The method of obtaining titanium tanning agent for leather

 

(57) Abstract:

Usage: for tanning leather. The inventive receive the original solution of titanylsulphate solution with high insoluble residue. It is maintained at a temperature of from 35 to 39oC to obtain a clarified solution with a concentration of titanium 38 - 44,5 g/L. the Upper layer is separated and docrepair the titanyl sulphate to a concentration of the titanium 80 - 140 g/l, the sulfate ion 180 - 340 g/l and chlorine-ion is not more than 65 g/L. Then carry out stirring and cooling. Vymalivayut sulphatoethyl ammonium by introducing into the solid solution of ammonium sulfate in two stages. In the first stage, download the 30 - 40% of the total amount of ammonium sulfate speed is 0.22 - 0.27 kg/s In the second stage, respectively 70 - 60% with a rate of 0.06 to 0.07 kg/s Produce crystallization, filtering the slurry and sludge treatment. table 2.

The invention relates to the production of mineral tanning agent of titanium containing materials, in particular from technicality solutions with high insoluble residue.

Currently in Russia and abroad for tanning leather instead of organic tannins are widely used cheaper mineral tanning agent.

the personal of such raw materials in different ways.

Technical product can be obtained from ilmenite, perovskite, sphene, Laporta and other titanium containing raw material with a mixture of sulfuric acid and ammonium sulfate to obtain SPECA, followed by leaching with water for translation of titanium in the solution from which vymalivayut double sulfate salt of Titania and ammonium ammonium sulfate and sulfuric acid, washed her solution containing 350 g/l of sulfuric acid and 20 g/l of ammonium sulfate, and the solution - preservative containing ammonium sulfate in the amount of 300 to 400 g/L.

The disadvantage of this method is the increased consumption of sulfuric acid and ammonium sulfate for processing of such raw materials and sludge.

A method of obtaining zirconium, titanium and titanzincoated of tannins by evaporation sulfate solutions of zirconium or titanium, or both of these elements in the presence of additives sodium sulphate or ammonium, or both of these compounds, as well as in the presence of additives compounds of chromium or aluminum, or both of these elements at a molar ratio of MeI2IIO3/MeIVO2(where MeIII- aluminium, chromium and MeIV- zirconium, titanium) is not less than 0.25.

The disadvantage of this method is the practical solution author chosen for the prototype is the method of obtaining titanium tanning agent for leather, including the production of the original titanium containing solution by dissolving in water chlorine-containing titanyl sulphate to a concentration of the titanium 80 - 140 g/l, the sulfate ion 180 - 340 g/l, chlorine-ion is not more than 65 g/l, its mixing and cooling, salting out sulphatoethyl ammonium by introducing into the solid solution of ammonium sulfate in two stages:

in the first stage, download the 30 - 40% of the total amount of ammonium sulfate speed is 0.22 - 0.27 kg/s, and the second stage respectively 70 - 60% with a rate of 0.06 to 0.07 kg/s,

subsequent crystallization, filtering the slurry and sludge treatment.

There is a method allows to obtain titanium tanning agent that meets the requirements of THE 95.290-79, soluble in water dry titanyl sulphate on THE 48-0501-344-92 with low content of insoluble residue (less than 0.5 g/l).

The disadvantage of this method is that it is marked by a relatively high consumption of dry titanyl sulphate and allows you to get a quality tanning agent from technicality solutions with high insoluble residue (more than 0.5 g/l), which accumulate in considerable lipata of Titania with high insoluble residue) and rejected products (tanning agent with low basicity, which during long-term storage becomes anhydrous, sulphatoethyl ammonium needle shape with a high content of insoluble residue).

From the above mentioned products get titanylsulphate solutions with a high content of insoluble residue (0.5 to 20 g/l) by dissolving them in water.

The invention is aimed at empowering the known method of producing tanning agent and savings dry titanyl sulphate through the use of technicality solutions with high insoluble residue.

This problem is solved as follows.

In contrast to the known method (prototype) get titanium tanning agent for leather, including the production of the original titanium containing solution of chlorine-containing titanyl sulphate with a concentration on Titan 80 - 140 g/l, the sulfate ion 180 - 340 g/l, chlorine-ion is not more than 65 g/l, its mixing and cooling, salting out sulphatoethyl ammonium by introducing into the solid solution of ammonium sulfate in two stages: the first stage load 30 - 40% of the total amount of ammonium sulfate speed is 0.22 - 0.27 kg/s, and the second stage respectively 70 - 60% with a rate of 0.06 to 0.07 kg/s, the subsequent crystallization, Atego solution with high insoluble residue, which is kept in the temperature range from 36 to 39oC to obtain a clarified solution with a concentration of titanium 38 - 44,5 g/l, the upper layer is separated and docrepair the titanyl sulphate to the desired concentration.

Comparative analysis of the proposed technical solution with the prototype shows that the inventive method differs from the known fact that the initial solution is obtained from titanylsulphate solution with high insoluble residue, which is kept in the temperature range from 35 to 39oC to obtain a clarified solution with a concentration of titanium 38 - 44,5 g/l, the upper drain is separated and docrepair the titanyl sulphate to the desired concentration.

In the analysis of patent and scientific and technical sources not identified technical solutions with the whole set of essential features of the claimed invention, which allows to make a conclusion on the conformity of the proposed technical solution the patentability criteria of "Novelty."

Comparison of proposed method with other technical solutions in this field of technology shows that the use of titanylsulphate solution with high insoluble residue to obtain titanium debit the strengthening of its chlorinated sulfatation low insoluble residue.

In the field of hydrometallurgy known operations: heating, aging, separation of the upper discharge and doreplace clarified part of the solution. However, only the claimed combination and the sequence of all known and unknown essential features and adherence to the above quantitative characteristics allows to achieve a positive effect, which consists in producing quality tanning agent from titanylsulphate solution with high insoluble residue and saving dry titanyl sulphate.

Saving dry titanyl sulphate (TU 48-0501-344-92) by the present method is achieved by replacing part of it in the preparation of the initial solution to obtain a tanning material on technicality solution with high insoluble residue.

Extract the above solution at a temperature of more than 40oC leads to the hydrolysis solution, the precipitation of titanium ions from the solution to precipitate in the form of a water-insoluble hydroxide and a sharp increase in the number of insoluble residue in the titanium tanning agent obtained from such a solution. The exception to the proposed method of obtaining titanium tanning agent operations associated with exposure titanylsulphate solution, will receive the RA can only be obtained titanium tanning agent with a high content of insoluble residue, that does not meet the requirements of THE 95.290-79 on the tanning agent.

The concentration of titanium in the clarified technicaldata solution less than 38 g/l leads to increased consumption of dry titanyl sulphate required to doreplace solution to the desired concentration. Obtaining the concentration of titanium in the clarified technicaldata solution more of 44.5 g/l leads to a sharp decrease in the performance of the process.

For experimental verification of the proposed technical solution was carried out the following activities. The prototype titanium tanning agent was prepared as follows. In 300 ml of water was dissolved chlorinated titanyl sulphate on THE 48-0501-344-92 to concentration, g/l: titanium 112; sulfate ion 260; on chlorine-ion 35.

The solution was stirred until complete dissolution of the titanyl sulphate for at least 1 h the resulting solution of titanyl sulphate is cooled to a temperature of not more than 28oC. To the cooled solution was injected into a dry ammonium sulfate in the amount of 1 kg per 1 kg of titanyl sulphate in two stages:

the first stage was loaded with 35% of the total amount of ammonium sulfate with a speed of 0.25 kg/s;

in the second stage, respectively, 65% with a rate of 0.065 kg/s

After the end of policies carried out in a Buechner funnel on the filter paper under vacuum. The obtained product was dried at room temperature and Packed in polyethylene bags.

By the present method titanium tanning agent obtained from technicality solutions with a high content of insoluble residue of 0.5; 3.5 and 16,23 g/L. Titanylsulphate the solutions were obtained by dissolving in water until saturated one option is rejected high-temperature titanyl sulphate content of soluble residue 0.5 and 16,23 g/l, while another option is rejected sulphatoethyl ammonium content of insoluble residue 0.5 and 3.5 g/l

Data titanylsulphate solutions are kept at different temperatures: 30, 35, 39, 40, 45oC to obtain a clarified solution with different concentration of titanium: 37, 38, 42; 44,5; 45 g/l

Then the upper layer of clarified solution was separated from the sludge by the method of decanting and doreplace its dry titanyl sulphate to obtain the original solution with a concentration on Titan 80 - 140 g/l, the sulfate ion 180 - 340 g/l, chlorine-ion is not more than 65 g/l

The resulting solution was stirred until complete dissolution of the titanyl sulphate for at least 1 h Data titanylsulphate the solutions were cooled with constant stirring to the titanyl sulphate in solution in two stages:

the first stage was loaded with 35% of the total amount of ammonium sulfate with a speed of 0.25 kg/s;

in the second stage, 65% with a rate of 0.065 kg/s

After submitting vicariates in the solution, the suspension was stirred for 15 minutes using a stir bar, filtering the suspension tanning agent was carried out in a Buechner funnel on the filter paper under vacuum. The obtained products were dried at room temperature and Packed in polyethylene bags. For each option was undertaken on three experiences.

During execution of this work determined the content of insoluble residue in the product, which received titanylsulphate solutions, the temperature of the solution, the titanium content in the clarified part of the solution, the chemical analysis okrepshego the titanyl sulphate bleached solution, the flow rate of the dry titanyl sulphate on THE 48-0501-344-92, the grain size of crystals of the tanning agent, and compliance obtained by different variants of the tanning agent to the requirements of TU 95.290-79. The research results are summarized in table. 1 and 2.

The analysis results are given in table. 1 and 2 shows that the inventive method differs from the prototype to the possibility of obtaining high-quality titanium tanning agent from titanically 32.9 - 39,4%.

The optimum parameters for obtaining titanium tanning agent by the present method are the following:

aging in the temperature range 35 - 39oC to obtain a clarified solution of titanium 38 - 44,5 g/l (experiments 4, 8, 9, 11 - 18);

the separation of the upper discharge (experiments 4, 8, 9, 11 - 18);

doreplace the titanyl sulphate to the desired concentration (experiments 4, 8, 9, 11 - 18).

Conducting exposure titanylsulphate solution at a temperature of less than 35oC (experiments 2, 3) leads to a significant decrease in the performance of the process by increasing the time required to achieve a desired concentration of the clarified solution by Titan.

Conducting exposure titanylsulphate solution at a temperature of more than 39oC (experiments 5, 6) leads to the hydrolysis solution and obtaining substandard tanning agent with high insoluble residue.

The decrease in the concentration of titanium in the clarified part of the solution less than 38 g/l (experiments 5 to 7) leads to a significant increase in the consumption of dry titanyl sulphate.

The increase in the concentration of titanium in the clarified part of the solution is more of 44.5 g/l (experiment 10) leads to a sharp decrease in process performance due to the significant increase is 2">

Analysis of the quality of titanium tanning agent obtained by the present method with optimal process parameters, shows that the tanning agent is no different in properties from the tanning agent obtained by the prototype, and meets the requirements of THE 95.290-79.

This method is tested in a production environment "CHMP" with the release of pilot batches of titanium tanning agent with a positive result. An experimental batch of tanning agent sent to consumers.

The method of obtaining titanium tanning agent for leather, including the production of the original titanium containing solution of chlorine-containing titanyl sulphate with a concentration of titanium 80 140 g/l, the sulfate ion 180 340 g/l, chlorine-ion is not more than 65 g/l, its mixing and cooling, salting out sulphatoethyl ammonium by introducing into the solid solution of ammonium sulfate in two stages, the first stage load 30 to 40% of the total amount of ammonium sulfate with the speed 0,22 0,27 kg/s, and the second stage respectively 70 - 60% with the speed of 0.06 to 0.07 kg/s, the subsequent crystallization, filtering the slurry and sludge treatment, characterized in that the initial solution is obtained from titanylsulphate solution with high insoluble residue, which is kept in intervalley separated and docrepair the titanyl sulphate to the desired concentration.

 

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FIELD: coal-chemical products.

SUBSTANCE: weathered vitrinite brown coals from Baga-Nursk coal field having ash level 36-48% and moisture 20% are ground to granule size 0.5-0.9 mm. Resulting powder us sulfurized for 6-8 h with 98% sulfuric acid at 60-80°С and coal-to-acid weight ratio from 1:3 to 2:3. Sulfurized coal is neutralized and treated with 10-15% sodium hydroxide aqueous solution at weight ratio of alkali solution to initial coal (10-15):1 to form water-soluble sodium sulfohumate, after which water-soluble residual coal is separated by centrifugation. Centrifugate is mixed with 10-15% aqueous hydrochloric acid at volume ratio (10-15):6 to form precipitate, which is allowed to settle into compact form during 40-60 min. After decantation of liquid phase, solid residue is partially dried at 40-60°С until pasty mass is obtained.

EFFECT: increased content of tanning substances in humate-containing compounds and enabled utilization of oxidized brown coal in open-cut production of brown coals.

4 tbl, 5 ex

FIELD: coal-chemical products.

SUBSTANCE: weathered vitrinite brown coals from Baga-Nursk coal field having ash level 36-48% and moisture 20% are ground to granule size 0.5-0.9 mm. Resulting powder us sulfurized for 6-8 h with 98% sulfuric acid at 60-80°С and coal-to-acid weight ratio from 1:3 to 2:3. Sulfurized coal is neutralized and treated with 10-15% sodium hydroxide aqueous solution at weight ratio of alkali solution to initial coal (10-15):1 to form water-soluble sodium sulfohumate, after which water-soluble residual coal is separated by centrifugation. Centrifugate is mixed with 10-15% aqueous hydrochloric acid at volume ratio (10-15):6 to form precipitate, which is allowed to settle into compact form during 40-60 min. After decantation of liquid phase, solid residue is partially dried at 40-60°С until pasty mass is obtained.

EFFECT: increased content of tanning substances in humate-containing compounds and enabled utilization of oxidized brown coal in open-cut production of brown coals.

4 tbl, 5 ex

FIELD: tannery industry, in particular method for syntan (synthetic tanning material) production.

SUBSTANCE: claimed method includes diphenolepropane sulgation and condensation with formaldehyde followed by acidifying with sulfuric acid. Formed product is dispersed in lignosulfates containing 0.5-1.5 % of aluminum sulfate as calculated to aluminum oxide.

EFFECT: syntans with stable content of tanned materials: environmentally friendly and economical process.

1 ex

FIELD: tannery industry, in particular method for syntan (synthetic tanning material) production.

SUBSTANCE: claimed method includes diphenolepropane sulgation and condensation with formaldehyde followed by acidifying with sulfuric acid. Formed product is dispersed in lignosulfates containing 0.5-1.5 % of aluminum sulfate as calculated to aluminum oxide.

EFFECT: syntans with stable content of tanned materials: environmentally friendly and economical process.

1 ex

FIELD: tannery industry, in particular method for syntan (synthetic tanning material) production.

SUBSTANCE: claimed method includes diphenolepropane sulgation and condensation with formaldehyde followed by acidifying with sulfuric acid. Formed product is dispersed in lignosulfates containing 0.5-1.5 % of aluminum sulfate as calculated to aluminum oxide.

EFFECT: syntans with stable content of tanned materials: environmentally friendly and economical process.

1 ex

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