Method of preparing black coloring composition compatible with oiling agent

FIELD: leather industry.

SUBSTANCE: preparation of composition is conducted on vertical-type bead mill. Induline, kerosene, and diesel fuel are consecutively charged into mill before stirring mechanism is energized, after which apparatus and contents thereof are slowly heated. Stirring is then stopped for 1 h while slow heating of mill contents is continued. When specified time expires, carboxylic acid or acid mixture, white spirit, fat additive, and aluminum oxide or hydroxide are added. Mechanic stirring is then switched on and contents of the bead mill are ground and the process is carried out at spontaneously fixed temperature caused by heat effects of the processes and natural cooling. When temperature is lowered to 85-120°C, desired product is discharged.

EFFECT: simplified process and increased product discharge degree.

1 tbl, 19 ex

 

The invention relates to the technology of black ink compositions on the basis of soot and indoline used in the production of colored oiling compositions, and can be used in the leather industry.

There is a method of making a composition for the fatliquoring of leather, which in their by liquid-phase air oxidation of a mixture of natural and synthetic fats with butter UNDER oxidat enter in the quantity of 3-3 .5% by weight of oxalate components of the ink composition ratio, wt.%: black pigment 35, organic acid 40 and kerosene 25. The resulting mass is thoroughly mixed, after which it enter in contact with an aqueous solution of sodium sulfite under intensive mechanical stirring (U.S. Pat. Of the Russian Federation No. 2099430). At the same time as the black pigment used indulin, nigrosine, carbon black, or mixtures thereof, and the acid is any saturated or unsaturated carboxylic acid, C8-C20or a mixture of these acids.

The downside of it is component input components of the ink composition and the actual formation of the latter in oxidate that does not provide stable results when using fattening.

Closest to the claimed is a method of obtaining compatible with the oiling composition of the black ink composition (EN 2002135258, CL 14 With 9/02, published 20.07.2004), where kr is generating composition composition, wt.%: black pigment 35, organic acid 25, solvent 35 and fat Supplement 5 receive as an independent intermediate. The process is carried out in a bead mill, vertical type in the following sequence of operations and combinations of operations:

download solid soot and indolinone dye, kerosene and diesel fuel and mixing of the mass within 0.25 to 1 hour;

- cessation of mixing for 0.5-2 hours, sucks the obtained mass and its heat through his shirt up to 50-60°by the end of the period of lay-up;

- download in a heated mass of melt acid, white spirit, fatty additives and process under stirring at arbitrarily fixed temperatures up to 115-120°C for 0.5 to 3 hours;

- continuation of the process without stopping stirring while controlling the temperature cooled by flowing water through the shirt for 1-2 .5 hours with the passage of the maximum temperature in the range of 140-155°C;

- forced cooling with continuous stirring to 130-135°0.75-1.5 hours;

the termination of forced cooling with continued stirring for another 0.5 to 1.5 hours until a temperature 115-120°C;

stop mixing and discharging the obtained composition first by gravity and then using a vacuum.

The disadvantage of this method is that 3-4,4 wt. composition is not unloaded from the bead mill, due to the high adhesion of the resulting composition to the surface of the beads and shell bead mill. In addition, the high viscosity of the composition determines its low fluidity, which makes it difficult to unload composition requires to start this operation, the temperature of 115-120°and the use of vacuum for holding and completion of this transaction.

The technical result of the proposed method is to increase the degree of emptying of the bead mill, as well as to facilitate the unloading of the black ink composition, in particular in reducing the temperature of the beginning of the discharge and renunciation of the use of vacuum in this operation.

This technical result is achieved in that in the method of obtaining compatible with the oiling composition of the black ink composition by typing in the contact of solid soot and indolinone dye first with kerosene and diesel fuel under stirring and sludge weak when heated to 50-60°and then with a carboxylic acid or mixture of acids, mineral spirits and adipose addition, mass transfer and chemical reactions between the loaded components under stirring, passing the maximum temperature using forced cooling and unloading of the product according to the invention in the composition is administered oxide or aluminum hydroxide sludge is a mixture of in any proportion in the amount of 0.5 to 1.6% by weight carboxylic acid or mixture of acids, when this input aluminum compounds carried out simultaneously with the introduction of carboxylic acid or mixture of acids, white spirit and fat supplements, and unloading of product are by gravity when the temperature of the discharge 85-120°C.

Characteristics of the raw materials used

Aluminium oxide AL2About3according to GOST 8136-85 "active aluminium Oxide".

Aluminum hydroxide Al(OH)3according to GOST 11841-76 "Aluminum hydroxide".

Indulin fat-soluble GOST 4770-77.

Nigrosine according to GOST 4014-75.

Carbon black according to THE 38-11551-77 E "technical Carbon (soot) PM-15 RVDM".

Synthetic fatty acids according to GOST 23239-89 "fatty Acid synthetic fractions of C5-C6With7-C9With5-C9With10-C16With17-C20".

Oleic acid according to GOST 7580-55.

Stearic acid according to GOST 6484-65.

Acid hydrolyzed at 95% sunflower oil (GOST 1129-81) and animal fat (GOST 1045-73 "technical animal Fat") in the presence of p-toluenesulfonic acid as catalyst at a temperature of 100±3°and close to stoichiometric quantities of water (U.S. Pat. Of the Russian Federation No. 2166534).

Waste ski beyond 38 1071231-89 "bottoms products production ski".

Fuel diesel type L-02-40 according to GOST 305-82.

Oil UNDER THE 113-03-476-82 "Oil (a mixture of high-boiling oxidation products of cyclohexane, the dehydrogenation College is canola, polycondensation of cyclohexanone)".

Kerosene according to GOST 28577.2-90, ISO 8217-87.

White spirit according to GOST 3134-78.

Getting compatible with oiling composition of the black ink composition of the inventive method consists in the following. Solid pigment and the bulk solvent is introduced into the contact bead mill, and then leave for some time without stirring. During this period the mass is heated to 50-60°With injected organic acid, a fat component, a hydroxide or aluminum oxide and the remainder solvent. Include mixing and pereir and lead the process from the beginning and at the end in the absence and in the period of most intense heat and cooling to the almost complete cessation of heat. The temperature passes through a maximum and falls to 85-120°at which, and begin to unload composition by gravity.

The obtained ink composition is metered and dissolved in oxidate from a mixture of natural and synthetic fats and oils UNDER before treatment with an aqueous solution of sodium sulfite.

Example 1

In a bead mill with a capacity of 5 l equipped with a bladed mechanical stirrer, reflux-condenser outlet to the atmosphere, the shirt along the entire height of the hull, capable of heating steam or hot water and cooling the flowing cold water, a drain pipe with a metal mesh to separate the beads from the discharge of the product and contains 2400 g of glass beads with a diameter of 1.5-2.3 mm, contribute consistently 563 g of carbon black, 312 g of indoline, 650 g of kerosene and 100 g of diesel fuel as a solvent. Include mechanical stirring for 20 minutes At the end of this period served the hot water in the jacket and begin the slow heating of the device and its contents. Continuing the slow heating off stirring for 1 hour. After a specified time through the loading hatch of the injected melt waste of FLC in the amount of 625 g at a temperature of 60°C. Simultaneously dispense 125 g of sulphonated fish oil, 125 g of white spirit and 6.25 g of aluminum oxide Al2About3.

Include mechanical mixing and pereir content bead mill and lead the process in spontaneously fixed temperature to 118°C for 45 minutes while Continuing the stirring, serves flowing water in the cooling jacket and observe the change of the temperature of the reaction mixture. Within 1 hour she grew up and reached the maximum value 151°C. Further, the temperature during stationary running cooling began to decrease and after 2.5 hours was 131°C. At this point, stop the water flow in the cooling jacket and continue stirring for another 1 hour. Te is the temperature dropped to 115° C. Stop stirring, connect the tank for receiving the products, open the valve on the drain pipe and lead the product discharge by gravity within 3,7 minutes eventually received 2482 g of the composition.

Examples 2-13

Raw black ink composition, the sequence of operations and reactor similar to that described in example 1. Differ in the nature and amount of additive aluminium-containing reagent, the temperature of the discharge product, and also the moment you enter the additive oxide or aluminum hydroxide. The results obtained are summarized in table.

Examples 14-19

The reactor, the mass of the load and the sequence of operations similar to that described in example 1. The addition of aluminum oxide to 0.7 wt.% from boot used acid and is introduced together with the acid. Is nature used indolinone dye and acid. The results are shown in the table.

DescriptionExample No.
2345678910111213
Add: reagentAl2O3Al2O3Al2O3Al(OH)3/sub> Al(OH)3Al(OH)3Al2O3+Al(OH)31:3Al2O3+Al(OH)33:1Al(OH)3Al(OH)3Al(OH)3Al(OH)3
number, wt.% on the number of injected acid0,50,71,20,60,91,61,30,81,21,21,21,2
the moment you enteracidacidacidacidacidacidacidacidacidwith sootBUTTO
The temperature of the discharge products-that °114110911081128510511192120120118
The duration of discharge, minof 5.4the 4.75,35,5a 4.95,84,64,4a 4.9204090
The number is the creation of unloaded product % by weight of loaded raw materials999999999999999999778368
Legend: BUT at the beginning of forced cooling;

KO at the end of the forced cooling

DescriptionExample No.
141516171819
Indolinone dyeNH+And (1:2)AndH+And (1:1)H+And (2:1)H+And (4:1)
Used additiveOlStWith10C17GPMGSG
The temperature of the discharge product, °919588939792
The duration of discharge by gravity, min4,56,0the 5.7a 4.95,36,0
The number of unloaded product, % by weight of loaded raw materials9999 99999999
Designation: - indolin, N - nigrosine, (...) the ratio of the mass; acid: Ol - oleic, St - stearic,10- faction With10-16SJK,17- faction With17-20FLC, GPM - hydrolysis of sunflower oil, GSG - hydrolysis of pork fat.

The positive effect of the proposed solutions is that

- improved unloading of the finished product and increases the fullness of the discharge from the reactor up to 99% and even a few more; discharge flows by gravity, for 6 min or less and does not require the use of coercive means a type of vacuum that simplifies the equipment of this operation; expands due to the lower bound and the range of temperatures at the beginning of unloading;

- input additive of aluminum oxide does not impair the individual properties of the composition, but improves their complex: fattening processed with such a composition leather get some water repellency.

Way to obtain is compatible with oiling composition of the black ink composition by typing in the contact of solid soot and indolinone dye first with kerosene and diesel fuel under stirring and sludge weak when heated to 50-60°and then with a carboxylic acid or mixture of acids, mineral spirits and fatty additives is th, mass transfer and chemical reactions between the loaded components under stirring, passing the maximum temperature using forced cooling and unloading of the product, characterized in that the composition is administered oxide or aluminum hydroxide or a mixture in any proportion in the amount of 0.5 to 1.6% by weight carboxylic acid or mixture of acids, and the input connections of aluminum carried out simultaneously with the introduction of carboxylic acid or mixture of acids, white spirit and fat supplements, and unloading of product are by gravity when the temperature of the discharge 85-120°C.



 

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FIELD: tanning industry.

SUBSTANCE: process is conducted in vertical mill to which soot, induline, kerosene and diesel fuel are introduced. Then components are mixed and slow heating the apparatus and its content is started after which mixing is switched off and slow heating of mill content is continued. Upon expiration of said time, acids or their compositions, white spirit and fatty additive are introduced and chemical mass-exchange process is performed at spontaneously fixed temperature due to thermal effects of this process and natural cooling at the beginning and at the end, as well as due to forced cooling at intermediate stage characterized by high rates of temperature at maximum of 140-150°C. At the moment when forced cooling is discontinued, 0.5-1.5 h before discontinuation of mixing and beginning of withdrawal at temperature of 80-115°C, 43-52-% solution of aluminum salts and C10-C20 of carboxylic acids is introduced into product being prepared.

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1 tbl, 15 ex

FIELD: leather industry.

SUBSTANCE: invention relates to area of dyeboarding operations in leather production, in particular to a method of dyeing genuine leather with active dyes including intermediate product neutralization, active dye dyeing and subsequent fixation with alkaline reagent. According to invention, neutralization is effected in presence of preparation "Deep Dying" in amount 4.5-5.0% of the weight of planned leathers, dyeing is effected with active dye consumed in amount 2.5-5% at medium pH 3.4-3.5 in presence of 0.9-1.2 g/L alizarin oil, and fixation of dye is performed simultaneously with greasing at medium pH 8.5-8.9 with sodium hydrocarbonate consumed in amount 1.3-1.8%, greasing composition in amount 3.8-4.2%, and "Polinap AD" in amount 1.8-2.2 of the weight of planned leathers. Finally leather is rinsed in presence of nonionic surfactant consumed in amount 0.8-1.2 g/L.

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1 tbl, 9 ex

FIELD: physical method for leather staining.

SUBSTANCE: claimed simplified method includes spraying of dyeing composition, containing (mass %): diphenylamine 0.3-2.0; tetrabromomethan 5.0-10.0; α-naphthol 0.01-0.03; and balance: methyl methacrylate-based varnish, onto the leather face, followed by ultraviolet exposure with wave-length of 300-400 nm at 25-300C for 0.5-1.0 min. Ferrocene and/or indole may be added in dyeing composition to complete color variety.

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2 cl, 2 tbl, 3 ex

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1 tbl, 15 ex

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5 cl, 1 tbl, 16 ex

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