Prom the shape of the optical brightener

C09B67/42 - Preparations of dyes not provided for in a single one of groups ; C09B0067240000-C09B0067400000


The invention relates to exhaust the forms of optical brighteners, designed for optical bleaching of cellulosic textile materials and paper. Describes the final form of the optical Brightener, including Mac. h: optical Brightener creatinineclearance number 100, a direct dye blue range of 0.05 to 0.15, a direct dye green range of 0.001-0.05 and direct red dye range from 0.01 to 0.0001. Effect: whitening ability of the proposed optical bleach (PA) increased 2.2 times in comparison with known CV containing a mixture of direct blue and blue acid dye, an undesirable reddish hue of white is changed to blue or neutral. 5 C.p. f-crystals, 1 table.

The invention relates to the production of final forms of optical whitening agents (ALE) based on fluorescent derivatives of 4,4'-bis-(1,3,5-triazine-2-yl-amino)-stilbene-2,2'-disulfonate intended for optical bleaching of cellulosic textile materials and paper.

Cellulose fibers are characterized by a greater or lesser yellow due to the presence of colored compounds [1, 2]. Wrong tone can be mitigated by using tint is durable KU, direct violet, acid blue, acid violet, basic violet To, direct blue fade resistant, acid bright blue antrahinonovye, etc., [3-5] . "Podchinennye" fabric look less yellow, but more dull and gray, because the total amount of light is reduced [6]. This disadvantage is eliminated, if you combine the action of blue dye and a fluorescent Brightener. In this case, the fluorescence optical Brightener is superimposed on the reflection of the white material, acting as an additional source of radiation [1, 2].

One of the most widely used ALE used to eliminate the natural yellowing of textile materials, is belfor CD 2: [4,4'-bis(4-aniline-6-morpholino-triazine-2-ylamino)-2,2'-stilbenedicarboxylic, disodium salt (bleach I).

However, this final form has insufficient bleaching ability and gives unwanted reddish tint material.

Eliminating unwanted color white material is achieved through the use of dyes gamma blue [1, 3-5]. After the "bluing" reflectance for all wavelengths is reduced, but to a greater extent for the range of 600-700 nm [6]. Visually perceived is worn white, blue increases [6].

The increase in the radiation absorption material in the range of 600-700 nm leads to a decrease of the reflection coefficient in this region, which increases the share of blue, blue and violet component in the spectrum of reflection [6]. Dyes blue gamma affect the change of the reflectance in a narrow wavelength interval. In order to reduce the reflection coefficient in a wider range, in the patent PRC [7] use temporary colours blue and red scheme. The proposed combination of dyes is not optimal, because it uses a very high relative concentration of dye in the red range, which makes a significant imbalance in the reflection spectrum and reduces the bleaching effect. In the American patents [8-9] proposed to use a combination of colors: blue, red and yellow or blue, red and purple scales, respectively. However, these proposals have a common drawback - the mixing of the individual components is not possible to obtain a white color. To eliminate the deficit and increase the whitening effect allows the use of a combination of dyes of blue, green and red colors. The mixture of dyes of these colors allows parolee optimally balance the reflectance spectrum throughout the visible region. Note, however, that the closer the maximum absorption tinting dye to the maximum fluorescence bleach (416-466 nm), the become more stringent concentration limits [10]. Therefore, the dyes of red and green mix are used in much smaller concentrations than blue.

The objective of the invention is to substantially increase the effectiveness of this fluorescent Brightener, while improving tone white materials, through the use of dyes of blue, green and red mix, add in the final form of the DAE.

The proposed composition of the final form of the DAE is different from the known composition of the fact that it is 100 wt.h. ALE introduced direct dyes, wt.h.: blue range: 0,05-0,15; green range: 0,001-0,05; red range: from 0.01 to 0.0001.

For the final form of the new structure as ALE used connection (bleach I): disodium salt of 4,4'-bis(4-aniline-6-morpholino-triazine-2-ylamino)-2,2'-stilbenedicarboxylic.

By adding dyes blue, green and red gamma whitening ability ALE cotton fabric increases 1.4-2.2 times, improves the shade of white, closer to blue, and the savings dragoste idca final shape of the optical Brightener, containing as a fluorescent derivative of 4,4'-bis[4"-diethanolamine-(p-sulfonanilide)-1,3,5-triazine-2-ylamino] -2,2'-stilbenedicarboxylic in the form of a salt with the addition of urea and diethanolamine (bleach II) [I].

This liquid discharge form has insufficient bleaching ability and creates undesirable reddish shade of white material.

The persistence of whiteness index paper, color is of great importance for the correct transmission of tone and accuracy of color reproduction of printed images.

Adding songs direct dyes blue, green and red scales leads to significantly improve the efficiency of the specified fluorescent Brightener and improve the tone of the white paper.

By adding dyes whitening ability ALE for paper increases 1.4-2.2 times, improves the shade of white, closer to blue or neutral and helps to save expensive optical bleach.

Preparation of final forms-based bleach I and II with the addition of the dyes shown in examples 1-10, 12, and the methodology and results of the whitening ability of the obtained final form in premi "Opton", which was calculated by the formula Berger [1, 5] WRy+3(RzRx), where Rx, Ry, Rzthe Reflectances in the red, green and blue color filters, respectively [1, 5].

Example 1 In a laboratory mixer was loaded with 100 g of bleach, 0.05% of direct turquoise lightfastness (C. I. Direct Blue 86), 0.05% of direct green lightfastness (C. I. Direct Green 26) and 0.01% direct red (C. I. Direct Red 23) (based on 100% by weight ALE). The process of mixing was carried out for one hour. The end of the process of mixing was controlled by sampling, which are then analyzed on the spectrophotometer SF-26.

Bleaching and dyeing of fabric samples was performed in a laboratory washing machine type "Launder - Ometer" when 52oC for 20 minutes. Each tissue sample weight of 1.5 g was placed in a hermetically closed glass pre-loaded with 200 ml of an aqueous solution containing 0.2% bleach (dry cloth). At the end of the bleaching process, the samples were rinsed with water and kept in an oven for 3 minutes at a temperature of 70oC. We obtained tissue samples was measured by the whiteness (W) and reflection spectra in the wavelength range of 400-740 nm. The reflectance spectra of measured on the device Color Eye 7000" company "Gret is topackage (C. I. Direct Blue 106), 0.01% of direct bright green lightfastness G (C. I. Direct Green 28) and 0.001% direct 2C red (C. I. Direct Red 54).

Example 3 Differs from example 1 in that the bleach I added 0.05% of direct pure blue (C. I. Direct Blue 1), 0,001% direct green lightfastness (C. I. Direct Green 96) and 0.0001 direct red lightfastness (C. I. Direct Red 79).

Example 4 Differs from example 1 in that the bleach I added a 0.1% direct turquoise lightfastness, 0,05% direct green lightfastness and 0.01% direct scarlet.

Example 5
Differs from example 2 in that the bleach I added 0.1% of direct bright blue lightfastness, 0.01% of direct bright green lightfastness G and 0.001% direct red 2C.

Example 6
Differs from example 3 that the bleach I added a 0.1% direct pure blue, 0,001% direct green lightfastness With and 0.0001% direct red lightfastness C.

Example 7
Differs from example 6 that the bleach I added to 0.15% direct pure blue, 0.05% of direct green lightfastness With and 0.01 direct red lightfastness C.

Example 8
Differs from example 1 in that the bleach I added to 0.15% direct turquoise lightfastness To 0.01% of direct green lightfastness and 0.001% of Pramogu the nternet bright blue lightfastness, 0,001% direct green lightfastness and 0.0001% direct red 2C.

Example 10
Differs from example 6 that the content of bleach I reduced 2-fold and 0.1% by weight, dry cloth.

Example 11 (control)
Differs from example 1 in that the bleach I does not contain colouring dyes.

Examples 12, 13 (prototype)
Differs from example 1 in that the bleach I contains as a tinting dye is 0.2% direct turquoise lightfastness.

The experimental results are shown in table.

From the table it follows that the use of a combination of dyes of blue, green and red scheme can significantly improve the effectiveness of bleach I. In the absence of a tinting dye (example 11) bleach I provides whiteness index for h/b fabric 133,4% when the content of the bleach of 0.2% (dry cloth). When using a new final form of the DAE with temporary dyes (example 10) whiteness index equal 137,3% when the content of the bleach 0,09% (dry cloth), which allows to reduce the consumption of bleach I 2.2 times. A significant improvement in the whiteness index of cotton fabrics for prototype (example 12) is achieved only by increasing the concentration ALE 2 is ttenone dyes blue, green and red range in amounts of 0.1 g 0.001 g 0.001 g, respectively.

The process of mixing was carried out for one hour at a temperature of 20oWith to dissolve dyes. Control over the completeness of the dissolution of the dyes was carried out by the method of sampling, which were analyzed on a spectrophotometer SF-26. For a complete elimination of mechanical impurities and partially undissolved dye solution was filtered on a suction filter.

The test liquid discharge forms-based bleach II were performed for bleaching paper in bulk according to GOST 27404. Dosage of bleach II was 0.5 to 2.0% (in terms of 100%) of the mass of absolutely dry pulp.

Samples of paper made from pulp containing chemically bleached pulp, rosin size, aluminum sulfate and kaolin. Whiteness index the paper samples was determined using a photoelectric colorimeter "Elrepho".

For bleach II without tinting dyes at the dosage of 1.0% (on the weight of absolutely dry pulp) whiteness index was of 124.7%, and when using a new final form of this ALE (with a tint dyes) in the dosage of 0.5% whiteness index 126,1%, which allows to reduce the consumption of bleach in 2 rates allows to increase the whitening ability of cellulose textile materials and paper 1.4-2.2 times and improves the shade of white. The result is a saving of expensive and scarce optical bleach.

Sources of information
1. Emelyanov, A., Optical bleaching agents and their use in the textile industry. M: Light industry, 1971.

2. B. M. Krasovitsky, B. M. Bolotin. Organic phosphors, M.: Khimiya, 1977.

3. Auth. mon. The USSR 1714013.

4. Auth. mon. The USSR 1714016.

5. RF patent 2081137.

6. I. A. Gorlovka and other Laboratory pigments and pigmented paints, varnishes and lacquers. L.: Chemistry, 1990.

7. Patent PRC 111034.

8. U.S. patent 5131910.

9. U.S. patent 2002/0038484.

10. K. Venkataraman. The chemistry of synthetic dyes. L.: Chemistry, volume VI, 1977.


1. Prom the shape of the optical Brightener for cellulosic textile materials and paper containing optical Brightener creatinineclearance number and color additive, wherein the additive is a composition of direct dyes, including dyes hues of blue, green gamma and the red gamma, in the following ratio, wt.h.:
Optical bleach - 100
Direct blue dye range 0.05 to 0.15
Direct dye green gamma - 0,001 - 0, optical bleach creatinineclearance series - the disodium salt of 4,4'-bis-(4-aniline-6-morpholino-triazine-2-ylamino)-2,2'-stilbenedicarboxylic.

3. Prom the shape of the optical Brightener under item 1, in which the optical Brightener creatinineclearance series - salt of 4,4'-bis-[4"-diethanol-amino-(p-sulfanilic)-1,3,5-triazine-2-ylamino] -2,2'-stilbenedicarboxylic.

4. Prom the shape of the optical Brightener under item 1, in which a direct dye blue gamma selected from the series comprising straight bright blue lightfastness C. I. Direct Blue 106, direct turquoise fade resistant To C. I. Direct Blue 86, direct pure blue C. I. Direct Blue 1.

5. Prom the shape of the optical Brightener under item 1, in which a direct dye green range selected from the group comprising straight green lightfastness C. I. Direct Green 26, direct bright green lightfastness I C. I. Direct Green 28, direct green lightfastness With C. I. Direct Blue 96.

6. Prom the shape of the optical Brightener under item 1, in which a direct dye red range selected from the group comprising a straight red C. I. Direct Red 23, direct red 2, C. I. Direct Red 54, direct red lightfastness With C. I. Direct Red 79.


Same patents:

The invention relates to new compounds of the number of 4,4'-diaminostilbene-2,2'-disulfonic acid, which can be used as fluorescent whitening tools

The invention relates to the chemical industry, in particular to a composition for dyeing fibers in the mass
The invention relates to the production of final forms of optical whitening agents /ALE/ on the basis of fluorescent derivatives of 4,4'-bis/1,3,5-triazine-2-yl-amino/stilbene-2,2'-disulfonate intended for optical bleaching of paper /mass and surface, and cellulosic textile materials

FIELD: organic chemistry, paper industry.

SUBSTANCE: invention relates to compositions used for coating paper covers. Invention describes a composition for coating paper cover comprising whitening pigment comprising: (a) product of melamine formaldehyde or phenol-formaldehyde polycondensation, and (b) water-soluble fluorescent whitening agent of the formula:

wherein R1 and R2 represent independently of one another -OH, -Cl, -NH2, -O-(C1-C4)-alkyl, -O-aryl, -NH-(C1-C4)-alkyl, -N-(C1-C4-alkyl)2, -N-(C1-C4)-alkyl-(C1-C4-hydroxyalkyl)- -N-(C1-C4-hydroxyalkyl)2 or -NH-aryl, for example, anilino-, anilinemono- or disulfonic acid or aniline sulfone amide, morpholino-, -S-(C1-C4)-alkyl(aryl) or radical of amino acid, for example, aspartic acid or iminoacetic acid that is replaced with radical in amino-group; M means hydrogen, sodium, potassium, calcium, magnesium atom or ammonium, mono-, di-, tri- or tetra-(C1-C4)-alkylammonium, mono-, di- or tri-(C1-C4)-hydroxyalkylammonium, or ammonium di- or tri-substituted with a mixture of (C1-C4)-alkyl and (C1-C4)-hydroxyalkyl groups. Covers prepared on coating paper elicit high photostability and enhanced whiteness degree.

EFFECT: improved method for preparing, improved properties of covers.

7 cl, 1 tbl, 3 ex

FIELD: household chemistry, in particular compositions for bleaching of white and random dyeing textile made of natural, artificial, synthetic and mixed fibers.

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EFFECT: non-layered composition during storage; decreased chemical failure of materials.

2 tbl, 12 ex

FIELD: chemistry.

SUBSTANCE: invention concerns fluorescent bleach containing a mix of two asymmetrically substituted and one symmetrically substituted triazinylaminostilbene disulfone acid, a new symmetrically substituted derivative, method of their obtaining, and application of the mix in synthetic or natural organic material (especially paper) bleaching and in fluorescent bleaching and sun resistance boost of textile.

EFFECT: high substantivity and light resistance of the claimed fluorescent bleaches and their mixes, and better water solubility of the claimed mixes in comparison to the solubility of each individual bleach.

15 cl, 2 tbl, 12 ex

FIELD: chemistry, textiles, paper.

SUBSTANCE: present invention relates to new amphoteric bis-triazinylaminostilbene fluorescent whitening agents for fluorescent whitening of organic materials, particularly paper. Description is given of use of compounds with formula (5) for fluorescent whitening of paper.

EFFECT: compounds have high bleaching power; fluorescence is not prevented by cation-active polymers or anion-active fluorescent whitening agents contained in the paper.

2 cl, 2 tbl, 48 ex

FIELD: chemistry.

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EFFECT: high solubility in water and increased stability when storing its aqueous solutions.

4 cl, 3 tbl, 3 ex

FIELD: textile fabrics, paper.

SUBSTANCE: aqueous solutions are related to toluylene optical bleaches and may be used in production of chalk overlay paper of high whiteness. Aqueous solutions contain at least one optical bleach, polyvinyl alcohol, having extent of hydrolysis over 75% and Brookfield viscosity of 2-40 mPa·s, and water. This composition may be used for paper coating. It may be applied on paper after its moulding to produce chalk overlay paper.

EFFECT: provision of stability in storage of aqueous solutions of toluylene optical bleaches and simplified method for production of chalk overlay paper.

9 cl, 3 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to concentrated aqueous solutions of hexa-sulfonated stilbene used optical brighteners. Description is given of an aqueous solution of hexa-sulfonated stilbene optical brightener which is stable during storage with over 0.214 mol/kg content thereof in the solution. The solution does not contain a soluble agent, for example urea. By removing salts formed during synthesis of the optical brightener, its concentration of up to 0.35 mol/kg can be achieved without losing stability during storage. Also described is a method of preparing an aqueous solution of the said optical brightener and its use for bleaching paper or cellulose materials.

EFFECT: high concentration solutions of the said optical brightener do not show crystallisation signs after 2 weeks at 5°C and enables formation of coating compositions with low water content, which reduces energy consumption on drying and reduces penetration of water and adhesive into the paper layer.

10 cl, 1 dwg, 1 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: invention describes an aqueous dispersion of an optical bleaching agent which is stable during storage, does not contain dispersants and stabilisers and contains 20-40% active substance in form of one or more optical bleaching agents obtained through successive reaction of cyanuric chloride with 4,4'-diamino-2,2'- stilbene sulphonic acid, amine and a product of reacting monoethanol amine with acrylamide.

EFFECT: disclosed dispersion of optical bleaching agent does not require dispersants or other stabilising additives to prevent settling during storage and has excellent properties for bleaching paper and other cellulose materials.

8 cl, 2 tbl, 4 ex

FIELD: chemistry.

SUBSTANCE: invention relates to solutions of optical bleaching agents which are stable during storage, based on defined salt forms of aniline-substituted bis-triazinyl derivatives of 4,4'-diaminostilbene-2,2'-disulphonic acid of formula where R denotes a hydrogen atom, R1 denotes a β-hydroxyalkyl radical having 2-4 carbon atoms, R2 denotes a hydrogen atom, M+ denotes Na+, n is less than or equal to 1.5; which do not require additional dissolution promoting additives.

EFFECT: high stability of the compounds during storage.

14 cl, 2 tbl, 6 ex

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EFFECT: increased whiteness.

25 cl, 2 dwg, 2 tbl, 3 ex