RO115448B1 - Additive composition for bitumens and process for preparing the same - Google Patents

Abstract

The invention relates to an additive composition for bitumens, applicable to the road building, for additivating road and insulating bitumens, comprising 01 95 % polyalkyl polyamidopolyalkylenepolyamine, 01 70 % fatty acids, 01 95 % ammonium salt, 01 6 % glycerine esters, 01 3 % glycerine, 01 2 % water, the parts being expressed by weight, and it also relates to the process of preparing the composition, comprising subjecting a linear polyethylenepolyamine having 2 6 baric nitrogen atoms to total thermal condensation reaction with fatty acids, at a molar ratio of fatty acids to amine of 1 5, at the temperature of 110 170 degrees C, for 2 8 hours, the obtained polyalkyl polyamido polyethylenepolyamine being mixed with fatty acids, ammonium salts, glycerine esters, glycerine, water and homogenized under the conditions known per se The additive composition for bitumens can be used for preparing the asphaltic mixtures, bitumen emulsions, bitumen primer solutions used for building and maintaining the roads; it is compatible with other bitumen additions, such as antioxidants, elastomers, cellulose, it is efficient as it increases the bitumen adhesiveness to the rocks of various acidic, basic, quarry or gravel pit mineralogic structures

Description

The invention relates to a composition of additives for bitumens, used in road construction, to the additives of road bitumen and insulation, and to a process for obtaining it.

It is known that the adhesion of bitumen to a mineral aggregate support, fiberglass, cellulose material, etc., is of great importance for the durability of bitumen coatings.

The adhesiveness of bitumen can be improved by adding, in bitumen, chemical agents that provide a tenacious bond between bitumen and support, known in the literature as adhesive additives, dopants or anti-stripping agents. Additives for bitumen, in general, and for road bitumen in particular, must be obtained from accessible raw materials, in order not to raise the costs of the work. They must have certain properties such as: be soluble in bitumen, not be soluble separate during storage, have a low drip point, be thermally and chemically stable at pumping temperature, mixing and use (15O ... 2OO ° C), do not negatively influence other properties of bitumen, be efficient at low concentration (0.2 ... 2%]. on both acidic and basic mineral aggregates.

Additives are known for bitumens that partially or completely satisfy the conditions mentioned above, such as additives in the class of heterocyclic amides, but which have the disadvantage that their production requires more accessible raw materials, such as piperazine and homologues of piperazine, as in in the case of bitumen additives from mixtures of linear, cyclic and branched polyamines, or such as alkyl amido-amine class additives, which has the disadvantage of requiring, in their production, N-alkylated polypropylene, difficult to access or, such as imidazolin and imidazolinic heterocyclic polymers, but which have the disadvantage that the percentage for their obtaining involves ozonation phases of the raw materials, the use of solvents and a high energy consumption for the cyclization phase.

The composition of bitumen additives, according to the invention, removes the disadvantages in that it consists of 0.1 ... 95% polyalkyl polyamide polyalkylene polyamine, 0.1 ... 70% fatty acids, 0.1 ... 95% salt of ammonium, 0.1 ... 6% glycerin esters, 0.1 ... 3% glycerin, 0.1 ... 2% water, the parts being expressed by weight, and having the consistency of a paste with density, at 20 ° C, 0.9 ... 1 g / cm ³ , drop point of 1O ... 8O ° C, inflammation temperature of 160 ... 280 ° C, basic nitrogen of

5 ... 9%, by weight, and an acidity index of 0.1 ... 220 mg KOH / g.

The process for obtaining the composition of bitumen additives, according to the invention, is that a linear polyethylene polyamine having 2 to 6 basic nitrogen atoms with natural fatty acids distilled in the C ₁₂ -C _1B range is subjected to the total thermal condensation reaction. and / or unsaturated and / or mixture thereof and / or naphthenic acids in the range C ₈ -C ₁₈ , at a molar ratio of fatty acids / amines of 1 ... 5, at a temperature of 110 ... 170 ° C 2 ... 8h, and the obtained polyalkyl polyamide polyalkylene polyamine, consisting of a mixture of linear alkylamidopolyamines, wherein the alkyl radical may be and / or and / or C ₁₅ H ₃₁ and / or and / or C _I7 H ₃₅ and / or

C ₁₇ H ₃₃ and / or C ₁₇ H ₃₁ and / or C and / or C _q1 H _2q ^ and / or C ^ H ^, where p = 6 ... 7, (7 = 8 ... 12, ιλλ = 12 ... 18 and wherein the number of nitrogen atoms can be 2 ... 6, included in a linear polyethylene polyamine structure, where the ratio of the acyl radical to the polyethylene polyamine radical is 1 ... 5 mixed with fatty acids, ammonium salts, glycerin esters, glycerin and water and homogenized under known conditions.

The ammonium salt can be a mixture of ammonium salts resulting from the saponification reaction of natural distilled fatty acids or techniques with the mixture of linear alkylamidopolyamines.

RO 115448 Bl

Glycerin esters can be a mixture of mono, di, and triesters, in any proportion 50 of natural fatty acids, such as vegetable fats or oils, but which may also be in the composition of natural technical fatty acids.

Fatty acids may be natural or technical distilled fatty acids, in the range C ₁₂ -C ₁₈ , and / or naphthenic acids in the range C ₈ -C ₁₈

The composition of bitumen additives according to the invention has the following 55 advantages:

- it is obtained from raw materials accessible as linear polyethylene polyamines, by a process that does not require the use of solvents, applicable in existing installations, at a low cost price;

- it can be used in the preparation of asphalt mixtures, bitumen emulsions, 60 bitumen-based solutions used in road construction and maintenance;

- it can be used for the additives of all kinds of road bitumen;

- does not change the basic properties of bitumen;

- is compatible with other bitumen additives such as antioxidants, elastomers, cellulose, etc .; 65

- is effective in increasing the adhesion of bitumen to rocks of different mineralogical, acidic, basic, quarry or ballast structures;

-Improves the resistance of asphalt mixtures to water;

- it is soluble in any proportion in bitumen;

- is physically, chemically and thermally stable; 7Q

- has a low drip point.

Three examples of embodiments of the invention are given below.

Example 1. 282 g oleic acid and 146 g triethylentetramine are introduced into a glass reactor, so that the molar acid / amine ratio is 1, homogenized, heated for 6 h at 165 ° C, when by total thermal condensation 18 is removed. g of 75 water and 410 g of linear oleylamidopolyethylene polyamine are obtained after cooling, having 3 basic nitrogen atoms. 20 g oleic acid, 6 g triolein, 2 g glycerin and 2 g water are added and homogenized at 50 ° C for 30 minutes, when 440 g of bitumen additive composition is obtained, consisting of a paste with a density at 20 ° C of 0.959 g / cm ³ , drop point of 32 ° C, inflammation temperature of 198 ° C, basic nitrogen 80 of 8.975%, and an acidity index of 4.51 mg KOH / g.

Example 2. In a glass reactor, 540 g of natural fatty acids, consisting of 1.3% lauric acid, 1.9% myristic acid, 31% palmitic acid, 3.9% palmitoleic acid, 13% acid, are introduced. stearic acid, 45.6% oleic acid, 3.3 linoleic acid and 189 g tetraethylene pentamine, so that the acid / amine molar ratio is 2, homogenized, heated 7 hours at 170 ° C when, by total thermal condensation , 36 g of water are removed and, after cooling, 693 g of linear polyalkyl polyamide polyethylene polyamine having 3 basic nitrogen atoms are obtained. 70 g of natural fatty acids, as above, 35 g of refined soybean oil, 15 g of glycerin and 8 g of water are added and homogenized at 50 ° C for 30 min, when 821 g of bitumen additive composition is obtained, having consistency of a paste with a density at 20 ° C of 0.942 g / cm ³ , a drop point of 54 ° C, a flash temperature of 265 ° C, a basic nitrogen of 5.11%, and an acidity index of 8 , 84 mg KOH / g.

Example 3. In a glass reactor 217 g of distilled technical oil, consisting of 15% sum of natural saturated and unsaturated C ₁₆ fatty acids and 85% of 95 natural C ₁₈ saturated and unsaturated fatty acids and 110 g of triethylenetetramine, is introduced so that the molar ratio of acids / amines to be 1.067, homogenized, heated gradually for 4 hours to 160 ° C and maintained at this temperature for 4 hours, when

RO 115448 Bl removes 14.5 g of water and, after cooling, 312.5 g of linear polyethylene polyamide polyethylene, having 3 basic nitrogen atoms. Add 23 g of distilled technical olein as above, 0.4 g of refined soybean oil, 0.4 g of glycerin and 0.4 g of water and mix at 50 ° C for 30 minutes, when 336.6 g is obtained. composition of additives for bitumen, consisting of a paste with a density at 20 ° C of 0.967 g / cm ³ , a drop point of 42 ° C, a flash temperature of 232 ° C, a basic nitrogen of 8.5%, and an index acidity of 6 mg KOH / g.

Claims (2)

claims 1. Composition of bitumen additives, characterized in that it consists of 0.1 ... 95% polyalkyl polyamide polyalkylene polyamine, 0.1 ... 70% fatty acids, 0.1 ... 95% ammonium salt, 0.1 ... 6% glycerin esters, 0.1 ... 3% glycerin, 0.1 ... 2% water, the percentages being expressed by weight, and consist of a density paste at 20 ° C. , of 0,9 ... 1g / cm ³ , drop point of 10 ... 8CPC, inflammation temperature of 16O ... 28O ° C, basic nitrogen of 5 ... 9%, by weight, and a acidity index of 0.1 ... 220 mg KOH / g. 2. Process for obtaining the composition of bitumen additives according to claim 1, characterized in that a linear polyethylene polyamine having 2 to 6 basic nitrogen atoms, with natural fatty acids, distilled in the field is subjected to the total thermal condensation reaction. C ₁₂ -C _1B saturated and / or unsaturated and / or mixture thereof and / or naphthenic acids in the range C _a -C ₁₃ , at a molar ratio of fatty acids / amines of 1 ... 5, at a temperature of 11O ... 17O ° C, for 2 ... 8h, obtained polyalkyl polyamide polyalkylene polyamine, consisting of a mixture of linear alkylamidopolyamines, wherein the alkyl radical may be C 1 H 2 and / or C ₁₃ H ₂₇ and / or C ₁₅ H ₃₁ and / or C ₁₅ H _2g and / or C ₁₇ H ₃₅ and / or C ₁₇ H ₃₃ and / or C ₁₇ H ₃₁ and / or ^ H ^ and / or C ^ H ^ and / or C ^ H ^ g, in which p = 6 ... 7, q = 8 ... 12, i / v = 12 ... 18 and wherein the number of nitrogen atoms can be 2 ... 6, included in a linear polyethylene polyamine structure, wherein the ratio of radical The acyl and polyethylene polyamine radical is 1-5, being mixed with fatty acids, ammonium salts, glycerine esters, glycerin and water, and homogenized under known conditions.