Connection triethynylbenzene, methods for their preparation, aqueous compositions containing them, and method for the fluorescent whitening of paper

 

Describes hydrate 4,4'-decreasingly-2,2'-desulfosarcina General formula I, in which M and M1independently represent hydrogen or alkali metal; x is a number ranging from 1 to 30, crystalline form, hydrate I is characterized by x-ray, shown in Fig.1-11; or a mixture containing two or more hydrates of the compounds 4,4'-decreasingly-2,2'-desulfosarcina formula I, and methods for their production and application of new hydrate to obtain a concentrated aqueous compositions of fluorescent whitening agents. 7 C. and 11 C.p. f-crystals, 1 tab., 11 Il.

The invention relates to new hydrates of salts of specific compounds 4,4'-decreasingly-2,2'-desulfosarcina, characterized by the content of their water of hydration; to crystalline forms that have new hydrates and which are distinguished by their x-ray; a process for the production of new hydrates; the application of new hydrates in obtaining the concentrated compositions of fluorescent whitening agents.

Recently, fluorescent whitening agents produce on sale mainly in the form of aqueous solutions or suspensions. To this end, Hugo order to improve the homogeneity, wettability and extend the shelf life of the suspension, there was added dispersing agents and thickeners. Often with these auxiliary ingredients add electrolyte. Despite the presence of such additives, there are limiting concentration for the suspension fluoresceine bleaching agents, over which the suspension is often unstable in storage and has unsatisfactory properties of dosing. Such extreme concentration to play very difficult, since they may be affected by the nature of the potential pre-treatment, which is subjected to a suspension of fluorescent whitening agent. In particular, depending on the nature of pre-processing, you can get different hydrates fluorescent whitening agent with a different crystalline forms.

Unexpectedly it was found that, if used in fluorescent otbelivayushe agent present specific hydrates or mixtures of hydrate having a specific crystal form or more defined crystalline forms, you can get the specific composition of the fluorescent whitening agent with a concentration of active substance more than 30 wt.%, which is stable in the position contain only small amounts of additional ingredients and good for the fluorescent whitening of multiple bases, including textiles and paper.

Accordingly, the present invention provides a hydrate of the compound 4,4'-decreasingly-2,2'-desulfosarcina with the formulain which M and M1independently represent hydrogen or alkali metal, x is a number ranging from 1 to 30, and crystalline form, hydrate, (I) characterizes the radiograph shown in Fig.1-11.

The invention relates also to a mixture containing two or more hydrates of the compounds 4,4'-decreasingly-2,2'-desulfosarcina formula (I).

The preferred hydrates of the formula (I) are compounds in which M and M1both represent hydrogen or sodium, and the hydrates are characterized by x-ray, which is shown in Fig.1-7.

Preferred is a mixture containing several hydrate disodium salt of the compound 4,4'-decreasingly-2,2'-desulfosarcina formula (I).

Other preferred hydrate of compound (I) 4,4'-decreasingly-2,2'-desulfosarcina are hydrates, in which both M and M1are potassium, while the hydrate is characterized by x-ray, shown in Fig.8, and x represents a number from 9 to 17, and hydrates, in which both M and M1presented the two or more hydrates of the compounds 4,4'-decreasingly-2,2'-desulfosarcina formula (I), thus M and M1- lithium, and in which x represents a number of from 9 to 30.

Appropriate radiographs in Fig.1-11 obtained using a powder diffractometer X'pert (Philips, Almelo) in the geometry of reflection and C-radiation. Control x-rays for crystal form (Fig.1) and With (Fig. 2) measured in suspensions in air atmosphere without control of relative humidity. Measuring a reference radiographs for crystal form D (Fig.3), E (Fig. 4), F (Fig. 6) and G (Fig.7) and x-rays dallievas salt (Fig.8) also hold in suspension, under nitrogen atmosphere with maintaining the relative humidity at the level of 80-90%, and radiographs of the three types of crystals deliciious salt (Fig.9-11), and x-ray crystal forms (Fig.5) did in the solid state. In each of the drawings 1-11 shows part of the measurement section 2T within the 1o-30o.

Each of the new hydrate of formula (I) has a distinctive x-ray.

The crystal forms a, b, C, D, E, F and G, and the crystals dallievas and lithium salts are, for the most part, of one or more hydrates of the formula (I) in which x is a number between 1 and 30.

The amount of water of hydration can be determined by differential thermal analysis or Dina isoWith, or subsequent water analysis by methods such as titration according to Karl Fischer, thermogravimetric analysis or loss on drying at elevated temperature.

Hydrate disodium salt of 4,4'-decreasingly-2,2'-desulfosarcina with crystals of crystalline form (A) can be obtained by successive reaction of chloride cyanuric acid disodium salt dissolvability 4,4'-diaminostilbene, aniline and diethanolamine, bringing the pH of the mixture to 9.0 to 9.5 with concentrated sodium hydroxide solution and evaporating the mixture to dryness. If before treatment with sodium hydroxide connection to isolate in the form of the free acid, the result is a hydrate having a crystalline form F.

Hydrate crystalline form can be obtained by neutralization of the free acid 4,4'-decreasingly-2,2'-desulfosarcina with hydrate crystalline form a diluted sodium hydroxide solution, homogenization and aged at room temperature; the crystalline hydrate form D - treatment of sodium salt of 4,4'-decreasingly-2,2'-desulfosarcina with hydrate crystalline form And an aqueous solution of sodium chloride, stabilization and homogenization; and the crystalline hydrate is eskay form a concentrated sodium hydroxide solution and homogenization. Hydrate crystalline form G can be obtained from the crystalline form E trim in a closed reactor at elevated temperature.

In addition, the crystalline hydrate form can be obtained by priming water suspension of the free acid seed crystals of the hydrate crystalline form C. This technology has the advantage that it is possible to use concentrations of the active substance is more than 30 wt.%, preferably 30-50 wt.%, and thus the suspension obtained has the desired concentration and does not require further concentration.

Hydrate crystalline form D according to Fig.3 or hydrate crystalline form E with the radiograph in Fig.4 can also be obtained by the technology of the seed described in connection with obtaining a hydrate crystalline form C.

In a preferred embodiment, a mixture of several new hydrate of formula (I) are controlled by mixing an aqueous solution of inorganic electrolyte salt, preferably a halide or sulfate of an alkali metal, better than sodium chloride or sodium sulfate; and the active substance of the formula (I). The way is usually by the thief electrolyte prepared sample of the active substance of the formula (I). While maintaining the pH hunted the electrolyte solution in the range from 7.5 to 9.0, better from 8.0 to 8.5, to Tatralandia the electrolyte solution at the same time and added in several portions of the active substance of the formula (I) in the form of the free acid, alkali, preferably sodium hydroxide, and water. Water and the active substance in the form of the free acid it is better to add up until a) the content of active substance in synthetic mixture up to the limits of 5-40 wt.%, better 10-30 wt.%, even better 15-25 wt.% and (b) the content of the electrolyte in the synthetic mixture will not be in the range of 0.5 to 2.5 wt.%, better from 1 to 2 wt.%, even better about 1.5 wt.%.

The seed crystals should be in the form of small crystals, the average size not exceeding 10 microns. This allows to greatly reduce the amount of the seed crystals, for example, 0.1-5 wt.% in relation to the total number of active substances. Seed is best done without stirring.

The total number of seed crystals is from 0.1 to 60 wt.%, better from 1 to 50 wt.%, in particular from 1 to 30 wt.% of the total number of the active substance. In all cases in which the new source material to replace only part of the target compounds, the transformation can be really to the invention is in the range from 10 to 95oWith, and preferably in the range from 35 to 55oC.

Dukelaw and dualities salts of 4,4'-decreasingly-2,2'-desulfosarcina can be obtained by neutralizing the form of the free acid 4,4'-decreasingly-2,2'-desulfosarcina respectively, potassium hydroxide or lithium. If deliciious salt other two crystalline forms, hydrates can be obtained by balancing the suspension obtained salt by direct neutralization at elevated temperatures.

The invention also provides an aqueous composition containing 30 to 50 wt.% the active substance in the form of one or more new forms hydrates of the formula (I). This composition remains fluid, has good features and dosing remains stable for months without precipitation even after maturation at temperatures 5-40oWith over an extended period of time.

Aqueous composition containing 30 to 50 wt.% the active substance in the form of one or more new hydrate crystalline forms a, b, C, D, E, F and G of formula (I) has a high viscosity even without the introduction of auxiliary ingredients and suitable for the production of pastes that are applied by brush, or may be included in the composition of such pastes.

Thus, VK and forms can be selectively set the desired viscosity of the aqueous composition without having to enter any auxiliary ingredients. The electrolyte, for example, NaCl or Na2SO4or their mixture can be pre-mixed with the aqueous composition to stabilize the hydrate contained in it.

A special advantage of hydrates in accordance with the present invention, having various crystal forms is that they provide a ready-to-use and stable composition with a large range of viscosity without the addition of environmentally harmful auxiliary ingredients.

However, if desired, obtained according to the invention a composition may include conventional auxiliary ingredients such as dispersing agents, other components, protective colloids, stabilizers, preservatives, perfumes and passivator.

Dispersing agents are preferably anionic dispersing agents, such as condensation products of aromatic sulphonic acids with formaldehyde, such as detailedinformation, naphthalenesulfonate or ligninsulfonate.

Examples of suitable components or protective colloids are modified polysaccharides obtained from cellulose or heteropolysaccharides such as xanthan gum, carboxymethylcellulose, and polyvinyl alcohols, Pelevin is ncentratio 0.01 to 2 wt.%, best of 0.05-0.5 wt.% the total weight of the composition.

Examples of additional ingredients that can be used for stabilization, are ethylene glycol, propylene glycol or the dispersant in amount of 0.2-5 wt.%, best of 0.3-2 wt.% the total weight of the composition.

Compounds that can be used as stabilizers include 1,2-benzisothiazolin-3-one, formaldehyde or chloracetamide in an amount of 0.1-1 wt.%, and preferably 0.1-0.5 wt.% the total weight of the composition.

A concentrated composition, thus obtained, can be used for the fluorescent whitening of paper or textile material, for example, in cleaning products. To this end, for practical use of them is usually diluted to the optimum concentration by the addition of other auxiliary ingredients or water.

The following Examples further illustrate the present invention. Parts and percentages refer to weight unless otherwise stated.

Example 1 In a reactor mix 400 g of ice, 120 g of cyanuric chloride acid and 785 g of methyl ethyl ketone and with intensive stirring and external cooling is treated with a solution of 120 g of disodium salt of 4,4'-diaminostilbene-2,2'-disulfonate in 800 g of water and 164,5 g 17% solution of sodium carbonate in Nata sodium. After adding impose a 55.4 g of aniline and 8.7 g of diethanolamine, at this pH, support 7,5 simultaneously adding to 72.2 g of 36% sodium hydroxide solution. After heating to 60oWith the introduce of 78.8 g of diethanolamine with maintaining a pH of 8.2 while the introduction to 72.2 g of 36% sodium hydroxide solution. The reaction mixture is heated to phlegmasia and methyl ethyl ketone is distilled off, gradually replacing it with 1000 g of water. At a temperature of 95oThe mixture is acidified to pH 4.5 by the addition of 170 g of a 16% solution of chloride-hydrogen acid and adding water volume was adjusted to 2.7 liters After cooling to 70oThe mixture is filtered and pressed the precipitate was washed with 1.8 l of water to obtain the free acid. 30% aqueous suspension of this free acid is heated to 95oC, and pH was adjusted to 9.0 to 9.5 by addition of 36% sodium hydroxide solution. Then the resulting solution is evaporated to dryness, to obtain the compound of formula (I) disodium salt having the crystalline form And containing 1 mol of water and appropriate radiographs is shown in Fig.5.

Example 2 75,0 g form of the free acid (with a content of active substance 40 weight. %) disodium salt of the formula (I) is dispersed 24.7 g of deionized water at 25oC. thus Obtained di is magenesium. Gomogenizirovannogo suspension is neutralized to 32.8 ml of 2N aqueous sodium hydroxide solution. Gomogenizirovannogo neutralized suspension contains crystals with a crystal form In the corresponding radiograph in Fig.1.

After maturation for 2 days at 25oTo receive a suspension, which is well-poured and contains crystals having a crystal form, containing 17 moles of water and corresponds to the radiograph in Fig.2.

Using the same procedure, but using as starting material disodium salt of the formula (I) in the form of pure hydrate crystalline forms a, b, D, E, F and G or their mixture, receive a suspension, which is well-poured and contains crystals of disodium salt of the formula (I) containing 17 moles of water and having a crystalline form With appropriate radiographs in Fig.2.

Example 3 700 g wet pressed sludge of Example 1 (265 g of the free acid) gradually add to 314 g of water at 40-45oWith while maintaining a pH of 8.7 and 9.1 simultaneous addition of 64 g of 36% sodium hydroxide solution. Further, when the 42oWith add 20 g of seed crystals of the hydrate crystalline form obtained in Example 2. After 5 hours idchannel resin (polysaccharide), pre-dispersed in 5.5 g of propylene glycol. Get a liquid suspension, which is well-poured and contains crystals of disodium salt of the formula (I) containing 17 moles of water, and having a crystalline form With appropriate radiographs in Fig.2.

The compound obtained of the formula (A)compared with compound (V) obtained according to example 1 of the patent GB 1293804.

Of the above compounds are prepared 20% aqueous slurry as follows: 44.4 g of each of the above compounds in five equal parts with a ten-minute interval stir in 155,6 g of demineralized water at room temperature. After stirring for 80 minutes the pulp. After storage of the pulp under different conditions was measured viscosity. The test results presented in the table.

The experiment results show that the compound according to the invention provides the receiving water of the pulp that remains liquid and soluble under all conditions of storage, in contrast to the pulp obtained from the compound to the patent GB 1293804, which result from the storage remains insoluble paste.

Example 4 In a reaction flask is heated to 60o400 the e active substance 90 wt.% and containing 10% sodium chloride) and the mixture is heated to 90oC. Add 180 g of 6% aqueous solution of sodium chloride and the mixture is cooled with stirring to 25oC. the Obtained liquid suspension stabilized by the addition of 2.45 g of xanthan resin, which is pre-dispersed 6.1 g of 1,2-propylene glycol and the mixture is heated to 90oWith 2 hours. The mixture is cooled with stirring to 25oWith, as a stabilizer add up 3.22 g of Proxel GXL (1,2-benzisothiazolin-3-one), the mixture is stirred for further 12 hours and finally homogenized using a high speed stirrer. The resulting suspension contains crystals of disodium salt of the formula (I) containing 14 mol of water and having a crystalline form D, which corresponds to the radiograph in Fig.3.

Example 5 In the reaction flask is heated to 40oWith 400 ml of deionized water. In this water portions impose 800 g of the form of the free acid (with a content of active substance 40 wt.%) disodium salt of the formula (I) and simultaneous batch adding 50,45 ml of 37% (50% g/% vol.) an aqueous solution of sodium hydroxide, the pH value of the mixture constant support of 8.2. When you are finished adding all the mixture is diluted with 400 ml of deionized water, stirred for 1 hour, and then homogenized. The resulting suspension contains testvol the radiograph in Fig.4.

Example 6
620 g wet pressed precipitate obtained in Example 1 (279 g of the free acid) was dispersed in 304 g of water and stabilized by the addition of 1.7 g of Proxel GXL and 1.7 g of xanthan gums (polysaccharides), which are pre-spray 3.3 g of propylene glycol. The resulting suspension contains crystals dunagrees salt of the formula (I) containing 7 mol of water and having a crystalline form F, which corresponds to the radiograph in Fig.6.

Example 7
a 20% suspension containing the hydrate crystals having a crystal form E, obtained as in Example 5, is stirred in a closed reactor at 60oWith and maintain at this temperature for at least 20 hours. After cooling to room temperature to obtain a liquid suspension, which contains crystals of disodium salt of the formula (I) containing 7 mol of water and having a crystalline form G, which corresponds to the radiograph in Fig.7.

Example 8
Prepare 400 ml of a 6.0 wt.% an aqueous solution of sodium chloride. Then this solution tatrallyay previously prepared portion of the aqueous suspension of disodium salt of the formula (I). The temperature of hunted solution was adjusted to 45oWith and at the same time to Tatralandia dissolve%) disodium salt of the formula (I), b) an aqueous solution of sodium hydroxide and with water, with constant maintenance of the pH value of the mixture of 8.2. Water and wet water filter pressly residue form of the free acid add up until the content of the active substance form of the free acid in the reaction mixture reaches 15-25 wt.%, while the content of sodium chloride and 1.5 wt.%.

Thus obtained composition are examined using powder diffractometer X'pert (Philips, Almelo) in the geometry of reflection and C-radiation. In the device enter an enclosed chamber with the sample (Anton Parr), which can blow out the gas. The aqueous composition is placed on a holder for the sample (thickness 0.8 mm) and the dimension chart of the sample is carried out in nitrogen to maintain the relative humidity at the level of 80-90%. The results show that such aqueous composition consists of pure hydrates having crystalline form a, b, C, D, E, F or G, or of their mixtures.

Example 9
Similar results are obtained when an aqueous solution of sodium sulfate is used as starting material in Example 8 instead of the aqueous solution of sodium chloride.

Example 10
Prepare 400 ml of a 3.0 wt.% an aqueous solution of sodium chloride. Then this solution tatrallyay prestaged is up>With and at the same time to Tatralandia solution was added and wet water filter pressly residue form of the free acid (active substance 40 wt.%) disodium salt of the formula (I), (b) an aqueous solution of sodium hydroxide and with water, with constant maintenance of the pH of the mixture of 8.2. Water and wet water filter pressly residue form of the free acid add up until the content of the active substance form of the free acid in the reaction mixture reaches 15-25 wt.%, while the content of sodium chloride and 0.75 wt.%.

Thus obtained composition are examined using powder diffractometer X'pert (Philips, Almelo) in the geometry of reflection and Cu-radiation. The results show that such aqueous composition contains crystals of pure hydrate disodium salt of the formula (I) having crystalline form a, b, C, D, E, F or G, or of their mixtures.

Example 11
Similar results are obtained when an aqueous solution of sodium sulfate is used as starting material in Example 10 instead of the aqueous solution of sodium chloride.

Example 12
Prepare 400 ml of a 1.5 wt.% an aqueous solution of sodium chloride. Then this solution tatrallyay previously prepared portion of the aqueous slurry to donationware add and wet water filter pressly residue form of the free acid (active substance 40 wt.%) disodium salt of the formula (I), b) an aqueous solution of sodium hydroxide and with water, with constant maintenance of the pH of the mixture of 8.2. Water and wet water filter pressly residue form of the free acid add up until the content of the active substance form of the free acid in the reaction mixture reaches 15-25 wt.%, while the content of sodium chloride is 0.25 wt.%.

Thus obtained composition are examined using powder diffractometer X'pert (Philips, Almelo) in the geometry of reflection and Cu-radiation. The results show that such aqueous composition contains crystals of pure hydrate having crystalline form a, b, C, D, E, F or G, or of their mixtures.

Example 13
Similar results are obtained when an aqueous solution of sodium sulfate is used as starting material in Example 12 instead of the aqueous solution of sodium chloride.

Example 14
Prepare 400 ml of a 1.5 wt.% an aqueous solution of sodium chloride. Then this solution tatrallyay previously prepared portion of the aqueous suspension of disodium salt of the formula (I). The temperature of hunted solution was adjusted to 45oWith and at the same time to Tatralandia solution was added and wet water filter pressly sediment disodium salt of the formula (I) (contents actionnow mixture of 8.2. Water and wet water filter pressly residue form of the free acid add up until the content of the active substance form of the free acid in the reaction mixture reaches 15-25 wt.%, while the content of sodium chloride is 0.25 wt.%.

Thus obtained composition are examined using powder diffractometer X'pert (Philips, Almelo) in the geometry of reflection and Cu-radiation. The results show that such aqueous composition contains crystals of pure hydrate having crystalline form a, b, C, D, E, F or G, or of their mixtures.

Example 15
Prepare 400 ml of a 1.5 wt.% an aqueous solution of sodium chloride. Then this solution tatrallyay previously prepared portion of the disodium salt of the formula (I). Pre-prepared portion of the disodium salt of the formula (I) prepared in the organic phase, containing the form of the free acid of the active substance and get the last stages of the reaction, which is carried out at 90-100oC. the Temperature of hunted solution was adjusted to 45oWith and at the same time to Tatralandia solution add a) specified organic phase, containing the form of the free acid of the active substance and (b) water. The water and found the organic phase containing the free form directional mixture reaches 15-25 wt.%, while the content of sodium chloride is 0.25 wt.%.

Thus obtained composition are examined using powder diffractometer X'pert (Philips, Almelo) in the geometry of reflection and C-radiation. The results show that such aqueous composition contains crystals of pure hydrate disodium salt of the formula (I) in crystalline form a, b, C, D, E, F or G, or of their mixtures.

Example 16
Similar results are obtained when an aqueous solution of sodium sulfate is used as starting material in Example 15 instead of the aqueous solution of sodium chloride.

Example 17
75,0 g of the free acid 4'4 creatininemia-2,2'-desulfosarcina with hydrate having crystalline form A (active content 40%), dispersed 24.7 g of deionized water, add 0.2 g of polysaccharide (like xanthan resin) and 0.1 g rl GXL and the mixture is homogenized. After maturation for 24 hours at 40oWith or at 60oThe mixture is neutralized to 32.8 ml of 2N potassium hydroxide solution. After maturation at room temperature to obtain a suspension of dallievas salt that pours well, contains crystals of hydrate dallievas salt of the formula (I), with 13 moles of water, and characterized by x-ray, shown in Fig.8.

Example 18
oThe mixture is neutralized to 32.8 ml of a 2N solution of lithium hydroxide. After maturation at room temperature to obtain a suspension deliciious salt that pours well, contains crystals of the hydrate with 29 mol of water and characterized by x-ray, shown in Fig.9.

Example 19
10 g deliciious salt obtained in Example 18, is stirred in a closed reactor at 60oC. After 15 minutes to obtain a clear solution, which, after long agitation begins to precipitate. After stirring for 12 hours at the same temperature, the mixture is cooled and the precipitated solid is filtered off. Get the hydrate deliciious salt containing 14 mol of water, and appropriate radiographs in Fig.10.

Example 20
Repeat Example 19, but with holding balance at a temperature of 55oC. Receive hydrate deliciious salt containing 13 moles of water and having x-rays, is shown in Fig.11.

Example 21
Sulfite pulp suspension beech/pine needles (50:50) is stirred in water (soderzhashchem Examples 1-20 added to a separate sample of the pulp suspension and each test suspension is stirred for 15 minutes. From each test pulp suspension make a sheet of paper with a weight area of 80 g/m2and these leaves are dried. Define whiteness (CIE-Whiteness, measured SCAN-P 66:93) each dried sheet, and it is 140-142. White paper on CIE obtained in the same way, but in the absence of the composition of the fluorescent whitening agents of the present invention is only 75.


Claims

1. The hydrate of the compound 4,4'-decreasingly-2,2'-desulfosarcina with the formula I

in which M and M1independently represent hydrogen or alkaline metal;
x is a number ranging from 1 to 30,
crystalline form which it differs in the radiograph shown in Fig.1-11.

2. A mixture containing two or more hydrates of the compounds 4,4'-decreasingly-2,2'-desulfosarcina formula I, where M, M1x have the meanings specified in paragraph 1.

3. The hydrate of the compound 4,4'-decreasingly-2,2'-desulfosarcina under item 1, in which M and M1both are sodium characterized by x-ray, shown in Fig.1-5.

4. The hydrate of the compound 4,4'-decreasingly-2,2'-desulfosarcina under item 1, in which M and M1represent hydrogen, vinylamine-2,2'-desulfosarcina by p. 1, in which M and M1both are potassium, x is a number from 9 to 17, characterized by x-ray, shown in Fig.8.

6. The hydrate of the compound 4,4'-decreasingly-2,2'-desulfosarcina under item 1, in which M and M1both are lithium, x is a number from 9 to 30, characterized by x-ray, shown in Fig.9-11.

7. The hydrate of the compound 4,4'-decreasingly-2,2'-desulfosarcina under item 3 in the form of crystals having a crystal form In the corresponding radiograph shown in Fig.1.

8. The hydrate of the compound 4,4'-decreasingly-2,2'-desulfosarcina under item 3, in which x represents a number from 14 to 20, in the form of crystals having a crystal form With corresponding radiograph shown in Fig.2.

9. The hydrate of the compound 4,4'-decreasingly-2,2'-desulfosarcina under item 3, in which x represents a number from 10 to 14, in the form of crystals having a crystal form D, corresponding to the radiograph shown in Fig.3.

10. The hydrate of the compound 4,4'-decreasingly-2,2'-desulfosarcina under item 3, in which x represents a number from 16 to 26, in the form of crystals having a crystal form E, the corresponding x-ray, presented at Fiat 1 to 6, in the form of crystals having a crystal form And corresponding to the radiograph shown in Fig.5.

12. The hydrate of the compound 4,4'-decreasingly-2,2'-desulfosarcina under item 4, in which x represents a number from 4 to 10, in the form of crystals having a crystal form F corresponding to the radiograph shown in Fig.6.

13. The hydrate of the compound 4,4'-decreasingly-2,2'-desulfosarcina under item 4, in which x represents a number from 4 to 10, in the form of crystals having a crystal form of G corresponding to the radiograph shown in Fig.7.

14. A method of obtaining a hydrate disodium salt of 4,4'-decreasingly-2,2'-desulfosarcina formula I under item 1, having a crystalline form And, consistent with the reaction of cyanuric chloride acid disodium salt dissolvability 4,4'-diaminostilbene, aniline and diethanolamine, bringing the pH of the mixture to 9.0 to 9.5 with concentrated sodium hydroxide solution and evaporating the mixture to dryness.

15. The method of obtaining a mixture of two or more hydrates of the compounds 4,4'-decreasingly-2,2'-desulfosarcina formula I on p. 2, in which M and M1both are sodium characterized by x-ray, shown in Fig.1-5, including the Pach is tion, including 30-50 wt.% the active substance in the form of a hydrate of the compound 4,4'-decreasingly-2,2'-desulfosarcina formula I under item 1.

17. The water composition, comprising 30-50 wt.% the active substance in the form of a mixture of hydrates of the compounds 4,4'-decreasingly-2,2'-desulfosarcina formula I on p. 2.

18. The way the fluorescent whitening of paper, comprising contacting the paper with the aqueous composition according to p. 16 or 17.

 

Same patents:

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Polymer composition // 2016010
The invention relates to polymeric compositions based on engineering thermoplastics, in particular on the basis of polyacetale intended for the manufacture of products for structural and electroradiotechnics destination

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

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: 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.

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: present invention relates to a method of treating and modifying materials. Described is a method of preparing materials which protects said materials from UV radiation and ozone using a modifier, involving obtaining the modifier by reacting a stilbene derivative in form of 4,4'-bis(s-triazinyl-)diamine-2,2'-disulphostilbene at temperature of up to 55°C in the presence of water with diamine of carbonic acid in amount of 0.5-55 wt % with respect to weight of said stilbene derivative, and material such as foamed or foamable plastic, cement or concrete is then directly treated with the prepared modifier, and/or active radicals of said modifiers are introduced into the surface of said materials. Described also is a method of preparing materials for their protection from UV radiation and ozone using a modifier, involving obtaining the modifier by inoculating a stilbene derivative in form of 4,4'-bis(s-triazinyl-)diamine-2,2'-disulphostilbene with solid diamine of carbonic acid with crystal size less than 40 mcm at 55°C in the absence of water, by grinding the modifiers in a mill and homogenisation at ambient temperature for more than 4 hours, with amount of diamine of carbonic acid of 0.1-45 wt % with respect to the solid stilbene derivative, and material such as foamed or foamable plastic, cement or concrete is then directly treated with the prepared modifier, and/or active radicals of said modifiers are introduced into the surface of said materials.

EFFECT: elimination of negative effect of UV radiation and ozone on surface of materials.

2 cl, 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

FIELD: chemistry.

SUBSTANCE: composition contains at least one fluorescent bleaching agent from bis-triazinylaminostilbene compounds containing taurine groups in a triazine nucleus, having formulae (1), (2) and (3). The composition is used to bleach paper in a wet process, in a gluing press or by coating.

EFFECT: increased whiteness.

25 cl, 2 dwg, 2 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: described is water solution of optic bleach, which contains from 10 to 40 wt % of compound, described by formula (1) [M+]n [(CH3)2NH+CH2CH2OH]2-n, where R is hydrogen or methyl, M+ represents Li, Na or K+, n is smaller or equals 1.5, and from 0.05 to 5 wt % of citric, glycolic, acetic or formic acid, method of claimed solution obtaining and its application for optic bleaching textile, paper, cardboard and non-woven materials and methods of paper bleaching.

EFFECT: water solution of optic bleach is stable in storage and does not require application of additional solubilising additives.

10 cl, 8 ex, 2 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to compositions for optic whitening of paper or cardboard. Composition includes at least two fluorescent whitening agents - derivatives of disulphonic bis-triazinylaminostilbenes, containing group -CO2M in aniline rings in para and/or ortho-position to aminogroup, where M is hydrogen, Li, Na, K, Ca, Mg, ammonium or ammonium, which is mono-, di-, tri- or tetra-substituted C1-C4-alkyl or C2-C4-hydroxyalkyl. Described is method of preparing said composition, its application, method of paper whitening and paper resulting from said process.

EFFECT: claimed composition possesses higher whitening ability in comparison with each of separate whitening agents and provides stable concentrated water compositions without addition of auxiliary solubility-improving substances.

25 cl, 1 dwg, 1 tbl, 4 ex

FIELD: chemistry.

SUBSTANCE: invention relates to disulphonic fluorescent bleaching agents for a coating composition for obtaining a coated paper. Described is the application of the disulphonic fluorescent bleaching agent derivative of bis-triazinylaminostilbenes, containing in aniline rings the group -COOM in a para- and/or ortho-position to an aminogroup, where M is hydrogen, Li, Na, K, Ca, Mg, ammonium or ammonium, which is mono-, di-, tri- or tetrasubstituted with C1-C4-alkyl or C2-C4-hydroxyalkyl, for the clarification of the coating compositions. The coating composition includes a white pigment, a synthetic binding agent, a synthetic cobinding agent, different from the synthetic binding agent, and the said fluorescent bleaching agent. The method of the coating composition clarification, its application for manufacturing the coated paper and the obtained paper are described.

EFFECT: claimed coating composition provides an increased efficiency of paper bleaching.

25 cl, 4 dwg, 4 tbl, 4 ex

FIELD: dangerous emissions protection methods.

SUBSTANCE: invention relates to protection of food products, drinks, pharmaceutical preparations, cosmetics, personal care agents, shampoos, and the like against UV emission. In particular, invention is dealing with storage of contents in clear or slightly colored thin-walled plastic container or film, the two including effective amounts of one or more stable UV absorbers selected from hydroxyphenylbenzotriazole and tris-aryl-simm-triazine compounds.

EFFECT: prolonged storage time and effectively protected packaged products.

28 cl, 1 tbl

FIELD: chemistry.

SUBSTANCE: stabilising composition is described, containing (A) compound of 2,4-bis-(4-phenylphenyl)-6-(2-hydroxyphenyl)-1,3,5-triazine series by formula (I), and (B) one or more compounds chosen from group, which include benzotriazoles by formula (IIa), 2-hydroxybenzophenones by formula (IIb), oxanilides by formula (IIc), 2-hydroxyphenyltriazines by formula (IId), cinnamates by formula (IIe), and benzoates by formula (IIf). There are also described: composition, containing stabiliser composition and organic material; method for organic material stabilisation; and application of stabiliser composition to organic material stabilisation.

EFFECT: increase in efficiency of labile organic materials stabilisation.

17 cl, 19 tbl, 24 ex

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