CS271759B1 - Method of combined tanning agent production - Google Patents

Abstract

The invention solves production problems of auxiliary tanning agents. The possibility of its use, is in plants producing mineral chemical agents, in tanneries and the basic fur industry.Correction of properties of basic naphthalene sulphoacid condensate by aluminium salts with stabilising agents. The method of production of the auxiliary tanning agent from naphthalene mono-, di-, trisulphonic acids or their mixtures is prepared by their condensation with formaldehyde in an acid medium. The method is characteristic by the fact that the condensates are thermally treated for 30 to 120 minutes at a temperature of 50 to 110 degrees C with aluminium salts of the formula AlOHn(SO4)(3-n)/2 or Al(OH)nCl3-n, where n = 0 to 3, or with salts of MA1(SO4)2.x H2O type, where M is Na<+> or K<+> or NH4<+>, in such an amount that the product dry matter contains 3 to 15 % by weight of Al2O3 and stabilizing agents of the formula <IMAGE> are added, where N = 2 t o6, R1, R2 = -H or -CHO or -CO-CH2OH, where m = 1 to 6 in the amount of 0,2 moles per 1 mol of aluminium and anorganic acids or alkalis in such an amount that the theoretical base of the aluminium salts contained in the product can be 75 degrees Schorlemmer.

Description

The present invention relates to a process for the manufacture of a tanner's adjuvant having a combined effect of synthetic tanning agent and aluminum salts.

The tanning aids used to accelerate the tanning of leather used to date use, in addition to the basic raw material, which is naphthalene condensate of mono-, di- and trisulfonic acids, decalcified sulphite leaches, in a maximum amount of 25% by weight of mono-, di- and trisulphonic or sulphite extracts modified by heating to 80 to 130 ° C and oxidizing the decalcified or non-decalcified sulphite liquor in an amount of 35 to 400% by weight of the modified sulphite liquor dry matter to the naphthalenesulphonic acid dry matter. At the same time, a maximum of 30% by weight of tanning agent produced by the condensation of phenols, sulfonated phenols and betanaphthol sulfonate may be added. All of these additions in the indicated amounts modify the properties of the naphthalene sulfoacid base condensate. In the current shortage of raw materials produced from naphthalene, the production of these tanneries is limited. Furthermore, the addition of weak organic acids such as formic, acetic, propionic, oxalic and many others is used to improve the properties of the compositions. These acids are also scarce and expensive.

Some of the disadvantages of the production methods used hitherto are eliminated by the production method according to the invention, which consists in the fact that the condensates of mono-, di- and trisulfonic acids or their mixtures and formaldehyde are heat treated in an acidic environment for 30 to 120 minutes at 50 to 110 C with the addition of the aluminum salt a conceptual formula Al (OH) -j (S0 ^) (3-n) / 2 ° ^{neb0 A} K ^H) N ^C1 (3-n) ^{'where n = 1 to 5 with salts neb0} type MA1 ( SO4) ₂ . xH ₂ O, where M can be Na ⁺ , K ⁺ or NH 4.

The addition of aluminum salts is such that the dry matter of the product contains 3 to 15% by weight of Al ₂ O 3. Next, a stabilizing agent of the formula is added

6, R 1, R ₂ = -H or -CHO or -CO-CH 3 OH or ^c m ^H 2m + 1 or ^{0 ° C} m ^H 2m-1 ° ^net5 ° ^C m ^H 2m-1 ' ^where m = 1 to 6, in an amount of 0.2 to 3 moles per 1 mol of aluminum. Further basification is performed by addition of inorganic acid or alkali in an amount such that the theoretical basicity of aluminum salts contained in the product was 75 ⁰ Schorlemmer.

The product prepared in this way can be applied in a liquid state or it can be dried, for example, in a spray dryer. The dried product may be admixed with gradual weighing agents in an amount of up to 10% by weight per dry product. Alternatively, the substance may be dried prior to basification and the resulting powder may be mixed with solids gradually acidifying in an amount of up to 10% by weight on the dry matter of the product.

The process according to the invention is illustrated by the following examples, which are given several of the many possible applications.

R _2, wherein n = 2 to

CH

AND

OH

Example 1

In a reaction vessel equipped with a stirrer, reflux condenser and heating and cooling, add 416 parts by weight of naphthalene mono-, di- and trisulfonic acid condensate or a mixture thereof with 50% by weight of formaldehyde, add 453 parts by weight of alum ammonium alum. until the ammonium alum alum has dissolved. Then boil the solution for 30 to 60 minutes. Add the amount of molasses to the solution so that the addition of dry matter is 60 parts by weight. Dry the solution in a spray dryer and transfer the resulting powder to a stirred silo, adding 33 parts by weight of MgO pellets.

CS 271759 B1 waste from cellulose production. Mix the silo content until the MgO pellets are evenly distributed throughout the silo content. A combined aluminum tanning agent with a self-base effect is formed.

Example 2

In a reaction vessel equipped with stirring, reflux condenser, heating and cooling, 1,300 parts by weight of a solid mixture of mono-, di- and trisulonic acids or a mixture thereof with a dry matter content of 95% by weight, having an acid number of 345, 160% by weight. parts of water, 10 wt. parts of sulfuric acid, heat to 95-100 ° C and gradually add 240 wt. % of formaldehyde 37 X wt. The reaction mixture is boiled and 150 wt. of aluminum sulfate and heated at 110-115 ° C for 3 hours. Cool to 60 ° C and gradually add 400 wt. parts of water, 40 wt. parts by weight of glycerine and 820 wt. % sodium hydroxide 40 wt. PH value 0.5X wt. the dry product solution is in the range of 3.2 to 3.6. Dry the finished product in a spray dryer.

Example 3

In a reaction vessel with stirring, reflux condenser and heating, add 500 wt. parts of water and 342 wt. The mixture was heated to 60-80 ° C with stirring until the aluminum sulfate dissolved. Then add the waste syrup from xyloza production so that the addition of xylose dry matter is 240 wt. parts, mix and add gradually 160 masses. parts of sodium carbonate, stir the resulting mixture. Add 450 wt. parts by weight of naphthalene mono-, di-trisulonic acid condensate, or a mixture thereof, with formaldehyde, 50% by weight; and dry the mixture to 80 ° C for 90 minutes. Dry the resulting solution in a spray drier. A combined aluminum tanning substance having a theoretical basicity of 50 ⁰ Schorlemmer.

Example 4

Into a reaction vessel equipped with a stirrer, a reflux condenser and the possibility of heating and cooling, 416 wt. parts of condensate with formaldehyde naphthalene of mono-, di- and trisulonic acids or a mixture thereof with a dry matter content of 50% by weight; add 115 wt. Heat the mixture and stir until the basic aluminum chloride dissolves, then boil the solution for 30 to 60 minutes. After boiling, add 36 wt. parts of glucose.

Example 5

The reaction vessel with stirring, reflux condenser and heating is then charged with 500 wt. parts of water and 249 wt. basified parts of aluminum sulfate 50 ⁰ Schorlemmer mixture are heated with stirring until basic aluminum sulphate dissolved. Then add 155 parts by weight of fructose to the solution, mix. Add 450 parts by weight. of condensate (50% by weight of dry matter) of naphthalene mono-, di- and trisulonic acids or their mixture with formaldehyde and heated to 80 ° C for 90 minutes. The resulting product is dried in a spray dryer.

Claims (2)

SUBJECT OF THE INVENTION Process for the preparation of a combined tanning agent from naphthalene mono-, di- and trisulfonic acids or a mixture thereof prepared by condensation with formaldehyde in an acid medium, characterized in that the condensates are heat treated for 30 to 120 minutes at a temperature of 50 to 110 ° C with aluminum salts of formula A10H _n <S0 ^) ^ j _n y / 2 ^neb0 Al (0H) _n Clj_ _n where n = 0-3 or salts type maks ^ jj. ^{x H} 2 ^{0, where M Na + or 0 K +} or ΝΗΪ, in an amount such that the dry matter of the product contains 3 to 15 X h of mass Al ₂ O 3 and stabilizing agents of the formula R 1 are added IpH OH where N 2 to 6, R 1 ’ R ₂ = -H or a -CHO or -C _0-CH2 0H where m = 1 to 6 in an amount of 0.2 to 3 moles to or inorganic acid or alkali in an amount such that the theoretical those salts contained in the product was 75 ⁰ Schorlemmera. per 1 mol of aluminum-