The method of obtaining titanium tanning agent for leather

 

(57) Abstract:

The invention relates to the production of mineral tanning material of titanium containing materials, in particular chlorine solution of titanyl sulphate. The invention solves the problem of reducing the volume of wastewater and consumption of ammonium sulfate, reuse, to obtain valuable tanning material components contained in the waste waters. The method of obtaining titanium tanning agent for leather includes preparation of the starting solution of titanyl sulphate, his stirring and cooling, salting out sulphatoethyl ammonium. As vicariates use a mixture of the product of the evaporation of the mother liquor, obtained after filtration of the suspension of titanium tanning agent, and ammonium sulfate in a ratio of not more than 3 : 1. The method also includes subsequent crystallization, filtration of the resulting suspension and sludge treatment. table 2.

The invention relates to the production of mineral tanning material of titanium containing materials, in particular chlorine solution of titanyl sulphate.

Recently in Russia and the CIS for tanning leather instead of organic tannins are widely used cheaper mineral tanning agent.

Cf the titanium containing materials in different ways.

The known method [1] obtain titanium tanning agent for leather by treating such materials 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 300-400 g/l

The disadvantage of this method is the presence of a significant amount of industrial waste waters, increased consumption of ammonium sulfate, the impossibility of re-use to obtain valuable tanning material components contained in the waste waters, which leads to reduction of technical and economic indicators of the process.

The known method [2] obtain 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 compounds, as well as in the presence of additives compounds of chromium or aluminum or both of these elements at a molar ratio of Me2III

The closest technical solution chosen by the authors for the prototype is the way [3] obtain titanium tanning agent for leather comprising preparing a starting solution of titanyl sulphate, his stirring and cooling, salting out sulphatoethyl ammonium sulfate ammonium subsequent crystallization, filtration of the resulting suspension and sludge treatment.

The disadvantages of this method are the availability of a significant amount of wastewater and loss with them valuable components, in particular ammonium sulphate, increased consumption of ammonium sulfate, which leads to reduction of technical and economic indicators of the process.

The invention is aimed at reducing the volume of industrial waste waters and the consumption of ammonium sulfate, for reuse to obtain valuable tanning material components contained in the waste waters.

This problem is solved as follows.

In contrast to the known method (prototype) get titanium tanning agent for leather comprising preparing a starting solution of titanyl sulphate, his stirring and cooling, salting out sulphatoethyl ammonium ammonium sulfate and subsequent crystallization, Phi is a mixture of the product of the evaporation of the mother liquor, formed after filtration of a suspension of titanium tanning agent, and ammonium sulfate in a ratio of not more than 3: 1.

Comparative analysis of the proposed technical solution with the prototype shows that the inventive method differs from the known fact that as vicariates use a mixture of the product of the evaporation of the mother liquor, obtained after filtration of the suspension of titanium tanning agent, and ammonium sulfate in a ratio of not more than 3:1. In the analysis of patent and scientific and technical sources not identified technical solutions with the whole set of essential features claimed in the present application, which allows to draw a conclusion about the novelty of this technical solution, and according to its patentability criteria of "novelty."

Comparison of proposed method with other technical solutions in this field of technology shows that it is known the use of sulfate solutions after evaporation as a raw material for titanium tanning agent [2] however, the use of product evaporation of chlorine-containing mother liquor, obtained after filtration of the suspension of titanium tanning agent, as vicariates in a mixture with ammonium sulfate in a ratio of not bloodvessel the patentability criteria of "inventive step".

The initial solution obtained by dissolution in water of titanyl sulphate with a chlorine content up to 10 wt. The mother liquor after vysalivaniya and filtering suspensions of titanium tanning agent contains (g/l): sulfate ion 200-400; ammonium ion 40-80; chlorine ion to 60; titanium 2-5. Product evaporation of the above mother liquor is a crystalline salt greenish color, consisting of a mixture of ammonium sulfate (NH4)2SO4, ammonium chloride NH4Cl, ammonium sulphate acidic NH4HSO4and small amounts of titanium.

With this product the following, wt. Ion ammonium 23,8-24,9 Sulfate ion 41-68 Chlorine-ion of 23.8-1.8 Titanium 0,056-0,11

Uncontrolled impurities Else.

The use of the above product evaporation as vicariates upon receipt of titanium tanning agent for leather allows you to:

reduce the amount of industrial waste waters due to the receipt of vicariates by evaporation mother solutions after filtration of a suspension of titanium tanning agent;

to return to the process of obtaining titanium tanning agent valuable components, such as sulfate ion, ammonium ions and titanium contained in waste waters, and reuse them as vicariates;of the mother liquor, formed after filtration of a suspension of titanium tanning agent.

For experimental verification of the proposed method has undertaken the following activities.

The prototype titanium tanning agent was obtained by preparing a 300 ml solution of titanyl sulphate with a concentration of 500 g/l and stirring for 15 min (the time of crystallization) with the help of a mixer. Filtering suspensions of titanium tanning agent was carried out in a Buechner funnel on the filter paper under vacuum. The obtained product was dried at room temperature.

By the present method titanium tanning agent received from titanyl sulphate by dissolving it in 300 ml of water to a concentration of 500 g/l and stirred to dissolve for at least 1 h the resulting solution of titanyl sulphate was cooled with constant stirring to a temperature of not more than 28aboutC. the cooled solution was injected as vicariates mixture of the product of the evaporation of the mother liquor, obtained after filtration of the suspension of titanium tanning agent in the amount of 1 kg per 1 kg of titanyl sulphate. The ratio of product evaporation and ammonium sulfate in a mixture of different: 0,33: 1; 1: 1; 3:1; 4:1. After submitting vicariates in the solution of susp in a Buechner funnel on the filter paper under vacuum. The obtained product was dried at room temperature.

In the process of doing this work evaluated the consumption of ammonium sulfate and the volume of the mother liquor, which is intended to discharge, upon receipt of titanium tanning agent of the prototype and the claimed method. Also evaluated the quality obtained by different variants of the tanning material for compliance with requirements of THE 95.290-79. The results are shown in table.1 and 2.

The analysis of the research results presented in table.1 and 2 shows that the inventive method of obtaining titanium tanning agent differs from the prototype smaller volume of wastewater (0,022-0,59 l/kg of tanning agent instead of 1.12 l/kg of tanning agent on the prototype), lesser consumption of ammonium sulfate (has 0.168-0,503 kg/kg of tanning agent instead of 0.67 kg/kg of tanning agent on the prototype) in all the stated range of the ratio of the product of evaporation and ammonium sulfate in a mixture of vicariates. In addition, the claimed method allows re-use in the process of obtaining valuable tanning material components contained in waste waters. Optimal ratio of product evaporation and ammonium sulfate in a mixture of vicariates is the ratio of no greater than 3:1 (experiments 3-5). The increase of this ratio (6) leads to decrease in the art of vicariates and accumulation in the tanning agent insoluble compounds in excess of the norm.

Analysis of the quality properties of titanium tanning agent obtained by the present method with the optimal ratio of product evaporation and ammonium sulfate in a mixture of vicariates 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 with the release of an experimental batch of titanium tanning agent with a positive result.

The METHOD of OBTAINING TITANIUM tanning agent FOR LEATHER comprising preparing a starting solution of titanyl sulphate with stirring, cooling, salting out sulphatoethyl ammonium sulfate ammonium subsequent crystallization, filtration of the resulting suspension and drying the precipitate, wherein the ammonium sulfate is used in a mixture with the product evaporation of the mother liquor, obtained after filtration of the suspension of titanium tanning agent, at a ratio respectively not more than 1 : 3.

 

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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

FIELD: light industry.

SUBSTANCE: invention relates to a method for treatment of fur hides before oxidative whitening of hair cover. Additional tanning and pickling are carried out separately at pH value 6.5-7.0. The preparation based on low-molecular alcohol polyacetals - "Dubitel M" is used as a tanning agent. Tanning agent is added for two steps wherein at the second step tanning agent is added in twice dose as compared at the first step. Additional tanning is carried out in the required ratio of components of an aqueous composition comprising sodium chloride, surface-active substance, preparation based on low-molecular alcohol polyacetals. Pickling is carried out with smearing on hair cover in the consumption 2-4 ml per 1 dm2 with the composition comprising iron sulfate, citric acid, surface-active substance and gelatin as a protecting additive. After pickling lying is carried out for 12-16 h. Method provides improved the quality of whitened fur hides.

EFFECT: improved method for treatment.

2 cl, 2 tbl

FIELD: light industry.

SUBSTANCE: invention relates to a method for treatment of fur hides before oxidative whitening of hair cover. Additional tanning and pickling are carried out separately at pH value 6.5-7.0. The preparation based on low-molecular alcohol polyacetals - "Dubitel M" is used as a tanning agent. Tanning agent is added for two steps wherein at the second step tanning agent is added in twice dose as compared at the first step. Additional tanning is carried out in the required ratio of components of an aqueous composition comprising sodium chloride, surface-active substance, preparation based on low-molecular alcohol polyacetals. Pickling is carried out with smearing on hair cover in the consumption 2-4 ml per 1 dm2 with the composition comprising iron sulfate, citric acid, surface-active substance and gelatin as a protecting additive. After pickling lying is carried out for 12-16 h. Method provides improved the quality of whitened fur hides.

EFFECT: improved method for treatment.

2 cl, 2 tbl

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