Method of production of black dyeing composition for oiling compounds

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.

EFFECT: facilitated procedure; increased amount of product.

1 tbl, 15 ex

 

The invention relates to the production technology is compatible with oiling composition of the black ink composition with soot and indolines as a combined dye and can be used in the leather industry.

There is a method of making a composition for the fatliquoring of leather (U.S. Pat. Of the Russian Federation No. 2099430), which prepared oxidate mixture of natural and synthetic fats and oils UNDER enter the components of the black ink composition in the relevant mass ratio and the total number 3-3,5% by weight of oxidate, mix until smooth, and then treated with an aqueous solution of sodium sulfite. In this case, the ink composition is formed in the presence of oxalate that negatively affects quality indicators pigmented fatliquoring agents and their stability during the transition from one batch of product to another.

Closest to the claimed method is the individual receiving compatible with greasing the black ink composition (EN 2002135258, CL 14 C 9/02, publ. 20.09.2004) according to which in a bead mill, vertical type a specific design first introduced in the contact of the estimated quantity of solid soot and indolinone dye kerosene and diesel fuel under stirring and further in a state of sludge and heating to 50-60°S, then PR is lead loading acid or composition of the acids, white spirit and fatty additives and then conduct chemical and mass transfer processes at arbitrarily fixed temperature due to thermal effects of developing these processes at the beginning and at the end when natural cooling, and in the period of most rapid growth and passing through a maximum in the forced cooling operation with the output end at 115-120°With, then stop stirring and carry out the unloading of the obtained composition, first by gravity and then using a vacuum.

The disadvantage of this method is certain difficulties in discharging the resulting black ink composition, consisting in the use of relatively high temperatures (115-120° (C) and vacuum in the final stages, quite a long time this operation (>20 min)and high (3.0 to 4.4 wt.%) the residual quantity of the product in the mill.

The objective of this solution is to eliminate the need for a vacuum unloading of the obtained black ink composition, reducing the dependence of the unloading temperature, and the increase of the degree of discharge of the obtained product.

This object is achieved in that in the method of obtaining the black ink composition for oiling compositions by entering into contact with the bead mill, vertical t the PA solid soot and indolinone dye kerosene and diesel fuel as part of a combined solvent under stirring and further in a state of sludge and heating to 50-60° With the subsequent uploading of acid or acid composition, white spirit and fatty additives and chemical and mass transfer processes in spontaneously fixed temperature due to thermal effects of these processes and natural cooling at the beginning and at the end, and forced cooling at an intermediate stage characterized by the highest rates of temperature increase with the passage of the maximum at 140-150°Since, according to the invention in the composition of the obtained product is injected 3-9% by weight of the component download songs 43-52%-aqueous solution of salts of aluminum and10-C20carboxylic acids, with this entry perform at the moment of cessation of forced cooling in the final stages of preparation of the ink composition for 0.5-1.5 hours before the termination of the mixing and began unloading at a temperature of 80-115°C.

Characteristics of the raw materials used.

Indulin fat-soluble GOST 4770-77.

Nigrosine water soluble 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 With5-C6With7-C9C5-C9C10-C16With17-C20".

Oleic acid according to GOST 7580-55.

Stearic acid according to GOST 6484-65.

Collateralizing 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 amounts of water (U.S. Pat. Of the Russian Federation No. 2166534).

Waste of FLC on THE 38 1071231-89 "bottoms products production FLC".

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

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

White spirit according to GOST 3134-78.

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

43-52%solutions of aluminum salts and10-C20carboxylic acids in the mixture of diesel fuel, kerosene and white spirit received in accordance with U.S. Pat. Of the Russian Federation No. 2092533 by direct tribochemical interaction of oxide or aluminum hydroxide with carboxylic acids or their compositions, including waste FLC, in a bead mill at 20-60°in the presence of 1-2 wt.% water and 0.05-0.4 wt.% tribochemical catalyst within 10-40 minutes

Getting compatible with oiling composition of the black ink composition of the inventive method consists in the following. Solid pigments 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°, then enter the organic acid, the fatty component and the remainder of the solvent include mixing and pereir and lead PR is the first process and at the end of the absence, and during the most intensivnogo heat with forced cooling to the almost complete cessation of heat. The temperature passes through a maximum and decreases. At the moment of disconnection forced cooling additive injected aluminium salts and10-C20carbon(Oh) acid(s) in an amount of 3 to 9% by weight of the component download songs and continue stirring for 0.5 to 1.5 hours. Stop stirring and carry out the unloading of the finished composition at a temperature of 80-115°With gravity in a specially designed for these purposes, the capacity (storage to use).

The composition is metered and dissolved in oxidate from a mixture of natural and synthetic fats and oils, followed by processing the resulting solution with an aqueous solution of sodium sulfite. The presence of aluminum salts in these quantities does not affect the performance of the treatment and does not reduce the quality of fattening on any indicator in relation obtained by RF patent for application No. 2002135258(037191).

Example 1.

In a ball mill with capacity type autoclave of 5 l equipped with a blade mechanical stirrer, a free exit to the atmosphere through a reflux condenser, jacket over the entire height of the side surface of the housing, capable of work shall be for heating steam or hot water and cooling water and a drain pipe with a metal mesh to separate the beads during the unloading of the finished product and containing 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. 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. Turn off the stirring for 1 hour, continuing the slow heating of the contents of bead mill. After a specified time through the loading hatch of the injected melt waste products of FFA in the amount of 625 g at a temperature of 60°C. the Temperature of the reaction mixture at this point was 58°C. Simultaneously dispense 125 g of sulphonated fish oil and 125 g of white spirit. Upon completion of loading include mixing and are pereir content bead mill with spontaneously fixed temperature for 45 minutes, the Temperature at the end of this time was 121°C. 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 continued to grow and reached a maximum value 149°C. Further, the temperature during stationary running cooling began to decrease and after 1.5 hours was 132°C. At this point, the stun is up water in the cooling jacket and give 75 g of a 52%aqueous solution of aluminum salts and acid hydrolysis of sunflower oil in a mixture 1:1 by volume of kerosene and diesel fuel. Continue stirring for another 1 hour. After this time the temperature had dropped to 115°C. Stop stirring, connect capacitance for receiving products and lead the product discharge by gravity within 6 minutes eventually received 2552 g of the composition.

After cooling to room temperature, unloaded weight becomes weakly homogeneous fluid close to a pasty condition with a glossy black surface and good luster. In this state, it is well kept, easily dosed and dissolved in oxidated intended for processing aqueous solution of sodium sulfite.

Examples 2-15

The reactor, download the basic components of the composition and additives, as well as the sequence of operations similar to that described in example 1. Different nature of the anion and the number of input composition of salts of aluminum, the temperature of the discharge product, the duration of this operation and the number of unloaded product. The results obtained are summarized in table.

Table
DescriptionExample No.
234567891011 12131415
The addition of a solution of salts of aluminum, wt.% from the component download ink composition3,374,175,115,986,546,63of 6.717,147,818,129,009,002,171,37
The content of aluminum salts added in the solution, wt.%5252504851474547514547435249
The nature of the anion salts of aluminum143875+36591+25+1266
The duration of mixing after entering aluminum salts hour1,501,371,411,030,840,750,750,850,900,640,530,501,501,50
The temperature of the discharge product by gravity, � 108111114971081041079881889380115120
The duration of the discharge product, min5,04,84,34,0a 3.95,04,4the 4.75,2the 4.73,43,72744
The number of paged by gravity ink composition (product), g or wt.%
25652578260126252634264426412657267826822703269524412115
99999999999999999999999995,683,5
Legend: acids and their composition: 1 - oleic acid; 2 - stearin; 3 - C17-C20the fraction of FFA; 4 - C10-C16the fraction of FFA; 5 - waste FFA; 6 - acid hydrolyzed sunflower oil; 7-9 - acid hydrolyzed animal fat (pork, mix pork and fish in the ratio of 3:1 and 1:1 respectively).

The positive effect of the proposed solutions is that:

1. Much easier discharging ink compositions of the bead mill, reducing the time of this operation, the operation itself takes place by gravity, does not require the use of vacuum, temperature decreases upload up to 80°C. All this is a direct consequence of increasing the fluidity of the ink composition as a result of entering into it aluminum salts.

2. Aluminium salts help to reduce adhesion of the composition to glass (glass beads) and the metal casing bead mill. As a result, the flow of product from the reactor when the discharge increases, and consistent with several parties accumulation of residual quantities of nespivshegosya from the reactor product does not occur.

3. Enter aluminum salts in the composition increases its mass and does not impair its main qualitative features as intermediate for oiling status is Bob either individually, neither the complex as a whole. On the contrary, the latter, in particular, is improved by reducing the negative impacts of water treatment processes sodium sulfite and using feeding. And the surface treated in this oiling skin acquires a certain water-repellent properties.

4. The required solutions of aluminum salts can be obtained in the same bead mill, where the production of the black ink composition. Therefore, no need to search their manufacturer and address associated with the purchase, delivery and storage issues.

The way to get the black ink composition for oiling compositions by entering into contact with the bead mill, vertical type solid soot and indolinone dye kerosene and diesel fuel as part of a combined solvent under stirring and further in a state of sludge and heating to 50-60°With subsequent uploading of acid or acid composition, white spirit and fatty additives and chemical and mass transfer processes in spontaneously fixed temperature due to thermal effects of these processes and natural cooling at the beginning and at the end, and forced cooling at an intermediate stage characterized by the highest growth rates of temperature with the passage of the maximum at 140-150° , Characterized in that the composition of the obtained product is injected 3-9% by weight of the component download songs 43-52%-aqueous solution of salts of aluminum and10-C20carboxylic acids, with this entry perform at the moment of cessation of forced cooling in the final stages of preparation of the ink composition for 0.5-1.5 h before the termination of the mixing and began unloading at a temperature of 80-115°C.



 

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