CS262845B1 - Impregnating and laminating agent - Google Patents

Abstract

The present invention relates to a composition for the manufacture of laminated materials, impregnation of porous materials, coating of various materials for the production of waterproof, benzine-resistant and oil-resistant seals and coatings based on phenol-formaldehyde resins. The composition is comprised of condensate which is not used in the purification of 2,6-xylonel by means of phenol formaldehyde or paraformaldehyde or a solution thereof in aromatic solvents emulsified in water.

Description

The invention relates to a composition useful for impregnating porous materials, such as wood, paper, concrete, against the effects of moisture, mold, fungi and bacteria, as a coating for surface treatment or as a binder for the production of laminated materials.

Recently, very advantageous chemical refining processes for crude xylenol have been patented (see, e.g., A.O. 230.842,

A.O. These processes are based on the fact that the by-products accompanying 2,6-xylenol, phenol derivatives having at least one free o-position relative to the phenolic OH group, can be practically removed by heating this mixture with paraformaldehyde, aqueous formaldehyde solution, or with formaldehyde-releasing substances, in the presence of catalysts, ensuring their condensation with formaldehyde predominantly into the o-position.

The condensation reaction product is a substantially linear low molecular weight condensate of phenol and its methyl derivatives with formaldehyde, characterized by disinfectant and fungicidal effects, readily fusible usually between 50 and 80 ° C and soluble in common organic solvents, especially alcohols, ketones, aromatic and chlorinated hydrocarbons.

The properties of this waste condensation product can be advantageously utilized on the one hand in the production of laminated materials, in particular paper, fabric and wood veneer, as disclosed in A.O. 240372, both as an impregnating agent as disclosed in A.O. 240579.

It has now been found that all the described applications and utilization of the waste condensation product can be achieved in a simpler manner by preparing an emulsion from the phenol-cresol-xylenol-formaldehyde condensate waste and impregnating, coating or laminating the emulsion.

SUMMARY OF THE INVENTION The present invention provides an impregnating and laminating agent based on the condensation products of phenol, cresols and xylenols with formaldehyde resulting from the chemical refining of 2,6-xylenol using for262 84S maldehyde or paraformaldehyde containing 100 parts by weight of condensate, 5 to 100 parts by weight of emulsifier. 1000 parts by weight of water and up to 200 parts by weight of an aromatic hydrocarbon.

The use of a condensate emulsion achieves a more advantageous effect, which results in higher smoothness and homogeneity of the coatings, easier spreading, impregnation and lamination with improved absorbency caused by the presence of the emulsifier in the emulsion, which ensures deeper penetration of the agent into the pores of porous materials and between fibers. This fact is especially evident on laminated materials, which even after water soaking practically does not show any significant change in strength. Laminated materials show an emulsion savings compared to the solution used, with improved mechanical properties and it turns out that these emulsions have a much wider application Thus, for example, emulsions may be added to concrete to reduce the water absorption of plasters for the same purpose, to bond various materials, at least one of which is porous, e.g. parquet on a concrete base - a water-oil-petrol-resistant joint, etc. is obtained, in addition to the mentioned economic and environmental benefits.

The preparation process is simple and does not depart from the general practice of preparing emulsion systems. For example, the condensation product of a mixture of cresols and xylenols with paraformaldehyde or an aqueous formaldehyde solution containing residual 2,6-xylenol is dissolved together with the emulsifier in an organic solvent, preferably aromatic a hydrocarbon, e.g. in toluene or xylene, or in chlorinated hydrocarbons such as chloroform, carbon tetrachloride or trichlorethylene (also chlorinated aromatic hydrocarbons may also be used) and this solution is mixed with the necessary amount of water. It is advisable to filter the solution, since the condensation product contains a smaller amount of catalyst (zinc salt) which does not dissolve in these solvents. The nature of the condensate allows the preparation of concentrates containing condensate, emulsifier or organic solvents and a small amount of water. use by dilution with water.

Various types of surfactants can be used as emulsifiers. anionic, cationic and nonionic. From anionic sodium dibutylnaphthalenesulfonate, for example cationic laurylamidoethylpyridinium chloride, or nonionic various oxyethylated fatty alcohols.

262 845

Emulsification should be carried out hot (to dissolve it faster in solution).

Solutions of waste condensation products in aromatic or chlorinated hydrocarbons can also be added (depending on the type of material to be treated) various additives soluble in these solvents, e.g. plasticizers, such as tricresyl phosphate, or dibutyl phthalate, to increase the flexibility of the lacquer layer, various flame retardants, e.g., Retar 131 (diphenylisopropylphenyl phosphate).

Treatment of materials with this suspension is smooth, shiny, mechanically and weather-proof, very transparent. Transparency allows the use of coatings where it is important that the structure of the original material remains visible. However, the waste condensate emulsion can be freely treated, such as dyeing, and The invention is illustrated by the following examples, in which the examples are by weight.

Example 1

As described in AO 231085, Example 1, 500 g of 2,6-xylenol were refined. The xylenol used for refining contained 20.2% of other phenol methyl derivatives.

After the refining and distillation of pure xylenol was complete, the residue in the digester was stirred with 150 g of toluene and the resulting condensation solution separated from a small amount of solid by filtration. 308 g of solution were obtained. The concentration of waste product dissolved in toluenes was determined by evaporation. , 36%. 20 g of Slovasol 0 were dissolved in the solution thus obtained at 40 ° C and the whole mixture was poured into 308 g of water heated to 65 ° C while stirring. The resulting emulsion can be diluted several times without breaking.

The prepared emulsion diluted 2-fold with water was impregnated with a wooden cube with a 6 cm edge of dried fir wood, which after drying the paint was alternately wetted with water (30 min) and after wiping water from the surface freely dried in the air stream.Maximum weight gain of impregnated cube after 30 cycles it was 2.2%. The condensate coating on the walls of the cube remained unchanged.

The weight gain of the unimpregnated identical test specimens is between 18 and 25%. After several cycles of the specimen, they burst.

The ability to use the prepared emulsion for the production of laminates was confirmed by the following procedure: the emulsions were impregnated at 35 ° C

4,262,845 100 mm x 100 mm cotton fabric strips and individual slices dried at 55 ° C. The slices were pressed together by 6 pieces at 70 ° C to 80 ° C, at a pressure of 7.5 kg / cm ² and from a compact. punching bodies of the shape of a double spoon, which had a width of 6 mm in the narrowest part. The exact height of the bodies was measured for each body separately before the tearing test / tab. 1 /.

The tear test was carried out on 10 bodies immediately after their preparation and on 10 bodies after 60 hours soaking in a 30 ° C water bath. The measured values given in Table 1 are average of the whole set of measurements and compared with the tear values of the base material and obtained from laminated bodies with the condensate solution described in AO 240372 Example 1.

The results show that emulsion lamination achieves higher strength and is little affected by long-term exposure to water.

Table 1

Sample Result of blasting tests Tensile strength of the body After exposure in o kg / mm Water No Dipping 2 kg / mm Basic material 2.6 3.2 AND Laminated material in the mold bodies-lamination performed according to AO 240372 4.4 4.6 Laminated material in the mold bodies-lamination performed by means of emulsion 4.8 5.2

Example 2

1000 g of crude 2,6-xylenol were refined as described in Example 4 of AO 230842, the xylenol used for refining contained 20.2% of other phenol methyl derivatives.

- 5,262,845

After the xylenol refining and distillation process was complete, the residue in the digester was stirred with 700 g of xylene and the resulting solution was filtered.

999 g of a solution, which was determined by evaporation to contain 300 g of dry matter, were dissolved in this solution. 160 g of Slovasol 905 were dissolved under stirring at 48 ° C, and the resulting mixture was subsequently diluted with water to a final volume of 3000 ml. .

Emulsion impregnation efficiency tests were performed as described in Example 1.

The maximum weight gain of the impregnated cube after 30 cycles was 1.8 The condensate coating on the walls of the cube remained unchanged.

Example 3

1000 g of crude 2,6-xylenol were refined as described in Example AO 230842. The xylenol used for refining contained 20.2% of other phenol methyl derivatives.

At the end of the xylenol refining and distillation process, the residue in the digester was mixed with 36 g of Slovasol 905 with stirring at 87 ° C and after complete mixing the entire digester contents were gradually dispensed into 1 l of boiling water. 254 g of a molten mixture of phenol-formaldehyde condensate and Slovasol 905 was metered in. The resulting emulsion could be freely diluted with water to emulsify the emulsion. The emulsion impregnation tests were carried out as described in Example * 1.

The maximum weight gain of the impregnated cube after 30 cycles was 1.9%. The smooth, homogeneous coating of condensate on the walls of the cube remained unchanged.

Example 4

The xylenol containing 3.6% of the other ethylened phenol methyl derivatives was refined as described in the inventive descriptions of Table 2, line 2, for xylenol chemical refining. From 100 g of the refining residue, emulsions for the production of laminates were prepared according to Example 1 The laminates were made for tear tests. The laminated materials and bodies were made as described in Example 1. The formulations were prepared from the solutions as shown in Example 1, or the melt as shown in Example 1. Example 3. Concentration and nature of the substances used are shown in Table 2. Tear tests were performed according to Example 1. The results are compared with the values given in

262 84S in AO 240372 (lines 14 and 14a in Table 2).

Table 2

Line Importance 1 Attempt number 2 Refining performed according to AO 3 Example number 4 Condensate emulsion for lamination Condensate weight g 5 solvents g 6 solvent 7 weight of emulsifier g 8 emulsifier 9 a process for preparing an emulsion according to an example 10 weight of water g 11 Lamination method of applying condensate 12 laminated material 13 Tensile strength of laminate kg / mm 2 without soaking 13a after soaking 14 Tensile strength of laminates kg / mm 2 without soaking

prepared according to AO 240372

14a after soaking

Basic tensile strength kg / mnr

1. 1 2 3 4 5 6 2. AO 232834 236607 AO 232 870 AO 235679 AO 235608 AO 236128 3. 3 13 4 1 5 7 4. 50 50 50 50 50 50 5. 50 20 May 0 0 150 200 6. toulen toulen - - xylene xylene 7. 25 10 30 30 30 30 8. Slovasol 6018 Slovasol 802 Slovasol 6018 Slovanik p _at 370 Slovasol 0 Slovasol 81 9. 1 1 3 3 1 1 10. 300 200 1 000 300 300 500 11. dipping spraying dipping dipping paint dipping 12. cotton fabric cotton fabric paper paper oak foil oak foil

- Ί 262,845

13. 4.7 4,5 1.1 1,2 5.7 5.9 13a 4.7 4,5 0.9 1,2 5.2 5.8 14. 4,5 4,5 0.9 0.9 5.6 4.1 14a 4.4 4.2 0.7 0.7 4.0 3.2 15 Dec 3.2 3.2 0.4 0.4 2.8 2.8

Notes: 1 / Average of 6 measurements / rows 13 to 15 /.

Example 5

As described in Example 4. AO 230842, 1200 g of crude 2,6-xylenol were refined. The xylenol used for refining contained 20.2% of other phenol methylderivatives. the solution was filtered.

1158 g of a solution, which was determined by evaporation to contain 328 g of dry matter, were dissolved in this solution. 200 g of Neokal were dissolved under stirring at 60 ° C and the resulting mixture was gradually diluted with water to a final volume of 1600 ml. .

Emulsion impregnation efficiency tests were performed the same; however, as shown in Example 1, the resulting emulsion was diluted with three times the volume of water.

The maximum weight gain of the impregnated cube after 30 cycles was 1.8%. The condensate coating on the walls of the cube remained unchanged.

Example 6

As described in Example 4. AO 230842, 1200 g of crude 2,6-xylenol were refined. The xylenol used for refining contained 20.2% of other phenol methyl derivatives.

After the xylenol refining and distillation process was complete, the residue in the digester was mixed with 40 g of Katexol 298 under stirring at 87 ° C, and after thorough mixing, the digester content was gradually dissolved in 1 l of boiling water. Differential weighing revealed ₀ to be dosed 275 g of molten phenol-formaldehyde condensate / cation exchange resin 298. The resulting emulsion could be freely diluted with water without breaking the emulsion. The emulsion impregnation tests were performed as described in Example 1, but the resulting emulsion was diluted with 2.5 times the volume of water. .

The maximum weight gain of the impregnated cube after 30 cycles was 2.1%. The smooth, homogeneous coating of condensate on the walls of the cube remained unchanged.

Claims (1)

262 845 Impregnating and laminating agent based on the condensation products of phenol, cresols and xylenols with formaldehyde> falling off in the chemical refining of 2,6-xylenol with formaldehyde or paraformaldehyde, characterized in that it contains from 5 to 50 parts by weight of condensate? up to 1000 parts by weight of water and up to 200 parts by weight of aromatic hydrogen.