RU2218369C2 - Method of production of composition mastics - Google Patents

Abstract

FIELD: petrochemical industry; production of composition mastics. SUBSTANCE: the invention is dealt with production of the bitumen- polymeric compositions based on the petroleum bitumen, rubber, that are used in construction, for waterproof finish, repair of concrete and asphaltconcrete coatings, filling their cracks, hermeticity, protection against corrosion, construction of a roof covering. Composition mastic contains taken in fixed amounts oil asphalt, ethylene-propylene-diene rubber , organic solvent, fuel oil, a mineral powder, comminuted rubber ant it is vulcanized by sulfur with organic accelerator of vulcanization. The method of production of the composition mastic provides for superposition of bitumen with the rubber solution in the mixture of organic solvent with fuel oil having concentration of polymer up to 25 % , where the produced reaction mass is oxygenated by an air blow at the temperature of 160 - 200 C and vulcanized with adding comminuted rubber. At production of the composition mastic they may use the mineral powder of up to 20 mass % to produced composition mastic. The invention allows to receive a high-quality material for a waterproof finish, hermeticity and manufacturing of roofing materials with use of the cheap elastomer stable to ozone-oxygen action and a thermochemical destruction, to strain ageing that influences duration of operation. Its wide range of heat and frost resistance allows to use the composition mastic in different environmental conditions of Russia. EFFECT: the composition mastic is highly resistant to high heat and frost action as well as ozone-oxygen action and a thermochemical destruction. 3 cl, 2 tbl, 1dwg, 3 ex

Description

 The invention relates to the field of production of compositions using bitumen and rubber used in construction, waterproofing, repair of asphalt concrete coatings, pouring cracks, etc.

Known mastics, consisting of bitumen, various polymers, fillers and some other components that do not have sufficient frost resistance, durability. The latest developments in this area are the following inventions:
- bitumen composition based on butadiene polymer, butadiene-styrene block copolymer (patent 2011666, France);
- bitumen composition and method for its preparation (patent 2011667, Russia);
- bitumen polymer composition and method for its preparation (patent 213285, RF).

 The disadvantages of these materials are the use of expensive elastomers, high energy consumption, low technical parameters of the materials being taught, stringent requirements for the quality of the feedstock, especially polymers, and the need to use special equipment.

 Known bitumen composition (patent 2011667) is obtained by mixing in two stages (claim 2 of the invention). First, concentrate is obtained, then heated bitumen is added and mixed. The concentrate consists of bitumen and a high molecular weight polymer of styrene-butadiene-thermoplastic elastomer or rubber crumb, which is a mixture of waste products of styrene-butadiene-latex and a low molecular weight polymer, which is a copolymer of butadiene with piperylene or acrylonitrile and a stearic acid 1,2-surfactant. .

 The disadvantages of this bituminous composition are the high cost and deficit of incoming components, especially high molecular weight styrene-butadiene thermoplastic elastomer, and the preparation technology, which provides for the final preparation of the composition in a building project, where, as a rule, there is no necessary equipment and the corresponding conditions. Moreover, it should be noted that mixing and dissolving thermoplastic elastomer in bitumen is difficult, requires high energy consumption and uniformity is not ensured. Achieving uniformity (complete dissolution of TEC in bulk) is possible with active solvents, such as benzene, toluene or mixtures thereof, which significantly worsens working conditions.

Closest to the technical nature of the proposed invention, which can be taken as a prototype, is a bitumen polymer composition and method for its preparation (patent 2132857, Russia). Bitumen-polymer composition containing rubber, bitumen, sulfur and an organic vulcanization accelerator, characterized in that the rubber contains a triple copolymer of ethylene, propylene and dicyclopentadiene and additionally contains fuel oil, or industrial oil, or toluene in the ratio of components, parts by weight: bitumen 41-94; fuel oil, or industrial oil, or toluene 3-48; rubber 3-8; sulfur 0.06-2.4; organic vulcanization accelerator 0.06-0.24. According to the second paragraph of this invention, a feature of the production method is the preliminary mixing of rubber with fuel oil, or industrial oil, or toluene at 100-180 ^o C to a homogeneous mass, adding bitumen, sulfur and an organic vulcanization accelerator to the resulting mass and mixing at 140-155 ^o C at the same proportions (parts by weight) of the components.

The disadvantages of this invention are the presence in the finished material of the so-called "bare fuel oil or industrial oil", which subsequently during operation, exposed to solar radiation, temperature and atmospheric effects (asphalt coating in the summer can heat up to a temperature of 70-80 ^o C), oxidize and dry out , aging occurs, a change in plasticity and physico-mechanical properties, internal stresses and a violation of internal bonds arise, which ultimately leads to deformation and destruction. It is assumed that fuel oil or industrial oil are plasticizers of the composition, which must be maintained at a lower limit of up to 3 parts by weight. But this assumption is refuted by the real possibility of dissolving rubber in fuel oil or oil. The maximum possible concentration of rubber in a mixture of fuel oil and / or organic solvent can be achieved within no more than 25%, by weight of the dry residue, and the minimum rubber limit in the composition specified in the invention is 3 parts by weight assumes a minimum concentration of rubber in the mixture of 50%, which is impossible to achieve.

 The use of aromatic hydrocarbons allows to achieve a higher concentration of rubber in the mixture, but distillation of an expensive solvent leads to a significant increase in the cost of the resulting composition and requires additional equipment for vapor recovery. The use of a mixture of fuel oil, oil, toluene according to the formula is not expected. It should be noted that the proposed composition has a low flash point, which increases the fire hazard of production. The present invention solves the above problems as follows.

Petroleum bitumen is combined with a solution of rubber SKEPT in fuel oil and an organic solvent, oxidized by blowing with air at a temperature of 160-200 ^o C, add crumb rubber, sulfur, sulfenamide and vulcanize the mixture at a temperature of T = 145-155 ^o C with stirring for 45-60 min with the following ratios of components, parts by weight:
Bitumen GOST 22245-90 - 70-75
State standard specification 10585-90 fuel oil - 10-30
Organic solvent TU 0250-001-04855329-94 or GOST 8505-80 - 15-30
Rubber SKEPT TU 2294-005-66801-95 - 5-15
Sulfur GOST 127.4-93 - 0.5-1.5
Sulfenamide TU 6-14-756-78 - 0.5-1.5
Rubber crumb TU 38.00149438-48-92 - 1-25
In accordance with paragraph 2 of the formula, mineral powder is added to the mixture after vulcanization up to 20% by weight of the resulting composite mastic, or according to paragraph 3 of the formula, mineral powder is added before vulcanization.

Composite mastic according to the invention is made as follows. First, a rubber solution of SKEPT is prepared. To do this, rubber pre-crushed to a crumb (fr. 5-30 mm) is mixed with an organic solvent and fuel oil and dissolved until completely homogeneous. Then the resulting solution is added to bitumen and purged with air at T = 160-200 ^o C until the required softening temperature is reached, determined by the method of Ring and Ball (T according to KiSh). Then, depending on the purpose and the required characteristics, rubber crumb, sulfur and sulfenamide are added and at a temperature of T = 145-155 ^° C for 45-60 minutes they are mixed and vulcanized. The amount of input sulfur containing (sulfur, sulfenamide) and the time of vulcanization control the final indicators of the prepared composite mastic. The degree of readiness is determined by the softening temperature GOST 11506, GOST 26589.

 Regulation of the composition and technological mode of the specified method allows you to get mastics with various properties. Mineral powder or seeding of crushing is introduced before or after vulcanization, depending on the required technical characteristics of the finished mastic, which affects the viscosity and fluidity of the mastic during operation during application, as well as its behavior during operation.

 The novelty of the invention is the oxidation of the mass by air blowing obtained after combining bitumen with a rubber solution of SCEPT, when vapors and volatiles are distilled off, oil fractions go into resins with an increase in the softening temperature and subsequent vulcanization with sulfur with an organic vulcanization accelerator - sulfenamide, which allows for minor changes in technology, on the same equipment, to receive mastics for various purposes, with different characteristics.

 Unlike the prototype, containing bitumen, fuel oil, or industrial oil, or toluene, rubber SKEPT and sulfur-containing vulcanizers, the invention allows to get rid of the dilution of the resulting composition resulting from the use of solvents that remain in its composition, which, as previously indicated, worsens the end performance. The present invention allows to get rid of the inevitable process of aging of the material from the effects of the environment during operation and during long-term storage. The use of cheap and affordable fillers extends the temperature range of operation, improves physicomechanical properties, and extends the service life.

 The invention is illustrated by the following examples of specific performance when cooking in real conditions.

 Example 1

Rubber SKEPT - 15 wt.h
Nefras S 155/200 - 30 parts by weight
M-100 fuel oil - 30 wt.h
Rubber crushed into crumbs SKEPT is mixed and dissolved in a mixture of fuel oil with nefras at T = 80-90 ^o With until complete dissolution. The resulting solution was added and mixed in 75 wt.h. bitumen BND 90/130. Next, the resulting mass is oxidized by blowing air at T = 180 ^o C, where the process is controlled by sampling with verification of the softening temperature in accordance with GOST 11506-73. After adding crumb rubber in an amount of 10 parts by weight, vulcanizing agents: sulfur and sulfenamide M., grade A, 1 part by weight each, the mixture is vulcanized at T = 150 ^o With constant stirring for 60 minutes The resulting mastic is poured into cans or boxes of thin tin with a release coating of 25-100 kg. The characteristics of the mastic are presented in table 2. The obtained composite mastic according to this method is used for waterproofing underground trunk pipelines, oil fields, etc.

 Example 2

Rubber SKEPT - 5 wt.h
Ligroin K-6 fr. 100/200 - 20 parts by weight
M-100 fuel oil - 30 wt.h
The crushed SKEPT (fr. 5-30 mm) is mixed and dissolved in fuel oil with ligroin at T = 90 ^o C. The resulting is added to 70 wt.h. bitumen BND 90/130 and oxidized by blowing air at T = 180 ^o C to the required softening temperature (T according to KiSh). Then add rubber crumb 15 wt.h., sulfur 1 wt.h., sulfenamide 1 wt. hours are thoroughly mixed and vulcanized at a temperature of T = 155 ^o C for 50 minutes Then, after vulcanization, a mineral powder is added to the mixture in an amount of 20% by weight of the resulting mastic or 31.25 wt. hours and mix thoroughly. The resulting material is packaged in cans. They are used for sealing interpanel joints of underground structures, local repair of damaged roof surfaces, and manufacturing of heat-resistant roofs. Technical characteristics are presented in table 2.

 Example 3

 Rubber SKEPT - 5 parts by weight

 Ligroin K-6 - 20 parts by weight

 M-100 fuel oil - 30 parts by weight

Rubber, solvent K-6, fuel oil is mixed and dissolved at T = 90 ^o C, the resulting mass is combined with 75 wt.h. bitumen and 10 parts by weight crumb rubber, blowing air at T = 180 ^o C to achieve the required softening temperature. The resulting mass is vulcanized at T = 155 ^o With sulfur and a vulcanization accelerator, after adding 1.5 wt.h. sulfur and an organic vulcanization accelerator, with active stirring for 60 minutes To the resulting vulcanizable mass add 30 wt.h. mineral powder (screening crushing, FR. 0,074 mm) and mix thoroughly. The finished product is poured into a bitumen truck or in tin boxes or cans. The resultant is used for rolled roofing integumentary materials, for example, roofing felt, hydrostekloizol, etc.

 The ratios of the components included in the production cycle during the production of composite mastics indicated in the examples can vary within the scope of the claims, the specified selection is made empirically in the laboratory, depending on the technological capabilities of the enterprise, the materials used and the purpose of the mastic. The dynamics of the processes is presented in the drawing, which shows the dependence of the degree of preparation depending on the concentration of CLEPT in solution. The higher the concentration of rubber in the solution, the higher the softening temperature can be achieved. Curve 1 corresponds to a solution of rubber in a mixture of organic solvents with a concentration of 20%. Curves 2 and 3, respectively, refer to solutions with a concentration of 15 and 10%. In addition to concentration, oxidation time also affects the degree of preparation. Considering the fact that different bitumens, depending on the source oil, the method of production, the degree of processing, oxidation or compounding, can be very different, then at a particular production the preparation time is specified when receiving experimental batches.

 Table 1 presents the performance of the prototype Bitumpolymer composition (patent 2132857).

 According to the results of the indicators of table 2, we can conclude about the properties and quality of composite mastic.

 The technical characteristics of the mastic allow it to be used in a wide range of climatic zones of Russia, including the northern regions of Siberia and the south of the Krasnodar Territory.

Claims (3)

1. A method of obtaining a composite mastic, comprising combining petroleum bitumen with fuel oil, rubber, rubber and vulcanization in the presence of sulfur and a vulcanization accelerator, characterized in that the composite mastic contains sulfenamide as an vulcanization accelerator, additionally an organic solvent and crumb rubber, the following operations : SKEPT is mixed and dissolved in an organic solvent and fuel oil to a polymer concentration of 25%, injected into bitumen and mixed until smooth, conduct an oxide ix blowing air at 160-200 ° C after which was added crumb rubber, sulfur, sulphenamide and curing the mixture at 145-155 ° C under stirring for 45-60 minutes at the following component ratio, mass parts: Bitumen 70-75 Fuel oil 10-30 Organic Solvent 15-30 Rubber SKEPT 5-15 Sulfur 0.5-1.5 Sulfenamide 0.5-1.5 Rubber crumb 1-25 2. The method according to claim 1, characterized in that the mineral powder is added to the mixture after vulcanization, in an amount up to 20% by weight of the resulting composite mastic. 3. The method according to claim 2, characterized in that the mineral powder is added before vulcanization.

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