independently represent hydrogen or C1-C4alkyl, especially hydrogen.

As With1-C4the alkyl in the context for each of R5, R6, R7, R8, R9, R10and R12regardless of any other(other), are considered, for example, methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, tert-butyl or isobutyl, preferably methyl or ethyl. Particularly preferably, R5, R6, R7, R8and R9and R10represent methyl. Particularly preferably, R12represents ethyl.

As With1-C4alkoxy in the context for each of R5, R6, R8and R9regardless of any other(other), are considered for example methoxy, ethoxy, n-propoxy, isopropoxy, butoxy or isobutoxy, preferably methoxy or ethoxy and especially methoxy.

As halogen for R6in the context considered, for example, fluorine, chlorine or bromine, preferably chlorine or bromine and especially chlorine.

With2-C4alkanolamine for R8represents, for example, acetylamino or propionamido, in particular acetylamino.

h is preferably equal to the number is a 0 or 1.

j is preferably equal to the number 1 or 2, especially 1.

In a preferred embodiment, (R5)hmeans hydrogen, where h is the number 0, or sulfo, where h is the number 1, especially sulfa.

In a preferred embodiment, (R8)jmeans 1 or 2 identical or different substituents selected from group C2-C4alkanolamine, ureido,1-C4the alkyl and C1-C4alkoxy.

In another preferred embodiment, (R8)jmeans2-C4alkanolamine or ureido, where j is the number 1, especially ureido.

Preferably, R9represents hydrogen or C1-C4alkoxy, especially hydrogen.

In represents, for example, With2-C12alkylen with unbranched or branched chain, which is unsubstituted or substituted by hydroxy, C1-C4alkoxy, sulfate or sulfo and chain which may be interrupted once or more than once,- O - or-NR*-, preferably-O-, and R* represents hydrogen or C1-C4alkyl, preferably hydrogen, methyl or ethyl and especially hydrogen. In a preferably represents C2-C6alkylen with unbranched or branched chain, which is unsubstituted or substituted by hydroxy, sulfo or Sul the ATO, especially hydroxy, and more specifically represents a C2-C6alkylen with unbranched or branched chain. Examples of preferred radicals are 1,2-ethylene, 1,2-propylene, 1,3-propylene, 2-hydroxy-1,3-propylene, 1,4-butylene, 2,2-dimethyl-1,3-propylene, 2-methyl-1,5-pentile, 1,6-hexylen.

Especially interesting as bridge members are those With2-C6alkylene radicals which correspond to the formula-CH2-CH(R13)- or (R13)CH-CH2-, in which R13represents a C1-C4alkyl, especially methyl. A very special value for a is 1,2-propylene.

X1and X2preferably represent, each independently, a chlorine or fluorine. The radicals X1and X2are identical or non-identical. In a specific embodiment, the present invention one of the radicals X1and X2represents fluorine and the other of the radicals X1and X2represents chlorine. The radicals X1and X2preferably are identical and mean fluoride.

Hal represents bromine or chlorine, preferably bromine.

k is preferably equal to the number 2 or 3, especially 3.

l is preferably equal to the number 2 or 3, especially 3.

m and n are preferably, each independently of the other, is what the Isla 2 or 3, especially 2.

Z1represents preferably a radical of formula (3A), (3b) or (3C), especially of formula (3A) or (3b) and more specifically (3A), in which l, m and Y have the meanings and preferred meanings indicated above.

As U removed under alkaline conditions, in the context considered, for example, -Cl, -Br, F, -OSO3H-SSO3H, -OCO-CH3, -OPO3H2, -OCO-C6H5, -OSO2-C1-C4alkyl-OSO2-N(C1-C4alkyl)2. U preferably represents a group of formula-Cl, -OSO3H-SSO3H, -OCO-CH3, -OCO-C6H5or ORO3H2especially-Cl or-OSO3H and, more specifically OSO3H.

Examples of suitable radicals Y, respectively, that are vinyl, β-bromo - or β-chloroethyl, β-acetoxyethyl, β-benzyloxyethyl, β-phosphatidyl, β-sulphatoethyl and β-thiosulfinates. Y preferably represents a vinyl, β-chloroethyl or β-sulphatoethyl and especially vinyl or β-sulphatoethyl.

Preferred active dyes of formula (1) are reactive dye of the formula

,

in which

In, R5, R7, R8X1X2, Z1and k each independently have the respective meanings and preferred meanings indicated above.

Particular preference is given to the active dyes of the formula (1b), in which a represents a radical of formula-CH2-CH(R13)- or -(R13)CH-CH2-, in which R13represents a C1-C4alkyl,

R5represents hydrogen or sulfo,

Z1represents for fiber reactive group of the formula

-SO2-Y (3a) or

-NH-CO-(CH2)l-SO2-Y (3b)

R7represents amino,

R8represents a C2-C4alkanolamine or ureido,

X1and X2represent, each independently, fluorine or chlorine,

it is equal to the number 2 or 3,

l is the number 2 or 3 and

Y is vinyl or β-sulphatoethyl.

The present invention relates also to a process for the preparation of dyes of formula (1), in which each of the compounds of formula

subjected to reaction with one another such connection in a suitable manner and in appropriate molar equivalents, where B, G, R1, R2, R3, R4, R5, R6, R7, R8, R9X1X2, h and j each independently have the respective meanings and preferred meanings indicated above.

As gelegenheid cyanuric acid of formula (6) and (7) are suitable acid chloride cyanuric acid and floramite cyanuric acid.

Compounds of formulas (6) and (7) are identical or non-identical. In an interesting embodiment, one of the compounds of formulas (6) and (7) represents the acid chloride cyanuric acid and other compounds of the formulas (6) and (7) represents floramite cyanuric acid.

Monotonicity formulas (4) and (5) can be obtained by reaction of diazotization and combinations. The diazotization is conducted in the usual way, for example by diazotization in the solution of mineral acid, for example in a solution containing hydrochloric acid, a nitrite, e.g. sodium nitrite, at a low temperature, for example from 0 to 30°C, and then the combination with a suitable component combinations in the environment from neutral to weak acid, for example at pH 3 to 7 and at low temperatures, for example from 0 to 30°C. as diazocompounds to get monotonicity formula (5) is considered, for example, 4-(β-sulphatoethylsulphonyl)aniline-2-sulfonic acid and 4-(β-sulphatoethylsulphonyl)aniline.

Monotonicity formula (4) described for example in US-A-5395925, you can get them on the analogy described in the mentioned patent the method.

Monotonicity formula (5) described for example in US-A-5747657, you can get them on the analogy described in the mentioned patent the method.

Because the stage of the method specified above, can be performed in different orders, in some cases, you can also use simultaneously the Menno different variants of the method. The reaction is usually carried out step by step, and the order of the simple reactions between the individual components of the reaction mainly depends on the specific conditions. In a preferred embodiment,

(i) a compound of the formula (4) condense with galogenangidridy cyanuric acid of the formula (6), thus obtaining the product of the formula

(ii) a compound of the formula (5) condense with galogenangidridy cyanuric acid of the formula (7), thus obtaining the product of the formula

(iii) a diamine of the formula (8) condense with one of the compounds of formulas (9a) and (9b)obtained according to (i) and (ii), resulting in the receive connection of the formula

or

and

(iv) a compound of the formula (10A) or (10b)obtained according to (iii), condensed in each case with another compound of the formula (9a) or (9b)obtained according to (i) and (ii), where B, G, R1, R2, R3, R4, R5, R6, R7, R8, R9X1X2, h and j each independently have the respective meanings and preferred meanings indicated above.

The condensation reaction between the compounds of formulae (4) and (6) and (5) and (7), the reaction of condensation between the compound of formula (9a) or (9b) and the diamine of formula (8) and the condensation reaction between the compound of formula (10A) or (10) and another compound of formula (9a) or (9b) is usually carried out analogously to known methods, usually in aqueous solution at a temperature of, for example, from -2°C to 50°C and at a pH of, for example, from 5 to 10. The condensation reaction with foramerica cyanuric acid or with condensation products of formulas (9a) and (9b), in which X1and X2represent fluorine, usually carried out at temperatures of, for example, from -2°C to 35°C.

The condensation reaction according to the above stages (i) and (ii) is usually carried out at temperatures of, for example, from -2°C to 20°C and at a pH of, for example, from 5 to 7. The condensation reaction according to the above stages (iii) and (iv) is usually carried out at temperatures of, for example, from 0°C to 50°C and at a pH of, for example, from 6 to 10.

In the above-described reactions of condensation of about 1 molar equivalent of each of the compounds of formulas(4), (5), (6), (7) and (8) is subjected to reaction with one another connection. In appropriate cases, the compounds of formulas (6) and (7) are used in equimolar or slightly excess amount, for example 1.0 to 1.5 molar equivalents of the compounds of formula (6) is condensed with 1 molar equivalent of a compound of the formula (4) and 1.0 to 1.5 molar equivalents of the compounds of formula (7) condense with 1 molar equivalent of a compound of the formula (5). Approximately 1 molar equivalent of each of the compounds of formulas (8), (9a) or (9b) and (10A) and (10b) are used in the condensation reaction between the compound of formula (9a) or (9b) and the diamine of formula (8) according to the decrees of the Anna above the stage (iii) and the condensation reaction between the compound of formula (10A) or (10b) and another compound of formula (9a) or (9b) according to the above stage (iv).

In another embodiment, a separate phase (i) and (ii) the above procedure is carried out together in one of the first stage of condensation, for example, approximately 1 molar equivalent of each of the compounds of formulas (4) and (5) with approximately 2 molar equivalents, for example 2 or 3 molar equivalents, gelegenheid cyanuric acid of the formula (6) or formula (7)) according to the above conditions, while receiving a mixture of compounds of the formula

and for further reaction in the second stage, approximately 1 molar equivalent of compound of formula (8) are added to the reaction mixture obtained in the first stage, and the reaction of condensation finish, while receiving a mixture of compounds of the formula

The present invention accordingly relates also to a mixture of reactive dyes containing at least one dye of the formulae (11a) and (11b) together with at least one dye of formula (11C) and (11d), especially one dye of each of the formulae (11a), (11b), (11c) and (11d), which applies the definitions and preferred definitions specified above for each of B, G, R1, R2, R3, R4, R5, R6, R7, R8, R9X1, h and j.

If necessary, the final product can also be subjected is the folder reaction conversion. This reaction conversion is, for example, the transformation ventiliruemye reactive group contained in Z1or Z2in its vinyl form by treatment with dilute sodium hydroxide solution, for example the conversion of β-sulphatoethylsulphonyl or β-Kharatishvili group in vinylsulphonyl radical, or the transformation of α,β-dialogproprietary.py in α-halogenallylacetic. Such reactions are essentially known. The reaction conversion is usually carried out in a neutral or alkaline medium at a temperature of, for example, from 20 to 70°C. when the pH value, for example, from 6 to 14.

Dyes and mixtures of dyes according to the present invention are active for fibers. It is assumed that the active fibers dyes are dyes which are capable of reacting with hydroxyl groups of cellulose, amino-, carboxy-, hydroxy - or colography in wool and silk or with the amino and possibly carboxyglutamic synthetic polyamides with the formation of covalent chemical bonds.

Dyes and mixtures of dyes according to the invention are suitable for dyeing and printing a very wide variety of materials, such as containing a hydroxyl group or nitrogen-containing fibre materials. Examples are silk, leather, wool, polyamide the e fibers and polyurethanes, and especially materials of cellulose fibers of all kinds. Such materials of cellulose fibers are, for example, natural cellulose fibers, such as fibers of cotton, flax and hemp, and cellulose and regenerated cellulose. Dyes and mixtures of dyes according to the invention are also suitable for dyeing or printing containing hydroxyl groups of the fibers present in the tissues of mixed fibers, for example mixtures of cotton with fibers of polyester or polyamide fibers. Dyes and mixtures of dyes according to the invention are particularly suitable for dyeing or printing cellulose, particularly those containing cotton fibrous materials. They can also be used for dyeing or printing materials of natural or synthetic polyamide fibers.

Dyes and mixtures of dyes according to the invention can be applied to the fibrous material and to fix the fiber in various ways, especially in the form of aqueous dye solutions and printing pastes dyes. They are appropriate as for a method of dyeing to depletion of the bath and the dyeing according to the method of dyeing management, according to which products are impregnated with aqueous, optionally containing salt solutions of dye and dyes are fixed after treatment with alkali or in the presence of alkali, optional when exposed to heat or aging at room temperature for several hours. After fixation products dyeing or printing thoroughly rinsed with cold and hot water, optionally with the addition of an agent which has a dispersing action and accelerates the diffusion of the unfixed dye.

Dyes and mixtures of dyes according to the invention have a high reactivity, good fixing ability and a very good ability to build color. So you can apply them in the way to exhaustion dyeing bath at low temperature dyeing and requires only a short time for steaming in the way of adding to hassle. The degrees of fixation are high, and the unfixed dye is easy to clean, and the difference between the degree of exhaustion and degree of fixation is extremely low, thus loss when washing in soapy water (after dyeing) is very small. Dyes and mixtures of dyes according to the invention are also particularly suitable for printing, more specifically on cotton, and also for printing nitrogen-containing fibres, for example fibres of wool or silk or mixed fabrics which contain wool or silk.

Painted and printed product p is obtained with the use of the dyes according to the invention, have high color saturation and high stability of binding fiber-dye in acidic and alkaline range, and good properties of resistance coloring to the action of light and of very good properties of resistance coloring to moisture, such as resistance to cleaning the environment, water, sea water, odnobannoyu dyeing products made of mixed fibres and perspiration, and also good resistance to wrinkling, hot pressing and rolling.

The present invention relates also to aqueous paints containing active dye of formula (1), and for B, G, R1, R2, R3, R4, R5, R6, R7, R8, R9X1X2, h and j of the formula used above the corresponding values and preferred values.

The dyes used in inks, preferably should have a low salt content, that is, they must have a total salt content less than 0.5 wt.% based on the weight of the dyes. Dyes, which have a relatively high salt content as a result of their receipt and/or the subsequent addition of diluents, you can obsolete, for example, procedures, membrane separation, such as ultrafiltration, reverse osmosis or dialysis.

The inks preferably have a total content of dyes from 1 to 35 wt.%, especially from 1 to 30 wt.% and preferably from 1 to 20 wt.%, calculated on the total weight of the paint. As a preferred lower limit is the limit of 1.5 wt.%, preferably 2 wt.% and especially 3 wt.%.

Paints may contain miscible with water and organic solvents, for example, With1-C4alcohols, such as methanol, ethanol, n-propanol, isopropanol, n-butanol, sec-butanol, tert-butanol and Isobutanol; amides, e.g. dimethylformamide and dimethylacetamide; ketones or ketaspire, for example acetone and datetoday alcohol; ethers, e.g. tetrahydrofuran and dioxane; nitrogen-containing heterocyclic compounds, for example N-methyl-2-pyrrolidone and 1,3-dimethyl-2-imidazolidone; polyalkylene glycols such as polyethylene glycol and polypropyleneglycol; C2-C6alkalophile and thioglycol, such as ethylene glycol, propylene glycol, butyleneglycol, triethylene glycol, thiodiglycol, hexyleneglycol and diethylene glycol; other polyols, such as glycerol and 1,2,6-hexanetriol; and (C1-C4alkalemia ethers, polyhydric alcohols, for example 2-methoxyethanol, 2-(2-methoxyethoxy)ethanol, 2-(2-ethoxyethoxy)ethanol, 2-[2-(2-methoxyethoxy)ethoxy]ethanol and 2-[2-(2-ethoxyethoxy)ethoxy]ethanol; preferably N-methyl-2-pyrrolidone, diethylene glycol, glycerol or especially 1,2-propylene glycol, usually in an amount of from 2 to 30 wt.%, especially from 5 to 30 wt.% and preferably about is 10 to 25 wt.%, calculated on the total weight of the paint.

Paints can also contain soljubilizatory, for example ε-caprolactam.

Paints may contain thickeners of natural or synthetic origin, among other things, for the purpose of regulating the viscosity.

Examples of thickeners that can be specified include commercially available alginate thickeners, ethers, starch or ethers flour carob, especially sodium alginate as such or in a mixture with modified cellulose, such as methylcellulose, ethylcellulose, carboxymethyl cellulose, hydroxyethyl cellulose, methylhydroxyethylcellulose, hydroxypropylcellulose or hypromellose, particularly preferably 20-25 wt.% carboxymethylcellulose. Synthetic thickeners which can be selected are, for example, synthetic thickeners based on poly(methyl)acrylic acid or poly(meth)acrylamides.

Paints contain thickeners, for example, in amounts of from 0.01 to 2 wt.%, especially from 0.01 to 1 wt.% and preferably from 0.01 to 0.5 wt.% calculated on the total weight of the paint.

Paints can also contain buffer substances such as borax, borates, phosphates, polyphosphates or citrates. Examples that can be specified include borax, sodium borate, sodium tetraborate, sodium dihydrophosphate, mo is gidrofosfat sodium, sodium tripolyphosphate, Pentapolis sodium and sodium citrate. They are used especially in quantities of from 0.1 to 3 wt.%, preferably from 0.1 to 1 wt.%, calculated on the total weight of the ink, to establish a pH of, for example, from 4 to 9, especially from 5 to 8.5.

As the following additives paints may contain surfactants or moisturizers.

Suitable surfactants include commercially available anionic or nonionic surfactants. As humidifiers in the inks according to the invention consider, for example, urea or a mixture of sodium lactate (mainly in the form of 50-60%aqueous solution) and glycerol and/or propylene glycol in amounts of preferably from 0.1 to 30 wt.%, especially from 2 to 30 wt.%.

The preferred inks have a viscosity of from 1 to 40 MPa, especially from 1 to 20 MPa and preferably from 1 to 10 MPa.

Paints can also contain conventional additives, such as protivovspenivayushchie agents or especially substances that inhibit the growth of fungi and/or bacteria. Such additives are usually used in amounts of from 0.01 to 1 wt.% calculated on the total weight of the paint.

Paint can be obtained in the usual way by mixing together the individual components in the desired amount of water.

Paints according to the invention ablauts is particularly suitable for use in the systems of registration (printing) type in which the paint is squeezed out of the little hole in the form of drops which are directed to the substrate on which is formed the image. Suitable substrates are, for example, paper, textile fibrous material or film plastics. Suitable printing systems are, for example, commercially available inkjet printers for use in printing on paper or textiles or recording device, such as a pen with a reservoir or ballpoint pens and especially inkjet printers.

Depending on the nature of paint application may be necessary if you want to modify, for example, viscosity or other physical properties of the ink, especially properties that affect its affinity in relation to the substrate.

As examples of paper that you can print inks according to the invention, it is possible to specify a commercially available inkjet paper, photo paper, glossy paper, paper coated with plastics, such as inkjet paper Epson photo paper Epson glossy paper Epson glossy film Epson, special inkjet paper HP glossy photo paper, Encad and photo paper IIford. Film plastics, which can be printed inks according to the invention are, for example, transparent or opaque/dark. Suitable plastics films are the two who are, for example, a transparent film of 3M.

As a textile fibrous materials in the context considered, for example, nitrogen-containing or hydroxy-group containing fibrous materials, such as fibrous textile materials made of cellulose, silk, wool or synthetic polyamides, preferably from cellulose.

The present invention accordingly relates also to a method of printing textile fibre materials, paper or plastics films, preferably fibrous textile material or paper and especially textile fibre materials, method of inkjet printing, which used water-based paint containing the active dye of formula (1), and for B, G, R1, R2, R3, R4, R5, R6, R7, R8, R9X1X2, h and j are used above the corresponding values and preferred values.

In the method of inkjet printing, individual ink droplets sprayed on the substrate is adjustable by way of the nozzle. For this purpose apply mainly the way a continuous supply of ink jet and drop-on-demand”. In the way a continuous supply of ink jet droplets are formed continuously and any drops that are not required for printing are transferred to the accumulating vessel and are recirculated, while in the method drop-on-demand” cap is like served and printing is carried out, when you want; in other words, droplets are formed only when needed for printing. The formation of droplets can be performed, for example, by means of a head piezotronic printing ink or by means of thermal energy (drip spray). Preference is given to print using head piezotronic printing method printing ink according to the invention. In addition, preference is given to printing according to the method of continuous ink jet printing inks for the method according to the invention.

Write, for example printing, which receive, are particularly high degree of color intensity and brightness of color, and good properties of resistance to the action of light and moisture.

The following examples serve to illustrate the invention. If not otherwise indicated, temperatures are given in degrees Celsius, parts are weight parts and percentages are by mass %. Mass parts belong to surround the parts in relation to kilograms to litres.

Example 1

(a) 10.0 mmol of monoethanolamine #1, which is in the form of its free acid corresponds to the formula

monoethanolamine #1

and 0.025 g of sodium tripolyphosphate is dissolved in 250 ml of water at 0°C and pH 7 by careful addition of an aqueous sodium hydroxide solution (30%). The resulting mixture is Hledat to -2°C by adding 50 g of ice and then at this temperature is added slowly at 13.0 mmol of foramerica cyanuric acid under vigorous stirring. During the addition the temperature of the support at 0°C and the pH is maintained within the range from 6 to 7 using aqueous sodium hydroxide solution. The first stage of condensation is completed by stirring the reaction mixture at pH 6 for an additional 30 minutes at a temperature of from 0 to 2°C. the resulting reaction mixture contains as its main component, the first product of condensation, which is in the form of its free acid corresponds to the formula

(b) To the reaction mixture, obtained according to stage (a), added dropwise a neutral aqueous solution of 10.3 mmol 1,2-Propylenediamine. During the addition the temperature of the support at 0°C and pH support of 6.5 by means of an aqueous solution of sodium hydroxide (30%). After complete addition, the temperature of the reaction mixture is allowed the opportunity to rise to 20°C and the reaction completed by additional stirring for another hour at pH 6.5 and 20°C. the resulting reaction mixture contains as its main product, which is in the form of the free acid corresponds to the formula

(C) To the reaction mixture, obtained according to stage (b), add 15.0 mmol of the primary condensation product, which is in the form of the free acid corresponds to the formula

if t is mperature from 30 to 35°C. while maintaining a pH in the range of 7.0 to 7.5. The first condensation product obtained by transformation of monoethanolamine #2, which is in the form of the free acid corresponds to the formula

monoethanolamine #2

with foramerica cyanuric acid by analogy with stage (a), as described above. After completion of the condensation reaction ventiliruemye β-sulphatoethyl groups meet increasing pH of the reaction mixture up to 11 with sodium hydroxide solution (30%) and stirring for 15 minutes at a temperature of from 30 to 35°C. Then the pH of the reaction mixture adjust to 7.5 careful addition of hydrochloric acid (32%). The resulting mixture absoluut for two hours with the use of membranes for dialysis and then lyophilized. Get 21,4 g of the product, the crude dye, the main component of which is in the form of the free acid corresponds to the compounds of the formula

max: 419 nm). Which is the product of the dye dyes cotton in Golden yellow color, has a high degree of fixation and good toughness properties for all indicators, in particular the resistance in the wash.

Example 2

Product, the main component of which is in the form of the free acid corresponds to the formula

max: 419 nm), can be obtained by repeating the procedures specified in the above example 1, but using instead of monoethanolamine #1 in stage (a) monotonicity #2 and used in stage (C) instead of the first product of the condensation of foramerica cyanuric acid and monoethanolamine #2 first product of condensation of foramerica cyanuric acid and monoethanolamine #1. Which is the product of the dye dyes cotton in Golden yellow color, has a high degree of fixation and good toughness properties for all indicators, in particular the resistance in the wash.

Examples 3-7

The following dyes, each of which dyes cellulose in a Golden-yellow color with good strength properties in all indicators, can be obtained in a manner analogous to the method described in example 1.

The dye dyes cotton in Golden yellow color, has a high degree of fixation and good toughness properties for all indicators, in particular the resistance in the wash.

Example 8

(a) 10.0 mmol of monoethanolamine #1 and 10.0 mmol of monoethanolamine #2, which is in the form of their free acids correspond to the formula above, is dissolved in 500 ml of water at 0°C and pH 7.5 cautious addition of aqueous sodium hydroxide solution (30%). To p is obtained mixture is added 1.0 g of sodium tripolyphosphate and 100 g of ice and the mixture allow to cool down to -2°C. At this temperature, slowly add 30.0 mmol of foramerica cyanuric acid under vigorous stirring. While adding pH support 6 by means of an aqueous solution of sodium hydroxide. The first stage of condensation is completed by stirring the reaction mixture for an additional 30 minutes at a temperature of from 0 to 2°C.

(b) To the reaction mixture, obtained according to stage (a), added dropwise a neutral aqueous solution of 10.0 mmol of 1,2-Propylenediamine. During the addition the temperature of the support at 0°C and pH support when 9,0 using an aqueous solution of sodium hydroxide (30%). After complete addition, the reaction temperature give the opportunity to rise to 20°C and the reaction is completed by further stirring for another hour at pH 9.0 and 20°C. Ventiliruemye β-sulphatoethyl groups meet increasing pH of the reaction mixture up to 11 with sodium hydroxide solution (30%) and stirring for 15 minutes at a temperature of from 30 to 35°C. Then the pH of the reaction mixture adjust to 7.5 careful addition of hydrochloric acid (32%). The resulting mixture absoluut for two hours with the use of membranes for dialysis and then lyophilized. Get to 20.0 g of the product, the crude dye which in the form of the free acid corresponds to a mixture of compounds of formulas(101), (102),

/p>

max: 419 nm). The mixture of dyes dyes cotton in Golden yellow color, has a high degree of fixation and good toughness properties for all indicators, in particular the resistance in the wash.

Dyeing to exhaustion bath: fabric tights injected at 60°C in an aqueous dye bath with respect to the liquid 1-10, and the liquid contains a quantity of the dye obtained according to example 1, and sodium chloride indicated in the table 1.

Table 1
The composition of the dye bath 1-6, containing the dye of example 1
The dyeing bath123456
%* dye0,51,02,04,06,08,0
Sodium chloride [g/l]40506090 100100
Sodium carbonate [g/l]101214181818
* % dye relative to the weight of the cotton fabric

After 45 minutes at 60°C add calcinated sodium carbonate in the amount indicated in table 1. The dyeing continued for 45 minutes. Painted articles are then rinsed with water, washed in a soap solution and rinsed again and then dried.

Coloring ability of the obtained dyes in dye baths 1-6 were measured photospectrometry way. Table 2 shows the ability to build color of the dye obtained according to example 1. The dye showed a very good ability to build up color.

Table 2
The ability to build color: dependence of the standard color depth (RD) on the concentration of dye
% dye00,51,04,06,08,0
RD dye of example 100,511,011,742,532,532,65

The procedure of dyeing I

100 parts of cotton fabric injected at 60°C in 1500 parts of a dye bath containing 45 g/l of sodium chloride and 2 parts of active dye obtained according to example 1. After 45 minutes at 60°C. add 20 g/l of anhydrous sodium carbonate. The dyeing continued for an additional 45 minutes at the same temperature. Painted articles are then rinsed, washed with boiling for a quarter of an hour nonionic detergent, rinsed again and dried.

Alternatively, the above-mentioned procedure, the dyeing can be carried out at 80°C instead of 60°C.

The dyeing procedure II

0.1 part of the dye according to example 1 are dissolved in 200 parts of water and add 0.5 parts of sodium sulfate, 0.1 part of an aid to alignment of the dye (based on the condensation products of a higher aliphatic amine and ethylene oxide) and 0.5 part of sodium acetate. the pH then adjust to values is a 5.5 with acetic acid (80%). The dye bath is heated at 50°C for 10 minutes and then add 10 parts of wool fabric. Heating is then carried out over a period of approximately 50 minutes to a temperature of 100°C. and dyeing is carried out at the same temperature for 60 minutes, after which the dye bath allow to cool to 90°C and coated products are removed. Woolen fabric was washed with hot and cold water and then twisting and dried.

Procedure print I

3 parts of the dye obtained according to example 1, sprinkle with rapid stirring to 100 parts of the finished thickener containing 50 parts of 5%of thickener sodium alginate, 27.8 parts of water, 20 parts of urea, 1 part of m-nitrobenzenesulfonate sodium and 1.2 parts of sodium bicarbonate. Thus obtained printing paste is used for printing on cotton fabric and the resulting printed material is dried and zaparivajut in a saturated water vapor for 2 minutes at 102°C., the Printed fabric is then rinsed, if necessary, washed in a soap solution by boiling and rinsed again and then dried.

The printing procedure II

(a) Mercerized Gros-grain satin plus with liquid containing 30 g/l of sodium carbonate and 50 g/l of urea (absorption liquid 70%)and dried.

(b) On half-silk satin, pre is sustained fashion treated according to stage (a), printed using water-based ink containing

- 15 wt.% active dye of formula (101) according to example 1

- 15 wt.% 1,2-propylene glycol and

- 70 wt.% water,

with the use of a head for ink-jet printing method “drop-on-demand” technology (drip spray). Printed material is completely dried and the dye is fixed in a saturated water steam at 102°C for 8 minutes, rinse without heating, washed with copaceni, rinse again and dry.

1. Active dye of the formula

in which
B represents a radical of the formula-CH2-CH(R12)- or -(R12)CH-CH2-, in which R12represents a C1-C4alkyl,
R5represents hydrogen or sulfo,
Z1represents for fiber reactive group of the formula
or
,
R7represents amino,
R8represents a C2-C4alkanolamine or ureido,
X1and X2represent, each independently, fluorine or chlorine,
k is the number 2 or 3,
l is the number 2 or 3 and
Y is vinyl or β-sulphatoethyl.

2. Active dye under item 1, which
one of the radicals X1and X2represent fluorine, and the other of the radicals is s X 1and X2represent chlorine.

3. Active dye under item 1, which
X1and X2represent fluorine.

4. The method of obtaining the active dye according to any one of paragraphs.1-3, in which each of the compounds of formulas

and

subjected to reaction with one another of them in a suitable order, where B, R5, R7, R8X1X2, Z1and k have the meanings specified in paragraph 1.

5. The use of active dye according to any one of paragraphs.1-3 or active dye obtained under item 4, when the dyeing or printing hydroxy-group containing or nitrogen-containing fibrous materials.

6. Application under item 5, in which the cellulose fiber materials, particularly those containing cotton fibrous material, color or type.

7. Water-based paint containing the active dye of formula (1) under item 1.

8. A method of printing textile fibre materials, paper or plastics films by the method of inkjet printing, which includes the use of water paints on p. 7.



 

Same patents:

FIELD: chemistry.

SUBSTANCE: invention relates to reactive metal-complex azo dyes, specifically to reactive dyes of formula where R1 is hydrogen, (R2)5 is a nitro group, X is chlorine, T is a radical of formula , ,

or

,

where (R3)0-2 -0, Z is a vinyl or -CH2-CH2-U, U is a group removable in an alkaline medium, Q - -CH(Hal)-CH2-Hal or -C(Hal)=-CH2, Hal is a halogen, s equals 0 or 1.

EFFECT: disclosed dyes have high resistance to wet processing, especially when dyeing or printing synthetic polyamide fibre materials.

7 cl, 12 ex

The invention relates to the synthesis of monoisocyanates, in particular to new connections - dinatrium salts 4-sulfondiethylmethane-2-X-4'-amino-N-metalsalt-2'-Y-azobenzene with versatility for dyeing wool, nylon, cotton and cotton-Dacron materials and natural leather and printing of cotton, Dacron and cotton Mylar material

The invention relates to dyeing and finishing production of textile and knitting industry and can be used in the finishing of fabrics and knitted fabrics of cellulose fibers

FIELD: chemistry.

SUBSTANCE: invention relates to compositions for obtaining electroconductive coatings on substrates surface. Described is a printing composition for obtaining the electroconductive coatings based on silver particles dispersed in water. The composition contains: a) from 5 to 40 wt.p. of metal silver particles with an effective diameter from 10 to 150 nm, with the silver particles having bimodal distribution of particles by sizes; from 50 to 99.5 wt.p. of water and, if necessary, to 30 wt.p. of a solvent; c) from 0.01 to 15 wt.p. of a dispersing agent; d) from 0 to 5 wt.p of additives; e) from 0 to 5 wt.p. of electroconductive, if necessary, water-soluble, polymers; f) from o.5 to 5 wt.p. of a thickening agent; g) from 30 to 70 wt.p. of silver particles or silver-coated copper particles with an effective diameter from 500 nm to 10 mcm. The composition has a viscosity, at least, 1 Pa·s. Also described is the application of the composition for obtaining the electroconductive coatings, method of obtaining current-conductive paths and a polymer substrate with the electroconductive coating from the claimed composition.

EFFECT: invention provides an effective elctroconductivity of electroconductive structures on thermally stable surfaces with the application of offset printing and screen printing.

15 cl, 2 ex

FIELD: chemistry.

SUBSTANCE: invention can be used for inkjet printing. A porphyrazine colorant or its salt is represented by formula (1), where rings A-D each independently represents a benzene ring or a 6-membered nitrogen-containing heteroaromatic ring. E represents alkylene, X represents sulfo-substituted group aniline or the like, which can additionally have a substituent, R1 represents C1-C6 alkyl group, b equals to 0.00 or more and less than 3.90, as the average value, c equals to 0.10 or more and less than 4, as the average value, and the sum of b and c equals to 1.00 or more and less than 4.00, as the average value. The composition of colorant for inkjet printing, which contains the porphyrazine colorant or its salt.

EFFECT: invention makes it possible to obtain the composition of a colorant, which has good shade, possesses excellent properties of various types of resistance, in particular, ozone resistance, provides a possibility of high density of printing, possesses properties which almost do not produce a bronze tint effect.

21 cl, 5 tbl, 17 ex

FIELD: printing.

SUBSTANCE: invention relates to an ink set containing chromophoric metals for digital printing on ceramic materials. The ink set comprises liquid colouring compositions (A), (B), (C) and one from (D) and (E). The (A) comprises at least a compound of cobalt. The (B) comprises at least a compound of iron. The (C) comprises at least a compound of a metal selected from chromium, nickel and their mixtures. The (D) comprises at least a compound of cobalt and at least a compound of iron. The (E) comprises one or more compounds of zirconium. The said metal compounds decompose at a temperature of from 500 to 1300°C. When interacting with the ceramic material the metal compounds of compositions (A)-(D) form colured oxides or colured compounds. The compounds of zirconium from the composition (E) with the ceramic material form white oxides or white compounds. Also the method of decorating ceramic materials by digital printing using the specified set of ink and the decorated ceramic products produced using this method are described.

EFFECT: invention provides ceramic materials decorated with digital printing of wide range of colours with the effect of natural stone.

11 cl, 45 tbl, 5 ex

Conductive pastes // 2509789

FIELD: chemistry.

SUBSTANCE: invention relates to conductive pastes for forming metal contacts on the surface of substrates for photovoltaic cells. The conductive paste is substantially free of frit glass. According to one version of the invention, the conductive paste contains organometallic components which form a solid metal oxide phase upon firing and conductive material. The organometallic components are selected from a group which includes metal carboxylates or metal alkoxides, where the metal is boron, aluminium, silicon, bismuth, zinc or vanadium. According to another version, the conductive paste includes multiple precursors which form conductive elements upon firing or heating. The paste is adapted for adhesion to the surface of a substrate and upon firing, forms a solid oxide phase while forming an electrical conductor from conductive materials on the substrate.

EFFECT: use of said conductive paste in a line of a conductive array of photovoltaic cells provides high efficiency and fill factor of the photovoltaic cell.

14 cl, 2 tbl, 2 ex

FIELD: chemistry.

SUBSTANCE: composition for making sensor coatings contains antimony-doped tin dioxide of the formula SbxSn1-xO2, where x=0.1-0.3, and water in ratio SbxSn1-xO2:H2O = 89-87:11-13 wt %. The method of preparing the composition involves hydrothermal treatment of tin and antimony hydroxides at 170°C for 48 hours. The tin and antimony hydroxides are obtained by dissolving Sn and Sb metal in concentrated hydrochloric acid, 18-20 wt %, while adding 3-5 wt % concentrated HNO3. The obtained solution is 2-3 times diluted with distilled water and a calculated amount of ammonia solution is added. Using a simple scheme, the disclosed method enables to obtain nanoparticles of said composition SbxSn1-xO2 with size of 30 nm and surface area of 154 m2/g, which can be used as the basic component of electroconductive ink for printing sensor arrays and microcontacts.

EFFECT: low labour and power consumption.

3 cl, 6 dwg, 3 ex

PRINTING PRODUCT AND METHOD OF ITS MANUFACTURING

FIELD: chemistry.

SUBSTANCE: conductive paste contains frit glass, a conductive material, an organic medium and one or more organometallic components which form metal oxides when burnt. The organometallic components are selected from a group comprising a metal carboxylate and a metal alkoxide, where the metal is boron, aluminium, silicon, bismuth, zinc or vanadium. When deposited on antireflecting coating on a substrate, the conductive paste is capable of penetrating the coating to form an ohmic contact with the substrate. Described also is a photovoltaic cell, having a semiconductor substrate, an antireflecting coating and lines of a conductive mesh formed from said conductive paste.

EFFECT: high efficiency of the photovoltaic cell, improved adhesion and ohmic contact between metallic elements and the substrate through antireflecting coatings.

10 cl, 1 tbl, 2 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to use of a composition which contains: a) 0.1-20 wt % binder which contains a polycarbonate derivative based on geminally disubstituted dihydroxydiphenyl cycloalkane, b) 30-99.9 wt % solvent, c) 0-10 wt %, with respect to dry mass, dye or mixture of dyes, d) 0-10 wt % functional material or mixture of functional materials, e) 0-30 wt % additives and/or auxiliary substances or a mixture thereof, as jet printing ink. The invention also relates to a method of producing a composite and a composite which contains a polymer layer on which there is a jet printing layer of said composition.

EFFECT: invention is aimed at producing agents which enable to use jet printing in making counterfeit protected documents and/or valuable documents based on polycarbonate layers, and which enable to deposit jet printing layers on layers which meet all optical requirements, which can be coloured, wherein lamination does not deteriorate optical properties of the layers and said layers do not act as a separating layer and facilitate formation of a monolithic composite.

31 cl, 2 tbl, 2 dwg, 8 ex

FIELD: chemistry.

SUBSTANCE: invention relates to jet printing inks, particularly non-aqueous inks for jet printing. The ink for jet printing contains a pigment, binder, polyetheramide resin as a pigment dispersant, an organic solvent and an anti-corrosion agent from an imidazole group or a group of volatile anti-corrosion agents, preferably dicyclohexylamine or cyclohexylammonium cyclohexylcarbamate.

EFFECT: disclosed inks have high dispersion stability and prevent corrosion of print heads of jet printers and nozzle clogging.

8 cl, 8 tbl, 34 ex

FIELD: food industry.

SUBSTANCE: proposed print compound in the form of print ink or print varnish includes a binding substance with a resinous component and a solvent component. The binding substance solvent represents a one-component or multicomponent saturated resin solvent and a food product or food additive of a number of monoglycerides and/or diglycerides and/or triglycerides. Preferably, the binding substance solvent component includes acetylated or esterified monoglycerides and/or acetylated or esterified diglycerides and/or acetylated or esterified triglycerides.

EFFECT: print ink solvent migration degree reduction and treatment simplification in view of the possibility of the print compound drying-out by way of absorption and re-varnishing exclusion.

4 cl, 3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to novel reactive dyes for dyeing or printing on fibrous textiles. Reactive dye of formula where R1 -optionally substituted C1-C4alkyl, R2 - sulfo group, Z1 -SO2-Y, -CO-NH-(CH2)k-SO2-Y, -NH-CO-CH(Hal)-CH2-HaI or -NH-CO-C(Hal)=CH2, where Hal - chlorine or bromine atom, Y - vinyl or -CH2CH2-U, U - an alkali-removable group, k - a number equal to 2, 3, 4, 5 or 6; n - a number equal to 0, 1 or 2; m - a number equal to 0 or 1, is described.

EFFECT: dyeing of hydroxyl-containing or nitrogen-containing fibrous materials with high colourability and good strength properties.

5 cl, 10 ex

FIELD: physical analytical methods.

SUBSTANCE: invention relates to bioanalytical methods involving dye-labeled indicators. Bioanalytical method without separation is provided directed to measure analyte obtained from biological liquid or suspension, wherein are used: analyte microparticles as first biospecific reagent; and second biospecific reagent labeled with biphotonic fluorescent dye based on dipyrromethene boron difluoride containing at least one water solubility imparting group selected from ammonium salt and sulfonic or carboxylic acid alkali metal salt and at least one chemically active group selected from carboxylic acid, reactive carboxylic acid ester, carboxylic acid anhydride, maleimide, amine and isothiocyanate. In the method of invention, laser is focused onto reaction suspension and biphotonically excited fluorescence from individual microparticles (randomly flowing or oriented by pressure provided by emission of exciting laser through focal volume of laser beam).

EFFECT: increased efficiency of bioanalyses.

5 cl, 5 dwg, 5 tbl, 25 ex

FIELD: chemistry.

SUBSTANCE: invention relates to novel active dyes, methods of their obtaining and their application in dyeing or printing textile fibrous materials. An active dye of formula in which B represents a radical of formula -CH2-CH(R12)- or -(R12)CH-CH2-, in which R12 represents C1-C4alkyl, R5 represents hydrogen or sulpho, Z1 represents a fibre-reactionable group of formula -SO2-Y (3a) or -NH-CO-(CH2)l-SO2-Y (3b), R7 represents amino, R8 represents C2-C4alkanoylamino or ureido, X1 and X2 represent, each independently on the other, fluorine or chlorine, k equals a number 2 or 3, l equals a number 2 or 3 and Y represents vinyl or β-sulphatoethyl.

EFFECT: invention makes it possible to obtain the improved active dyes with high reaction ability, chemical affinity, as well as with good dyeability with a high degree of fixation.

8 cl, 2 tbl, 8 ex

FIELD: chemistry.

SUBSTANCE: invention relates to novel active dyes, methods of their obtaining and their application in dyeing or printing textile fibrous materials. An active dye of formula in which B represents a radical of formula -CH2-CH(R12)- or -(R12)CH-CH2-, in which R12 represents C1-C4alkyl, R5 represents hydrogen or sulpho, Z1 represents a fibre-reactionable group of formula -SO2-Y (3a) or -NH-CO-(CH2)l-SO2-Y (3b), R7 represents amino, R8 represents C2-C4alkanoylamino or ureido, X1 and X2 represent, each independently on the other, fluorine or chlorine, k equals a number 2 or 3, l equals a number 2 or 3 and Y represents vinyl or β-sulphatoethyl.

EFFECT: invention makes it possible to obtain the improved active dyes with high reaction ability, chemical affinity, as well as with good dyeability with a high degree of fixation.

8 cl, 2 tbl, 8 ex

FIELD: physical analytical methods.

SUBSTANCE: invention relates to bioanalytical methods involving dye-labeled indicators. Bioanalytical method without separation is provided directed to measure analyte obtained from biological liquid or suspension, wherein are used: analyte microparticles as first biospecific reagent; and second biospecific reagent labeled with biphotonic fluorescent dye based on dipyrromethene boron difluoride containing at least one water solubility imparting group selected from ammonium salt and sulfonic or carboxylic acid alkali metal salt and at least one chemically active group selected from carboxylic acid, reactive carboxylic acid ester, carboxylic acid anhydride, maleimide, amine and isothiocyanate. In the method of invention, laser is focused onto reaction suspension and biphotonically excited fluorescence from individual microparticles (randomly flowing or oriented by pressure provided by emission of exciting laser through focal volume of laser beam).

EFFECT: increased efficiency of bioanalyses.

5 cl, 5 dwg, 5 tbl, 25 ex

FIELD: chemistry.

SUBSTANCE: invention relates to novel reactive dyes for dyeing or printing on fibrous textiles. Reactive dye of formula where R1 -optionally substituted C1-C4alkyl, R2 - sulfo group, Z1 -SO2-Y, -CO-NH-(CH2)k-SO2-Y, -NH-CO-CH(Hal)-CH2-HaI or -NH-CO-C(Hal)=CH2, where Hal - chlorine or bromine atom, Y - vinyl or -CH2CH2-U, U - an alkali-removable group, k - a number equal to 2, 3, 4, 5 or 6; n - a number equal to 0, 1 or 2; m - a number equal to 0 or 1, is described.

EFFECT: dyeing of hydroxyl-containing or nitrogen-containing fibrous materials with high colourability and good strength properties.

5 cl, 10 ex

FIELD: chemistry.

SUBSTANCE: invention relates to novel active dyes, methods of their obtaining and their application in dyeing or printing textile fibrous materials. An active dye of formula in which B represents a radical of formula -CH2-CH(R12)- or -(R12)CH-CH2-, in which R12 represents C1-C4alkyl, R5 represents hydrogen or sulpho, Z1 represents a fibre-reactionable group of formula -SO2-Y (3a) or -NH-CO-(CH2)l-SO2-Y (3b), R7 represents amino, R8 represents C2-C4alkanoylamino or ureido, X1 and X2 represent, each independently on the other, fluorine or chlorine, k equals a number 2 or 3, l equals a number 2 or 3 and Y represents vinyl or β-sulphatoethyl.

EFFECT: invention makes it possible to obtain the improved active dyes with high reaction ability, chemical affinity, as well as with good dyeability with a high degree of fixation.

8 cl, 2 tbl, 8 ex

FIELD: protection coatings.

SUBSTANCE: invention aims at protecting bank notes and security papers against counterfeiting. Optically changing pigment contains interferential multilayer structure including light-transmitting dielectric layer having at least one luminescent material. Dielectric layer is selected from of rare-earth metal, bismuth, and principal group III element trifluorides; of principal group II element difluorides; mixtures thereof; organic or organometallic compounds. Luminescent material should be selected from organic or organometallic compounds containing transition or rare-earth metal ions. Above-defined structure may contain one or more semitransparent, partly reflecting layers, one or more nontransparent, fully reflecting layers, and one or more conducting layers. Pigment is prepared by a method including physical or chemical precipitation of the dielectric layer.

EFFECT: preserved proper properties of color shift, increased reliability of protection, and ensured identification simplicity at relatively low cost.

30 cl, 1 tbl, 9 ex

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