DE1249445B - Impregnation of leather - Google Patents

Description

FEDERAL REPUBLIC OF GERMANY

GERMAN

PATENT OFFICE

EDITORIAL

Int. Cl .:

C14 c.

JlooS \

German class: 28 a-9

Number: 1 249 445

File number: B 5.3244 IV c / 28 a

Filing date: May 14, 1959

Opened on: September 7, 1967

The subject of patent 1,061,478 is the use of solutions of the condensation products Aluminum alcoholates and monoesters of phosphoric acid with higher molecular weight organic hydroxy compounds in organic solvents for impregnating leather. Apply the impregnations the leather has water-repellent properties as well as water resistance and impermeability and primarily used for the production of pastel-colored or white suede and grain leathers Interest.

It has now been found that these impregnating agents can be improved significantly if one uses it in conjunction with silicone oils. This achieves a considerable improvement in the so-called dynamic water resistance, d. H. the water resistance under mechanical stress. This The effect can be improved even further if hard waxes are also used in addition to these two components used.

With silicone oils alone or with wax impregnation alone, you cannot achieve a really satisfactory one Increase in dynamic water resistance, which also applies to the use of the impregnation agent of the main patent has to apply alone. This effect can only be achieved if you use the invention the combinations described above are used. It is possible to do the normally necessary Reduce quantities of impregnation agents according to the main patent.

Accordingly, when using solutions, the condensation products are made from aluminum alcoholates and monoesters of phosphoric acid with higher molecular weight organic hydroxyl compounds in organic solvents for impregnating leather according to patent 1 061 47S silicone oils according to the invention and, if necessary, hard waxes are also used.

The use of the mixtures described above takes place in the usual way by spray application, application machines or by dipping. Cheap Application concentrations of the organically dissolved impregnation agent mixtures are 2 to 15%, preferably 5 to 10% solutions. When spraying with a spray gun, mau is best used 10% solutions, when diving it is best to use around 5% solutions. The concentration of impregnating Components in these solutions oll about 15 to 50% of condensation products according to the main patent, about 15 to 50% silicone oil and about 0 to 30% hard wax.

Suitable solvents are chlorinated hydrocarbons, such as trichlorethylene or perimpregnation of leather

Addendum to the patent: 1,061,478

Applicant:

Böhme Fettchemie G. mb H.,
Düsseldorf-Holthausen, Henkelstr. 67

Named as inventor:

Dr. Rudi Heyden,

Dr. Jürgen Plapper, Düsseldorf

chloroethylene, volatile hydrocarbons, such as petroleum fractions having a boiling point of 50 to 200 ⁰ C, or further organic solvents such as methyl ethyl ketone, cyclohexanone or Butylessigsäureester.

The condensation products used according to the main patent are described in detail in that patent. These are primarily condensates made from aluminum isopropylate or aluminum butylate with preferably monoalkyl phosphoric acid esters with alkyl radicals of at least six carbon atoms.

Oil-like silicones are primarily understood to mean the known organopolysiloxanes, which are characterized by —Si — O — Si groups.

The silicon atoms of the silicones can be substituted by organic radicals, such as alkyl, aryl, aralkyl, alkylaryl radicals, or alkoxy groups. Of particular interest are those organosilicon polymers that, in addition to the organic radicals, such as. B. the methyl radical, still contain hydrogen atoms. These products are in the form of solutions in organic solvents, such as. B. methylene chloride, commercially, which also usually katalg p a to en. such as B. tetrabutyl titanate, enthg ^ n. ~ "^

For those under the Enmdjljjjl aj | Impregnation-tung components are used natural or synthetic waxes used

709 640/488

bar, like ζ. Β. Paraffin wax, beeswax, camauba wax or in particular montan wax or ester or. Synthetic carbonamide waxes. the various components can be resolved without difficulty in the solutions according to the main patent.

While you are using the immersion procedure is pretty much independent of the type of solvent mentioned, are suitable when using the Spraying process for impregnating leather only solvent mixtures that contain higher boiling components, such as heavy gasoline, toluene or xylene. You can by adding small amounts of mineral oil ensure that the impregnation agent does not adhere too strongly to the leather surface layer when spraying, but penetrate the leather. Low-boiling solvents are unsuitable in this case because they When spraying the diluted impregnation agent evaporate too quickly and the impregnation agent is mainly deposited on the leather surface, even when using the immersion process one can the distribution of the impregnation agent in the leather by changing the proportion of higher boiling points Regulate solvents.

The use according to the invention as an impregnating agent can be used for all types of leather and is especially preferred for the production of pastel-colored or white suede or grain leather Upper leather suitable.

example 1

20 parts by weight of the solution of a condensation product according to the main patent 1 061 478, from 204 parts of aluminum isopropoxide and 144 parts by weight of monoalkyl phosphoric _{acid ester (alkyl radicals C 12} to C ₁₈ ) in 500 parts by weight of trichlorethylene are diluted with 30 parts by weight of trichlorethylene and then mixed with 50 parts by weight of a solution that consists of 5 parts of montan wax, 7.5 parts of an oily dimethylpolysiloxane and 110 parts of trichlorethylene. The finished solution contains about 12% impregnating ingredients. The solution is suitable for impregnating chrome leather by dipping, whereby excellent dynamic water resistance effects are obtained.

Example 2

2.5% montan wax and 3.7% oily silicone were dissolved in 70 parts of heavy gasoline (boiling point 140 to 200 ^{° C.).} This solution was mixed with 20 parts of the solution of the condensation product of aluminum isopropoxide and a monoalkylphosphoric ester mixture used according to Example 1. This impregnation agent is particularly suitable for spraying chrome upper leather. After drying and a storage time of a few days, the leather was tested in the maeser machine.

Water-

Start of entry according to number Buckling water absorption (%) after

10000 I 20000

Kinks

Let through
Amount of water

after

10000 buckles (g)

Untreated leather
Treated leather ...

1200 more than 50,000 7.8
5.3

14.8
8.4

0.17

Example 3

An aniline-dyed calfskin was soaked in the trichlorethylene solutions of the following impregnation agents for 5 minutes submerged:

Solution A, consisting of 2.5% of the condensation product of aluminum isopropylate used according to Example 1 Monoalkyl phosphoric acid ester and 1.25% oily silicone;

Solution B, composed like solution A with the addition of 1.25% montan wax;

Solution C, consisting of 3.75% of the condensation product prepared according to Example 1 and 0.65% oily silicone.

Solution D, consisting of 3.75% of the condensation product produced according to Example 1 and 0.65% oily silicone and an additional 1.5% montan wax.

When testing these leather impregnations, the following values are obtained:

Untreated leather

Impregnated with

Solution a

Solution b

Solution C

Solution D

As comparison impregnations are used

Oily silicone alone (5%
Solution)

Montan wax alone (5%
Solution)

Water-

Start of entry according to number
Kinks

over 100,000

over 100,000

18 500

85,000

Example 4

Chrome-tanned, aniline-dyed clothing leathers were immersed in 5% trichlorethylene solutions for 5 minutes dipped into the following impregnation agent:

1. Oily silicone (100 ° / ₀ ig),

2. Impregnation agent according to Example 1 above.
After drying and a storage time of a few

Days the following impregnation effects were measured:

Water-

Durchtrittsbegiiui according to the number of kinks water absorption (%) according to

10,000! 20000

Kinks

Let through
Amount of water

after

10,000 kinks
(G)

Untreated leather

Leather impregnated with oily silicone

Impregnated leather according to Example 1

200

2,300 more than 100 124

13th
4.1

131

5.4

21.7
1.4

It is already a process for waterproofing leather on the basis of silicone oils in a mixture became known with alkoxypyridinium salts. However, this procedure does not provide any appreciable improvement the impermeability of the leather to water. In contrast, there is that according to the invention achieved effect not simply in an intensification of the usual water repellent effect, as it is achieved by the individual components is given. Rather, the special combination according to the invention a completely new and extremely valuable waterproofing effect is achieved by knowing the effect of the individual components could not be derived.

Claims (2)

Patent claims: 1. Further development of the use of solutions of the condensation products from aluminum alcoholates and monoesters of phosphoric acid with higher molecular weight organic hydroxyl compounds in organic solvents for impregnating leather according to patent 1,061,478 through the use of silicone oils and, if necessary, hard waxes. 2. Use of solutions according to claim 1 together with leather oils, in particular mineral oils. Considered publications: German Patent No. 968 723;
German Auslegeschrift No. 1 018 836;
French Patent Nos. 1078 673,1110,286; Swiss patent specification No. 230 181.