RU2461594C1 - Modified bitumen - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: modified bitumen contains an amine adhesion activator. Components are in the following ratio in wt %: amine adhesion activator 0.5-2.0, bitumen - up to 100. The amine adhesion activator used is a product of reaction of boric acid, diethanolamine and a mixture of C₆-C₂₀ plant oil fatty acids, with molar ratio of reactants of 1:3:(0.5-2.5), respectively.

EFFECT: use of the modified bitumen enables to obtain hydrophobic structural materials and protective coatings with high biostability.

5 tbl, 5 ex

Description

The invention relates to a new composition of bitumen, which can be used in road construction, in the construction of foundations of buildings and structures, the manufacture of roofing and waterproofing materials, pipeline construction.

Known modified bitumen for road construction, including an amine adhesion promoter - aniline production waste - aniline resin with an amine number of at least 150 in an amount of 1.0-1.5 wt.%. A binder is obtained by mixing bitumen and resin at a temperature of 120-140 ° C for 40-60 minutes (RU 2063990 C1, class C08L 95/00, C04B 26/26, 20.07.1996).

A disadvantage of the known binder is that it contains aniline production waste, the composition of which varies in a wide range, which does not allow to obtain ready-made bitumen of standard quality.

The closest analogue of the proposed technical solution is modified bitumen, including hexamethylenetetramine as an amine adhesion promoter and additionally a product of semi-coking coals in the following ratio of components, wt.%: Bitumen - 80.00-92.00, semi-coking product of coals - 8.00-20 , 00, hexamethylenetetramine in excess of 100% - 0.35-1.00. Modified bitumen is obtained by mixing the initial bitumen with a semi-coking product of coal at 110 ° C until a homogeneous mixture is introduced into which hexamethylenetetramine is introduced, followed by heating to 160 ° C and isothermal exposure of the mixture for 30 minutes with continuous stirring (RU 2241011 C1, cl C08L 95/00, C08K 5/17, C04B 26/26, 11/27/2004).

The disadvantage of this bitumen is its relatively low resistance to mold. In addition, modified bitumen is subject to a fairly rapid aging process, as evidenced by changes in mass and softening temperature after heating.

The technical result of the invention is to improve the quality and mushroom resistance of bitumen.

This result is achieved by the fact that the modified bitumen, including the amine activator of adhesion, as the amine activator contains the reaction product of boric acid, diethanolamine and a mixture of fatty acids of vegetable oils of the C ₆ -C ₂₀ fraction with a molar ratio of reactants 1: 3: (0.5- 2.5), respectively, in the following ratio of components, wt.%:

Specified Amine Adhesion Activator 0.5-2.0 Bitumen up to 100

A distinctive feature of the proposed binder is that the introduction of a product of the interaction of boric acid, diethanolamine and a mixture of fatty acids of vegetable oils of the C ₆ -C ₂₀ fraction with a molar ratio of reactants 1: 3: (0.5-2.5) in an amount of 0, 5-2.0 wt.% (Hereinafter referred to as the interaction product) allows to increase the resistance of bitumen to mold, adhesion to stone materials, metals, wood, etc. In addition, the interaction product slows down the aging process of bitumen, as its mass and temperature softening after warming up rakticheski not changed.

The introduction of the proposed bitumen in asphalt mixtures, building, roofing and insulation materials makes it possible to increase their water-repellent properties and biostability.

The introduction of the interaction product in an amount of less than 0.5% does not significantly improve the quality of bitumen. Its introduction of more than 2% is impractical, since it does not have a further impact on quality indicators.

The process of interaction of boric acid with diethanolamine and a mixture of fatty acids of vegetable oils of the C ₆ -C ₂₀ fraction with other molar ratios of the reagents, other than those stated, does not allow to obtain a product that is soluble in bitumen.

Fatty acids are isolated from vegetable oils (sunflower, coconut, flaxseed, soybean, etc.) by splitting triglycerides, for example by saponification of the oil with alkali, followed by treatment of the soap with mineral acid to isolate the mixture of acids of the C ₆ -C ₂₀ fraction (Raw materials and intermediates for paints and varnishes: Reference manual / Edited by M.M. Goldberg. - M .: Chemistry, 1978. - P.230, 234).

In the synthesis, boric acid is used, corresponding to GOST 18704-78, diethanolamine - TU 6-09-2652-91.

A method of obtaining an interaction product is as follows.

In a reactor equipped with a stirrer, a Dean-Stark nozzle, a reflux condenser and a thermometer, a mixture of fatty acids of vegetable oils of fraction C ₆ -C ₂₀ and diethanolamine (DEA) is loaded. The reaction mass is heated with stirring to 90-100 ° C, after which boric acid is introduced and the temperature of the reaction mixture is raised to 180-200 ° C, keeping it at this temperature for 2.0-2.5 hours until a homogeneous mass with amine forms not less than 40 mg HCl / g. The molar ratio of boric acid: diethanolamine: a mixture of fatty acids is 1: 3: (0.5-2.5).

The resulting product is an oily brown viscous liquid. It is soluble in mineral oils, bitumen, organic solvents and has the following characteristics:

Kinematic viscosity at 100 ° C, cSt - not more than 65.0.

Amine number, mg HCl / g - at least 40.

Water content,% - not more than 0.5.

Ash content,% - absence.

Flash point in an open crucible, ° С - not lower than 230.

Oil bitumen is used as bitumen in accordance with GOST 22245-90, oil construction bitumen in accordance with GOST 6617-76, oil roofing bitumen in accordance with GOST 9548-74 and oil insulating bitumen in accordance with GOST 9812-74.

The technology for producing the proposed modified bitumen is as follows.

98.0-99.5 wt.% Of bitumen and 0.5-2.0 wt.% Of the reaction product are loaded into a mixer equipped with heating and a mixer, and mixing is carried out at a temperature of 130-150 ° С for 10-20 min. obtaining a homogeneous mass. The resulting bitumen is mixed with a mineral filler heated to 160-170 ° C for the preparation of the asphalt mix, and is also used in the manufacture of roofing material and insulation coating.

The specific compositions of the proposed modified bitumen are presented in table 1, their quality indicators are shown in table 2. Examples 4 and 5 are control.

For a comparative analysis of quality indicators, bitumen BNK 90/30 and BNI-IV were obtained, modified with a thermal fraction> 230 ° C of a semi-coking coal tar and hexamethylenetetramine according to the patented prototype method.

The penetration of bitumen was determined according to GOST 11501-78, ductility (elongation) - according to GOST 11505-75, softening temperature on the ring and ball - according to GOST 11506-73, flash point - according to GOST 4333-87, fragility temperature - according to GOST 11507-78 , weight change after warming up - according to GOST 18180-72, resistance to mold fungi - according to GOST 9.049-91 method 1. The scale for assessing mushroom resistance according to method 1 is presented in table 3.

Hot asphalt mixes of standard composition according to GOST 9128-2009 type B grade II, wt.%: Crushed stone of fraction 5-20-30, sand from crushing screenings - 58.5, mineral powder were prepared with the proposed binder according to example 1 and the binder according to the prototype - 5, modified bitumen - 6.5, of which dense asphalt concrete was made.

Evaluation of the adhesive ability of the proposed modified bitumen to gravel was carried out according to the method described in the description of the patent of the Russian Federation 2241011 (prototype).

For this, individual gravel particles with dimensions of at least 10 mm were dried to constant weight at a temperature of 105 ° C. Then each particle of crushed stone was tied to a thin wire, heated in a thermostat for 1 h at a temperature of 140-160 ° С and immersed for 15 s in a cup with a binder heated to the same temperature. The particles extracted from the binder were suspended on a tripod to drain excess binder, after which they were cooled at a temperature of 20 ° C for at least 15 minutes. Then, the treated particles of crushed stone were lowered into a glass with slowly boiling distilled water for 30 min and the adhesion force of the binder was determined according to the scale given in Table 4.

With the proposed bitumen according to example 2 and similar bitumen according to the prototype, fused roofing materials were made, which were fiberglass, on which 3 to 5 kg of each of the modified bitumen was applied.

With the proposed bitumen according to example 3 and the corresponding bitumen according to the prototype, compositions for protecting pipelines were prepared, containing, wt.%: Modified bitumen - 50, solvent - 50.

Qualitative indicators of the resulting coatings are presented in table 5.

The resulting asphalt concrete was tested according to GOST 12801-98, roofing materials - according to GOST 2678-94, protective coatings for the pipeline - according to GOST 9.054-75 and GOST 15140-78.

Using the proposed modified bitumen allows to obtain hydrophobic building materials and protective coatings with high biostability.

Table 1 Components The composition of the modified bitumen according to examples, wt.% one 2 3 four 5 The product of the interaction of boric acid, DEA and a mixture of fatty acids of vegetable oils fraction C ₆ -C ₂₀ in a molar ratio of 1: 3: 0.5 0.5 0.3 The product of the interaction of boric acid, DEA and a mixture of fatty acids of vegetable oils fraction C ₆ -C ₂₀ in a molar ratio of 1: 3: 1,5 1.25 2.5 The product of the interaction of boric acid, DEA and a mixture of fatty acids of vegetable oils fraction C ₆ -C ₂₀ in a molar ratio of 1: 3: 2.5 2.0 Bitumen BND 90/130 99.5 99.7 BNK 90/30 98.75 BNI-IV 98.0 97.5

table 2 Indicator The value of the indicator for examples one 2 3 four 5 Suggestions modif. BND90 / 130 Prototype modif. BND90 / 130 Suggestions modif. BNK 90/30 Prototype modif. BNK 90/30 Suggestions modif. BNI-IV Prototype modif. BNI-IV Suggestions modif. BND90 / 130 Suggestions modif. BNI-IV Needle penetration depth at 25 ° C, 0.1 mm 102 96 thirty 28 35 32 94 36 Ductility at a temperature of 25 ° C, cm 75 78 10 12 10 13 73 9 The softening temperature of the ring and ball, ° C 55 57 90 92 80 83 53 82 Change in softening temperature after heating, ° C 0.5 four 0.5 5 0.5 6 one 0.5 The change in mass after heating,% 0,07 0.7 0.05 0.5 0,03 0.5 0.09 0.02 Fraas fragility temperature, ° С -19 -16 -fourteen -12 -12 -10 -17 -12 Flash point, ° С 270 260 265 257 267 260 270 268 Mushroom resistance according to method 1, points one 3 one 3 one 3 2 one Adhesion to mineral materials, points 5 5 5 four 5 four four 5 Adhesion to steel, MPa 0.5 0.4 0.9 0.7 1,0 0.9 0.4 1,0

Table 3 Method The degree of development of molds Material grade GOST 9.049 ISO 846 one 0 The material is not a nutrient medium (neutral or fungistatic) 12 - The material contains nutrients that provide insignificant development of mushrooms. 3, 4, 5 The material contains a sufficient amount of nutrients conducive to the development of mushrooms.

Table 4 Evaluation of adhesion of bitumen with crushed stone, points Characterization of the surface of mineral particles treated with a binder in the evaluation of wetting before boiling, and adhesion after boiling 5 (excellent) The entire surface of the mineral particles is uniformly coated with a binder, i.e. the binder film is fully preserved 4 (good) The entire surface of the mineral particles is covered with a binder, but the binder is unevenly distributed throughout the thickness 3 (satisfactory) Some parts of the surface of mineral particles are not covered with a binder, i.e. the binder film is displaced by water. There is an exposure of individual sections on the surface of the particles (at least 50%) 2 (bad) The surface of the mineral particles is exposed to more than 50%

Table 5 Indicator Asphalt concrete Roofing material Protective coating for the pipeline with the proposed bitumen with bitumen prototype with the proposed bitumen with bitumen prototype with the proposed bitumen with bitumen prototype Water saturation, vol.% 0.90 1.55 - - - - Water resistance coefficient 1.10 0.90 - - - - Swelling, vol.% 0.10 0.50 - - - - Water absorption during the test 24 hours,% 1.15 1.30 Water resistance at a pressure of 0.001 MPa, h one hundred 90 Water displacement, mm - - - - 120 90 Mushroom resistance according to method 1, points 0 2 0 2 0 2

Claims (1)

Modified bitumen, including an amine adhesion activator, characterized in that it contains the product of the interaction of boric acid, diethanolamine and a mixture of fatty acids of vegetable oils of the C ₆ -C ₂₀ fraction with a molar ratio of reactants 1: 3: (0.5- 2.5), respectively, in the following ratio of components, wt.%:
specified amine adhesion promoter 0.5-2.0 bitumen up to 100