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INVENTION
Patent of the Russian Federation RU2286998
METHOD OF DISPOSED TIRES RECYCLING
The name of the inventor: Andreykov Evgeny Iosifovich (RU); Amosova Inna Sergeevna (RU); Oleg Chupakhin (RU)
The name of the patent holder: Institution The Institute of Organic Synthesis of the Ural Branch of the Russian Academy of Sciences (RU)
Address for correspondence: 620219, Yekaterinburg, ul. S. Kovalevskaya / Academic, 22/20, IOS of the UrB RAS, Director of Ak. V.N.Charushin
Date of commencement of the patent: 2004.12.24
The invention is intended for utilization of rubber chips obtained from waste tires. Rubber crumb in a mixture with heavy oil residues in a ratio of 10: 90-40: 60 is subjected to thermal oxidation by air at 250-300 ° C or by heat treatment at 280-320 ° C, followed by air oxidation at 230-270 ° C to obtain a modified bituminous Material. The obtained product according to the invention has adhesion to marble and granite of 100%, a reduced temperature dependence of the "penetration" index and can be used as a binder in road construction for insulation works and in other areas.
DESCRIPTION OF THE INVENTION
The invention is intended for utilization of used tires, namely rubber crumb obtained by grinding tires.
The constantly increasing number of used tires creates serious environmental problems. One of the directions of recycling rubber crumb obtained by grinding from worn tires is the production with its use of modified bituminous materials that can be used in road construction, for insulation coatings and in other directions.
It is known to use finely dispersed rubber chips as additives to road bitumen. The essence of the method consists in the introduction of rubber chips into liquid bitumen and effective homogenization of the system at temperatures of 150-250 ° C. [B.G. Pechenyi. Bitumen and bitumen compositions. M., Chemistry. 1990. P.119; Patent RF 2,164,927] .
The drawbacks of the method, which determine the small scale of its use, are the need to use finely dispersed rubber chips having a high cost, but also a strong influence on the properties of the composition of the homogenization regimes and characteristics of the original crumb. In the temperature range 150-250 ° C there are both processes of swelling and plasticization of rubber, and its partial destruction. The ratio of these processes and, consequently, the properties of the final product depend on many factors and are difficult to regulate.
There are known methods for recycling rubber crumbs to produce bituminous materials in which waste rubber is thermally depolymerized in high boiling petroleum products at elevated temperatures up to 454 ° C, in analogy with the coals liquefaction process [US 4,211,576] . In the patent [GB 2024245], thermal dissolution of rubber crumb is carried out at temperatures of 100-500 ° C in oil residues in order to obtain the feedstock for the coking process.
An essential feature of these patents, in common with the features of the present invention, is the heat treatment of rubber crumb in high-boiling products at elevated temperatures, i. E. In conditions under which complete depolymerization and dissolution of the rubber component of the tires in the solvent is ensured.
The drawbacks of these methods include the need to use high temperatures and to obtain a product of tire dissolution in oils, which is an intermediate product for the production of marketable products or by mixing with bitumen [US 4,211,576] or subsequent coking [GB 2024245] .
In order to obtain well-homogenized, storage-stable bituminous materials, treatment of mixtures of heavy oil residues and rubber crumb with air is used. In the method [WO 9520623], a modified bitumen is prepared by treating a mixture of heavy oil residues and rubber crumbs at temperatures not higher than 252 ° C (485 F) by air for 2-8 hours. The air consumption is 45 m 3 / ton of mixture · h, maximum 57 m 3 / ton of mixture · h, the ratio of rubber crumb: solvent is 1-27: 99-63. A rubber crumb with a size of 200-20 mesh can be used, i.e. Not more than 0.83 mm. The process time varies in order to obtain a bitumen product of the required quality, which can be used for road construction or as an insulating material.
Essential features of this method, taken as a prototype, common to the proposed invention are: air treatment of a mixture of oil product and rubber crumb, the use of heavy oil residues as a petroleum product and the production of a commodity bitumen product in the process.
A disadvantage of this method is the need to use in the process fine-dispersed rubber chips obtained from waste tires having a high cost.
OBJECTS OF THE INVENTION
1. Utilization of waste tires by obtaining bitumen products from heavy oil residues and rubber chips, obtained from waste tires, with a particle size of 5-10 mm and more.
2. Production of bituminous materials with adhesion to marble and granite 100%, and with a reduced temperature dependence of the "penetration" index to ensure their greater operational resistance to temperature changes.
The tasks are solved due to the fact that the mixture of oil residue with rubber chips obtained from waste tires with a rubber crumb ratio: the oil residue of 10: 90-40: 60 is treated with air in the temperature range of 250-280 ° C in a single or two-stage process. In a one-stage process, the mixture is treated with air in a temperature range of 250-300 ° C, preferably at 260-270 ° C, for 1-8 hours. In a two-stage process, the mixture is heat treated in the temperature range of 280-320 ° C, preferably at 300-310 ° C, for 0.5-1 hour and then treated with air in the temperature range 230-270 ° C for 1-6 hours .
As shown by the treatment of the product of the process with a solvent, tetrahydrofuran, the complete destruction of the macromolecular three-dimensional rubber structure takes place under the claimed conditions, and the reaction product is a fine suspension of tetrahydrofuran insoluble filler of tire rubber, carbon black and inorganic additives in a homogeneous solvent consisting of the products of joint oxidation of tar and compounds, Obtained during the thermal solvolysis of rubber. The degree of conversion of rubber crumb into soluble products is 65-70% by weight. Carrying out the process under conditions that provide complete thermal dissolution of the rubber component of tire rubber allows us to use cheap large crumb as raw materials (in the examples we used rubber crumbs of 5-10 mm size, we can expect identical results for larger crumbs). The obtained bitumen compositions modified with finely dispersed soot acquire new useful properties due to the structuring effect of the latter, in particular, the bitumens have a lowered temperature dependence of the "penetration" index.
The recommended process conditions are established experimentally, and are determined by the following ideas about the process.
When the mixture of oil residue and rubber crumb is treated with air at a temperature below 250 ° C and heat treatment at a temperature below 280 ° C, there is no complete dissolution of the rubber component of tire rubber, which is a necessary condition for the efficiency of the proposed method.
For a two-stage process, heat treatment at a temperature above 320 ° C leads to an increase in the proportion of low molecular weight rubber degradation products and an increase in losses of organic substances with the exhaust air in the second stage.
The upper limits of air treatment temperatures are determined by the permissible level of entrainment of organic compounds with exhaust air, which at 300 ° C does not exceed 1-2% by weight.
Execution of the process with the content of rubber crumb in the initial mixture below 10% is not effective from the point of view of processing of its large quantities, at a crumb content of more than 40% it is difficult to homogenize the initial mixture and the product of the process contains an increased amount of solid filler rubber, soot, which makes it difficult to directly use in As bituminous material.
The duration of the process or its stages, as well as the air flow, are selected based on the requirements for the characteristics of the resulting bitumen product. The increase in the duration of air treatment and its consumption lead to an increase in the softening temperature and corresponding changes in other characteristics of the product. The recommended air flow rate can be from 80 to 300 m 3 / ton of the mixture per hour (preferably 200-250 m 3 / ton mixture).
Rubber crumbs or rubber pieces obtained from used tires after separating the metal cord, up to 10 mm in size and larger, and heavy oil residues such as tar, asphalt, propane deasphalting asphalt, visbreaking residue and other petroleum products having a high boiling point .
The process is carried out at atmospheric pressure and a mass ratio of rubber crumb: an oil residue of 10: 90-40: 60.
The claimed method is explained by the following examples.
EXAMPLE 1 A mixture of 71 g of tar and 36 g of rubber crumb is treated at 260 ° C. for 1.5 hours with air. The air consumption is 240 l / h · kg.
The product obtained has the following characteristics:
- softening point on the "ring and ball" 43 ° C;
- penetration, 10 -1 mm, 104 at 25 ° C and 52 at 0 ° C;
- the ratio of penetration values at 25 and 0 ° C is 2.0;
- extensibility (5 cm / min) 23 cm at 25 ° C;
- adhesion to granite and marble 100%.
The content of substances insoluble in tetrahydrofuran (exhaustive extraction in the Soxhlet apparatus) was 12.6% by weight.
The conversion of crumb rubber into soluble products is 62.6% by weight.
EXAMPLE 2 A mixture of 73 g of tar and 36 g of rubber crumb is heated with stirring to 300 ° C and held at this temperature for 30 minutes, then treated for 2.5 hours with air at a temperature of 250-260 ° C. The air consumption is 240 l / h · kg.
The product obtained has the following characteristics:
- temperature of softening by "ring and ball" 50 ° C;
- penetration, 10 -1 mm, 48 at 25 ° C and 33 at 0 ° C;
- the ratio of penetration values at 25 and 0 ° C is 1.45;
- extensibility (5 cm / min) 30 cm at 25 ° C;
- adhesion to granite and marble 100%.
The content of substances insoluble in tetrahydrofuran (exhaustive extraction in a Soxhlet apparatus) is 12.3 wt.%.
The conversion of crumb rubber into soluble products is 62.8% by weight.
In the examples, a rubber crumb, not containing a metal cord, measuring 5-10 mm, obtained by grinding the used tires, was used.
Since the feature of the present invention is the complete dissolution of the rubber component of the tires, it is possible to expect positive results when using a larger crumb, which is preferable from an economic point of view.
The initial tar had the following characteristics:
- softening point in the "ring and ball" 34 ° C;
- penetration, 10 -1 mm, 177 at 25 ° C and 68 at 0 ° C;
- the ratio of penetration values at 25 and 0 ° C is 2.6;
- extensibility (5 cm / min) 65 cm at 25 ° C.
By varying the process conditions, especially the processing time, it is possible to obtain bituminous materials with different softening point and other characteristics required for their use as binders in road construction, insulation work and in other areas.
CLAIM
1. A method for utilizing waste tires by heat treatment and air treatment of rubber chips obtained by grinding tires in high boiling oil residues, characterized in that the heat treatment and air treatment are carried out together in a temperature range of 250-300 ° C. at a rubber crumb ratio: 10: 90-40: 60.
2. A method for utilizing waste tires by heat treatment and air treatment of crumb rubber obtained by grinding tires in high boiling oil residues, characterized in that the process is carried out in two stages: the first stage is the heat treatment at 280-320 ° C, the second stage is the treatment Air at 230-270 ° С at a ratio of rubber crumb: oil residue 10: 90-40: 60.
print version
Date of publication 10.12.2006гг
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