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INVENTION
Russian Federation Patent RU2156270
METHOD FOR RECYCLING RUBBER INDUSTRIAL AND ORGANIC
And household waste
Name of the inventor: Platonov VV
The name of the patentee: Limited Liability Company "Scientific and environmental programs"
Address for correspondence: 103051, Moscow, Color Blvd. 19, page 4, Junior automotive school, Sokolov VG
Starting date of the patent: 2000.03.21
The invention relates to methods for processing of rubber and organic industrial and domestic waste and can be used in the petrochemical and chemical industries. Essence: the waste is subjected to thermal catalytic liquefaction at 220-360 ° C and a pressure of 1-3 MPa hydrogen-hydrocarbon solvent in the presence of an initiator - free iodine and / or iodine-containing compounds taken in an amount of 0,01-0,50 mass. % Of the solvent followed by separation of the liquid products and their distillation to afford the desired products. Use of organic and inorganic iodine-containing compounds selected from the group consisting of potassium iodide, titanium, cobalt, nickel, iodide, tretbutiliodid et al., Or mixtures thereof. The alkyl benzene is used as solvent mixture of alkylbenzenes alkilbenzolsoderzhaschie hydrocarbon mixture. Preferably the process is carried out at a weight ratio of waste: solvent ratio of 1: 2 - 4. Holding method helps simplify the process technology, to improve the yield of liquid products of better quality, which may be used as a fuel or chemical feedstock components.
DESCRIPTION OF THE INVENTION
The invention relates to chemical processing of industrial and domestic wastes (rubber, polyethylene, polystyrene, polypropylene, nylon, polyester, polyvinyl chloride, etc.), chemical raw materials and in the motor fuel components which can be used in the petrochemical, organic synthesis and biochemistry , the production of hydro, thermal and acoustic insulation materials, asphalt concrete for road construction, the anode mass for electrothermal industries and other purposes.
The problem of the chemical processing of various industrial and domestic wastes is quite relevant, because of ever-increasing number of waste and, at the same time, the lack of effective methods for their processing to obtain valuable products. Given the complexity of the chemical composition of various organic wastes and rubber materials are the most promising methods for their complex chemical processing to produce fuel oil, high octane components of motor fuels, raw materials for the petrochemical industry, organic and biochemical synthesis, hydro production, thermal and acoustic insulation materials, asphalt concrete for road construction, carbon materials, anode paste for electrothermal and electrochemical industries.
Solving this problem will significantly expand the resource base of hydrocarbons, which, due to a significant reduction in stocks of natural oil, the pace of its exploration, production and further processing, there is an acute shortage in recent years; solve the environmental problem of complex and harmless disposal of rubber and a wide range of industrial and domestic waste; significantly reduce the consumption of hydrocarbons, produced on the basis of oil, lignite and coal, shale oil, natural bitumen.
A method of processing rubber waste - of waste tires, comprising crushing waste rubber tires to 4-0,75 mm, mixing with the oil, heating the mass in the reactor at 65-370 o C for a time sufficient to dissolve the material, catalytic cracking resulting solution in a reactor at a temperature not lower than 450 o C and elevated pressure, discharging product from the reactor and its subsequent distillation to form gaseous products, gasoline fractions, light and heavy oils (US N 4175211, 1976).
Said method is characterized by multistage, complexity of technology related to the necessity of using a specific catalyst and its periodic regeneration using high temperature and pressure to form significant amounts of low molecular weight gaseous products.
A method of obtaining the resin of the rubber waste, comprising heating them at a temperature above 200 o C in a hydrocarbon liquid duration providing conversion rubber viscous oil was the product, and contacting the latter with a catalyst alkirovaniya (H 2 SO 3; S 2 Cl 2) after adding it aliphatic aldehyde or ketone. The resulting resin mixture is introduced into the rubber for tire production (US 3,895,059, 1975).
Said method characterized by multistage, the necessity of using sulfuric acid, sulfur poluhloristoy capable of causing the flow of the condensation reaction, condensation, which complicates the preparation of low molecular weight liquid products. Further, specific area is limited and the use of the obtained product.
A method of processing rubber waste, comprising mixing at a temperature of 290-380 o C rubber waste solution with a concentration of 10-80 wt.% Hydrocarbon oil and low-boiling fractions distilling off. As the hydrocarbon medium used propane deasphalting oil product sludge containing 2.4 -. 5.9% by weight of asphaltenes and a softening point of 34-45 o C. distilled off low-boiling fraction with boiling temperature 230-310 o C is carried out continuously during the entire mixing process (SU 16134555, 1990).
The disadvantages of this method are primarily limitations on the content of asphaltenes in a hydrocarbon medium. This condition is difficult to implement, since the extracted oil in recent years and their products are of high asphaltene content, organic sulfur compounds and tarry therefore necessary to increase the number of cycles of removal of these compounds. Furthermore, this method is characterized by inadequate light fractions in high yield. The total amount of light fractions boiling in the range of t bales. 230 o, is 12.4 - 37.8 wt.%.
A method of processing rubber waste, comprising in their thermal liquefaction at 270-420 o C, a pressure of 6.1 MPa in a hydrocarbon solvent, which is used as the waste production of synthetic rubber, in the presence of a rare earth metal (REM) in the presence or intermetallics rare earth metals, or in the presence of titanium hydride taken in an amount of 0.5 -. 10.0 wt% of the reaction mixture. The method involves thermal liquefaction at a weight ratio of the hydrocarbon solvent and waste 2: 1 - 4: 1. The method is characterized by low capacity factor using hydrogen donor solvent components that require reusing it in the process, continuous separation of the liquid products of thermal liquefaction feedstock, and a pressurizing a reaction vessel (RU N2109770, 1998).
A significant drawback of this method is the use of a hydrocarbon solvent as synthetic rubber wastes which are not always available in the required quantities. Also needed is enough deficient REM intermetallic compounds based on them, calcium hydride, titanium.
The closest in technical essence to the proposed method is a method for recycling rubber and organic industrial and household waste in chemical raw materials and components of motor fuels, conducted similarly to the above, wherein the hydrogen-hydrocarbon solvent is one or a mixture of alkylbenzenes (toluene, xylene, ethyl benzene, diethyl -, and trimethyl tetramethylbenzenes), which are the basis of "raw benzene" - the product of high-temperature coking coals. These hydrocarbons are effective hydrogen donors, are available in large quantities, their use of this technology allows us to solve a technical, environmental and economic problem (RU N 2110535, 1998).
A significant drawback of this method is the use of rare-earth metals, intermetallics neodymium, lanthanum, cerium, aluminum, and and titanium hydride, calcium pertaining to a fairly scarce material, the difficulty of retrieval of technical hydrocarbon mass and vysokosmolistyh heavy hydrocarbon residues, the high pressure in the reaction machine due to the low degree of utilization of hydrogen from the gas phase formed as a result of thermal degradation of organic waste.
The object of the invention to provide a method that allows to abandon deficient REM, intermetallic compounds based on them, titanium hydride, calcium; simplify the technology and reduce the temperature increase process performance while improving explosion and fire safety, environmental cleanliness, increase the output of fractions with a boiling point of 200 o C, characterized by a low content of organic sulfur and unsaturated compounds.
The assigned task is achieved by a method for recycling rubber and organic industrial and household waste in chemical raw materials and components of the motor fuel comprising thermocatalytic liquefaction of waste at elevated temperature and pressure in a hydrocarbon hydrogen-donor solvent followed by separating the liquid product and distillation to give the desired products, which, according to invention, the process is conducted in the presence of an initiator - free iodine and / or iodine-containing compounds taken in an amount of 0.01 - 0.50 wt% of solvent, at a temperature of 220 -. 360 o C, a pressure of 1 - 3 MPa.
It is expedient to use organic and inorganic iodinated compounds selected from the group consisting of potassium iodide, titanium, cobalt, nickel, iodide, or mixtures thereof tretbutiliodid. Possible to use other iodine-containing compound.
Preferably, as solvent use alkylbenzene mixture of alkylbenzenes alkilbenzolsoderzhaschie hydrocarbon mixture.
It is advisable to use one alkyl benzene, such as toluene, xylenes, tri- and tetramethylbenzenes, diethylbenzenes, mixtures thereof, alkilbenzolsoderzhaschie hydrocarbon mixture.
Preferably the process is carried out at a weight ratio of waste: solvent ratio of 1: 2 - 4.
The use of iodine and its compounds eliminates the rather scarce REM: lanthanum, dysprosium, cerium, neodymium, intermetallic compounds based on them, titanium hydride, calcium; lower the temperature of the process, improve yield fractions having a boiling point up to 200 o C, to reduce its content of unsaturated, sulfur-, nitrogen- and kislorodsodrzhaschih components lower the pressure in the reaction vessel by a more effective transfer of molecular hydrogen from the gas phase and on the components and hydrogen donor solvent to radical products of thermal degradation of organic waste material; significantly simplify the technology owing to the failure of the recovery stage of REM, intermetallic compounds of titanium and calcium from tar fractions products thermo liquefaction of organic waste, reduce production costs, improve the economic performance of the whole process.
As a source LAB is advisable to use "raw benzene" or some of its components (toluene, xylenes, solvent fraction) obtained by high-temperature coking coals and is a waste of metallurgical coke.
The amounts of "raw benzene" big enough, but the rational application of it is not yet found.
As initiator thermal degradation reactions of organic waste material, improving the efficiency of hydrogen transfer from solvent hydrogen donor component and molecular hydrogen from the gas phase using a free iodine and iodinated compounds. Their use makes thermal catalytic liquefaction process rubber, and a wide variety of industrial and domestic wastes more stable at low operating pressures and lower temperatures; no need for separation of iodine and its compounds from the liquefaction products, as their number is extremely low, they are highly volatile and will go into the gaseous products.
Method is as follows
In the rotating autoclave (2 l) was charged rubber-and other industrial and household organic waste (waste tires, conveyor belts, polyethylene, polystyrene, polypropylene, polyisobutylene, synthetic rubber, polyvinyl chloride, nylon, polyester, enanth etc.). Then added hydrogen donor hydrocarbon solvent such as toluene, o-, p-, m-xylene, ethylbenzene, trimethylbenzene, or mixtures thereof, industrial "crude benzene," free iodine and / or its organic and inorganic compounds in an amount of 0.01 - 0.5 wt. % of solvent.
The process of thermo-catalytic liquefaction of waste is carried out at a temperature of 220-360 o C and a pressure of 1-3 MPa; waste weight ratio: solvent 1: 2 - 4. The elemental iodine or compounds thereof initially undergo homolytic cleavage to form an iodo radical. Last cleaves atomic hydrogen from hydrogen-hydrocarbon solvent component and transfers it to the radical products of the thermal degradation of the organic waste material. This explains the high speed past the liquefaction process, the low temperature and pressure, a high degree of hydrogen use, the solvent and the gas phase components, a low content of oxygen, nitrogen and oxygen, but also unsaturated compounds in liquid products produced, higher yield of the latter; increasing the selectivity of isomerization reactions, dehydrocyclization, dehydrogenation, hydrogenation, hydrodealkylation hydrogenation heterocycles and their subsequent destruction, responsible for the formation of significant amounts of cycloalkanes, isoalkanes, hydroaromatic and aromatic hydrocarbons with a high octane; decrease in the content in liquid products oxygen-, nitrogen- and sulfur-containing, and and unsaturated compounds. The liquid products are separated from the solids (metal cord, carbon black, etc.), and then subjected to distillation to give the desired product fractions with a boiling point of 200 o C or above 200 o C.
Embodiments of the method are given in the table. Example Description (N in Table 7) in a rotating autoclave (2 L) charged with 150 g of waste (Recycled Tire, polyethylene, polystyrene, polyisobutylene, synthetic rubber and others.), 450 g of toluene, 0.45 g of the free iodine and / or its inorganic and organic compounds (potassium iodide, titanium, cobalt, iodide, tretbutiliodid et al.) The process is carried out at a working temperature of 360 o C, a pressure of 3.0 MPa for 30 minutes. Liquid yield of 90 wt.% Of the waste, the content of fractions with a boiling point of 200 o C is 95% of the liquid products.
The resulting fractions may be used as a motor fuel and chemical raw material components for the petrochemical, organic and biochemical synthesis.
The table shows that the use of iodine and its compounds allows to increase the yield of liquid products and their content in the composition of the fraction with a boiling point up to 200 o C, enriched isoalkanes, tsiklolalkanami, hydroaromatic and aromatic hydrocarbons, lower the temperature, pressure, reduce the process time.
CLAIM
1. A method for recycling rubber and organic industrial and household waste in chemical raw materials and components of motor fuels, comprising thermocatalytic liquefaction of waste at elevated temperature and pressure in a hydrogen-hydrocarbon solvent, followed by separation of the liquid products and their distillation to give the desired products, wherein the process carried out in the presence of an initiator - free iodine and / or iodine-containing compounds taken in an amount of 0.01 - 0.50 wt% of solvent, at a temperature of 220 -. 360 o C and a pressure of 1 - 3 MPa.
2. A method according to claim 1, characterized in that the iodine-containing organic and inorganic compounds selected from the group consisting of potassium iodide, titanium, cobalt, nickel, iodide, or mixtures thereof tretbutiliodid.
3. The method of claim. 1 and 2, characterized in that the alkylbenzene is used as a solvent mixture of alkylbenzenes alkilbenzolsoderzhaschie hydrocarbon mixture.
4. A method according to claims 1 - 3, characterized in that the process is carried out at a weight ratio of waste: solvent of 1 - 2 - 4.
print version
Publication date 16.01.2007gg
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