Method of processing rubber granulates for producing semi-active carbonised substance and plasticiser

FIELD: chemistry.

SUBSTANCE: invention relates to chemical industry. The method comprises the following steps: performing pyrolysis of rubber granulates at 400-500°C in the presence of liquid water to obtain a carbonised substance and a gas phase and then collecting the carbonised substance.

EFFECT: invention enables to obtain pyrolysis products of good quality and direct use.

5 cl, 3 dwg, 6 tbl, 2 ex

 

The present invention relates to a method of processing rubber granulates, in particular, obtained by crushing waste tires for the production of hydrocarbon and possibly a plasticizer that can be used in mixtures intended for the manufacture of rubber products.

In the rubber industry receive large amounts of waste production and operation. The final shape and operating parameters of products received during the irreversible process of vulcanization. Therefore recycling of rubber products requires the implementation of expensive operations associated with time-consuming and labor resources.

Usually recyclable materials have low physical and mechanical properties and can't compete against the feedstock for the production of rubber. For this reason, rubber waste is a serious problem from the viewpoint of both the economy and the environment.

The scale of this problem can be evaluated from the production of rubber, which reach approximately 35 million tons per year. Now 150 years attempts have been made to the recycling of rubber waste. But until today the development of appropriate technologies for their destruction remains a big problem in the production of rubber. From the point of view of environmental protection recycling �Jn is important since they make up 60-70% of total production of rubber products.

Worn tires can be burned (for example, in cement factories, pulp and paper mills, industrial boilers). They can also be crushed mechanically to obtain waste rubber, textiles and scrap metal. Among them, rubber waste, depending on their grain-size is called a powder or granulate, wherein the powder has an average size of less than 2 mm, and the granules have an average size of from 2 to 10 mm. Rubber granulate can be used in particular for floors in sports facilities, sound insulation, etc. the Powder can be used in road pavement construction, insulating concrete, etc. Advantage of rubber granule is the high content of rubber (depending on spec, for example, 98%). The use of rubber granulate is of particular interest given its low selling price, besides, he does not yet have a high demand in the market.

Pyrolysis of tyres is one of the methods developed for processing of waste tires. The pyrolysis products are, on the one hand, high-temperature gases (in excess of 600ºC), which is typically burned to generate energy, and, on the other hand, a solid residue with a high carbon content, which is either taken to a landfill, or used in cachestorage.

In some recently developed processes part of the pyrolysis gases are condensed to obtain pyrolytic oils that can be used as a fuel or blended with gasoline. However, the solid residue is often contaminated components (textiles, metal, sand, mineral fillers, rubber), which reduces its value and reduces the profitability of the process.

Pyrolysis of rubber is carried out at high temperatures, usually much exceeding 500º, as described in documents US 4588477 or BE 820012. Pyrolysis at a lower pressure reduces the temperature of pyrolysis, as described, for example, in US 2003/0079664 or US 5229099. However, these methods of pyrolysis of rubber does not allow to obtain a solid residue that can be immediately used. Indeed, the obtained solid residue has the characteristics of inactive coal, which does not have sufficient reinforcing ability when used as an additive in rubber mixtures.

There are ways pyrolysis, carried out with the use of rubber granulates in the feedstock. So, in the international application WO 02/38658 described method for processing pellets tires through pyrolysis in the temperature range from 400 to 950º, preferably from 500 to 750º. However, although in the described method and used rubber granules, WO'658 �e clarified the pyrolysis is carried out in the presence of water. Thus, the solid residue, disclosed in WO 02/38658, cannot be considered as suitable for direct use in the rubber industry.

The inventors unexpectedly found that, if the pyrolysis of rubber granulates to carry out in the special conditions, in particular at low temperature and in the presence of water, all the products of pyrolysis can be used directly as raw materials, in particular, in the rubber industry.

To the knowledge of the inventors, only in the international application WO 2003/91359 mentioned the use as a raw material of the solid residue obtained by pyrolysis. This solid residue can be used as an inactive component mixtures for the manufacture of rubber products. However, in the method of use of pyrolysis waste tires, and therefore its products are not of interest from the standpoint of use as a raw material, obtained as a solid residue does not possess sufficient purity for use in the rubber industry without pre-treatment.

The invention is primarily intended to provide a method for recycling rubber granules.

Thus, the first object of the present invention is a method for processing of rubber granulates in the hydrocarbon, containing the following steps:

(a) carry out pirol�W rubber granulates at a temperature of from 400 to 500º, adding during pyrolysis liquid water, to thereby produce a hydrocarbon and a gas phase,

(b) collecting the hydrocarbon obtained in step (a).

Preferably the method allows to recycle rubber granules into products that can be used directly as raw material. Under the "direct use" it should be understood that for use of the products obtained by implementing the method in accordance with the present invention, requires no cleaning (in addition to clearing referred to in the present application, namely, separation from the gas phase).

The term "pyrolysis" is used in its most classical meaning, i.e. it refers to the chemical decomposition of rubber granules under the action of heat in the atmosphere with low oxygen content. In practice, during pyrolysis minimize the addition of oxygen, air or any gas containing oxygen. However, pyrolysis is not necessarily carried out in an inert atmosphere (e.g. nitrogen, argon). Just enough to limit or prevent the ingress of air during the pyrolysis to limit the supply of oxygen.

Under "rubber granules" as a rule, you know the rubber fragments ranging in size from 2 mm to 10 mm, in particular from 3 mm to 9 mm, preferably from 4 mm to 8 mm and a purity of the tire, usually in quantities larger�ing 95%, preferably greater than 98%. In particular, the rubber granulate used in the framework of the invention, does not contain iron particles. Typically, the rubber granulate is obtained after grinding tires, rubber conveyor belts and rubber products.

Method in accordance with the present invention is carried out with the addition of liquid water during pyrolysis. Thus, the method differs from known methods in which a heat carrier during pyrolysis is heated water vapor. Water is added to the pyrolysis chamber in liquid form at a temperature less than 100ºC. Because during the pyrolysis temperature is in the range from 400 to 500º, water turns during pyrolysis in steam, wherein said steam is one of the components of the gas phase. The conversion of liquid water to water vapor requires heat energy consumption. In the framework of the invention water is added not in order to provide the heat required for pyrolysis.

The inventors unexpectedly found that the addition of liquid water during pyrolysis allows to obtain products of pyrolysis (hydrocarbon, heavy oil) best quality and direct use. In particular, the method allows to obtain a hydrocarbon with the desired properties, in particular having reinforcing ability, which allows its use as� additives in rubber mixtures in particular, in the preparation of the fallopian mixtures in the rubber industry.

Without going into private theoretical arguments, you can specify that the addition of liquid water during pyrolysis allows you to:

- cooling of the hydrocarbon in the bottom of the pyrolysis chamber, which, in all probability, allows to obtain a good quality hydrocarbon ("quenching" reaction),

- to carry out the pyrolysis at a temperature below 500º that, in all probability, allows to obtain a hydrocarbon of good quality and use less energy (economic profit),

- improve the removal of pyrolysis gases and vapors outside of the reaction medium. In particular, water is usually injected in the lower part of the pyrolysis chamber, evaporates immediately and is mixed with the pyrolysis gases, which prevents the formation of clusters of rubber granulates, "stick" to the top of the pyrolysis chamber due to turbulence.

Preferably in the above-described method, the weight content of water relative to the weight of rubber granules in step (a) varies from 5% to 20%, in particular from 7% to 17%, preferably from 10% to 15%.

The pyrolysis in step a) is carried out at a temperature from 400 to 500º, in particular, from 425º to 495º and preferably from 450 to 480º.

Preferably, the method of processing of rubber granulates in accordance with the present invent�training is carried out in continuous mode.

Preferably, the method of processing of rubber granulates in accordance with the present invention and, in particular, step a) is carried out at atmospheric pressure, i.e., without decreasing or increasing the pressure.

For the implementation of the pyrolysis in step (a) is not necessary to add additives, such as catalyst and/or an organic solvent. However, such variants are also excluded. In particular, rubber granulates can contain minor amounts of materials in the form of traces (e.g., pollutants) that are in the technique of simultaneously considered catalysts. According to a preferred embodiment, only components introduced into the environment, are the rubber granulates and water. This embodiment yields a hydrocarbon, intended in particular for use as a reinforcing filler in rubber compounds.

In an embodiment of the above method of processing the rubber granulates is carried out in a cyclic mode, in which all or part of the water present in the gas phase in step (a), produced water is separated and reused in step (a).

The advantage of this embodiment is the possibility of recycling water. In practice, during the pyrolysis of the water is added in liquid form. The water evaporates and is one to�of mponents gas phase, the resulting pyrolysis. While the water is separated from the other components of the gas phase for recycling to a pyrolysis chamber.

A second object of the present invention is also a hydrocarbon, obtained by the above-described method of processing rubber granules.

This hydrocarbon has special characteristics and is therefore identified as another object of the invention. This hydrocarbon contains:

- semi-active carbon black,

- one or more metal oxides containing titanium dioxide or zinc oxide, and

- sulphur.

In particular, hydrocarbon in accordance with the present invention and contains mainly represents:

- semi-active soot produced during pyrolysis,

- one or more metal oxides containing titanium dioxide or zinc oxide, are used as curing catalysts, and

- sulphur resulting from the decomposition of the disulfide bridges of rubber. Typically, hydrocarbon according to the present invention contains:

- 80-95%, usually about 90% of semi-active carbon black,

- 4-8%, usually about 6% titanium dioxide and/or zinc oxide, and

- 0.5 to 3%, usually 1-2,8% sulfur.

The value of the content expressed in mass % relative to the total mass of the hydrocarbon.

Typically, hydrocarbon in accordance with this ISO�the acquisition is characterized by a high content of ashes, components, in particular from 8 to 16%, preferably about 12%. "Ashes" means the residue obtained from the combustion of hydrocarbon (which basically leads to the removal of carbon and sulphur). Usually these ashes consist of metal oxides. About half of these evils are titanium dioxide and/or zinc oxide.

Carbon black is an amorphous carbonaceous material that has the appearance of beads and clusters of these balls, size of balls, usually ranges from 10 to 250 nm.

Soot present within the hydrocarbon, obtained by the method in accordance with the present invention is "semi-active" soot corresponding to the norm ASTM D 1765-00, in particular, taking into account its specific surface area. By "hydrocarbon containing semi-active carbon black", or "semi-active hydrocarbon" is understood as the hydrocarbon, which when injected into the rubber compound before vulcanization behaves as a semi-active carbon black in accordance with ASTM D1765-00.

Typically, hydrocarbon in accordance with the present invention has a specific surface area of from 25 to 40 m2/g.

Hydrocarbon in accordance with the present invention can be used directly in the technological production scheme, in particular as a reinforcing filler for the manufacture of rubber compounds.

Carbonizate in soo�cordance with the present invention also contains titanium dioxide and/or zinc oxide. Indeed, the entire titanium dioxide and/or zinc oxide, which was in the original rubber granulates is in the hydrocarbon, the resulting pyrolysis reaction. Titanium dioxide and/or zinc oxide is(are) a curing catalyst, which was used for the vulcanization of rubber, which is part of the granulates. Since the oxide is ZnO and/or TiO2are accelerators of vulcanization, most often used during receiving of rubber compounds, when the hydrocarbon according to the present invention is used as a reinforcing filler in the manufacture of rubber compounds, there is no need to add more zinc oxide and/or titanium dioxide, which is an advantage not only from the standpoint of ease of use, but also because these compounds are expensive.

In addition, hydrocarbon according to the present invention contains sulfur. Sulfur is of interest for vulcanization of rubber products. Indeed, sulfur allows crosslinking between the macromolecular chains of the elastomer.

Therefore, hydrocarbon in accordance with the present invention is of particular interest for use as a reinforcing filler in the preparation of rubber mixtures.

By "reinforcing the floor�the RER" is understood as the filler, which when added to the mixture after vulcanization allows the mixture to obtain a vulcanizate with high mechanical strength and, in particular, with higher tensile strength and higher abrasion resistance.

In an embodiment according to the first object, a method of processing rubber granulates in the hydrocarbon is carried out with the possibility of subsequent use of the gas phase obtained during pyrolysis. In this embodiment, the method further comprises the following steps:

(c) is isolated by distillation of the connection of the gas phase obtained in step a) that have a boiling point above 300 º C, which receive the liquid composition, called heavy oil,

(d) collecting heavy oil obtained in stage C). In the private embodiment, which is used most frequently (in particular, for practical reasons), the method contains the following steps:

(c) is isolated by distillation of the connection of the gas phase obtained in step a), in the form of three fractions, namely

- compounds that have a boiling point above 300 º C, which receive the first liquid composition, called heavy oil,

- compounds that have a boiling point above ambient temperature but below 300 º C, which receive a second liquid composition, called light m�scrapping,

- compounds that have a boiling point below ambient temperature, thereby receiving gaseous composition, called enriched gas

(d) collecting heavy oil obtained in stage C),

e) if necessary, collect the enriched gas and light oil obtained in stage (C).

In these embodiments preferably get both used in further hydrocarbon and used in further heavy oil.

"Enriched gas" means a mixture, the components of which have a boiling point below ambient temperature and which mainly contains the following components: methane, butane, ethane, ethylene, propylene, hydrocarbons with C4(in particular, C4H8With4N10), hydrogen, nitrogen, oxygen, carbon monoxide and carbon dioxide and water, the content of which varies depending on operating conditions.

"Light oil" means a liquid composition, which is obtained from gas-phase components which have a boiling point below about 300ºC.

"Heavy oil" means a liquid composition, which is obtained from gas-phase components which have a boiling point above about 300ºC.

By "ambient temperature" means temperature, usually component from 5 to 35 ° C, in particular from 15 to 25º.

Becom�PTO method in accordance with the present invention is the ability to get the products, which can be directly used as raw materials, in particular, in the rubber industry.

Enriched gas and light oil can be collected. If necessary, they can be incinerated to produce heat energy, for example, to heat the pyrolysis chamber, used for the implementation of pyrolysis.

A third object of the present invention is also heavy oil, which can be obtained through the above-mentioned method.

Preferably, the heavy oil has a high flash point, usually exceeding 210º, for example, component 210 to 300 º C (according to the norm ISO 2592), and one or more of the preferred characteristics specified in the following table.

Table 1
Typical properties of heavy oils
PropertiesThe intervals of values
Density at a temperature of 15 ° C, kg/m3700-1100, preferably 800-1000
Sulfur content, %Of 0.7 to 1.5, preferably 0.9 to 1.1
The chlorine content, %Example, 0.005-0.1, preferably of 0.01-0.06
0.1 to 0.2, preferably 0,13-0,15
Water content, %2-15, preferably 5-11
The content of emulsion, %1-3, preferably of 2.0-2.5
Flash point, ºC30-50, preferably 34-40
Kinematic viscosity at 40 ° C, mm2/s7-13, preferably 9-11
Acid number, mg KOH/g3-6, preferably 4-5
Combustion residues, %Of 0.01-0.05, preferably 0,02-0,04
The remains of charring, %1-3, preferably of 1.9 to 2.1

Heavy oil obtained by the method in accordance with the present invention, can be used as the plasticizer, in particular, in the manufacture of rubber products. It should be noted that the heavy oil obtained by the method corresponds to the plasticizer with a low content of polycyclic aromatic hydrocarbons (PAHs), which corresponds to the most recent changes in legislation relating to �Anna area.

Plasticizers are used to facilitate the use of mixtures of elastomers when they are received, in particular by improving the viscosity and properties of fluidity. They also improve the mechanical properties of the elastomer after vulcanization.

The fourth object of the invention is a composition comprising:

- the above-described hydrocarbon,

- at least one elastomer,

- it is possible, as described above heavy oil. The invention also concerns a composition containing:

- the above-described hydrocarbon,

- at least one elastomer.

The invention also concerns a composition containing:

- the above-described hydrocarbon,

- at least one elastomer,

as described above heavy oil.

These compositions are of interest for obtaining uterine mixtures in the rubber industry.

"Royal mixture" should be understood a mixture that can be used by itself or as a component of the final composition for the manufacture of rubber products by means of vulcanization.

By "elastomer" should be understood all types of synthetic rubber and natural rubber. Used elastomers are preferably natural rubber extracted from rubber and/or SBR rubber from styrene and butadiene.

As stated above, hydrocarbon according to the present invention contains the CE�, which, as a rule, is present in sufficient quantity to implement the vulcanization of rubber. However, it should be noted that during the pyrolysis of the sulfur originally contained in the rubber granulates, goes in the gas phase in the form of various volatile organic molecules, and that only a more or less large part of the sulphur remains in the hydrocarbon. In most cases, the hydrocarbon contains enough sulphur for the implementation of vulcanization. In more rare cases, when the content of sulfur obtained is insufficient, it can be increased by adding sulfur, in particular, in the form of a purified powder directly before vulcanization.

Preferably in masterbatches with the use of hydrocarbon according to known technology is added stearic acid, which serves as a vulcanization activator. You can also add sulfur and/or zinc oxide or titanium dioxide.

In a preferred embodiment of the composition type of masterbatches in accordance with the present invention includes;

- from 50 to 150 parts by weight of hydrocarbon,

- from 80 to 120 parts by weight of at least one elastomer, and

probably from 25 to 75 parts by weight of heavy oil. In an even more preferred embodiment of the composition type of masterbatches in accordance with the present invention with�holds:

- from 50 to 150 parts by weight of hydrocarbon,

about 100 parts by weight of at least one elastomer. In another preferred embodiment of the composition type of masterbatches in accordance with the present invention contains:

- from 50 to 150 parts by weight of hydrocarbon,

about 100 parts by weight of at least one elastomer, and

- from 25 to 75 parts by weight of heavy oil.

The elastomer may be, for example, elastomer type SBR series 1500 or 1700 series.

The invention also relates to the use of the above-mentioned hydrocarbon, the above heavy oil or the above composition to obtain a master batch.

The fifth object of the present invention are installed, made with recycled rubber granulates in the hydrocarbon using the methods described above.

The invention relates to a unit for processing of rubber granulates in the hydrocarbon containing pyrolysis chamber equipped with heating means that can heat the chamber to a temperature of 400-500º, and contains:

- the first entrance, equipped with means for supplying rubber granules,

- second entrance, equipped with means of supplying water in liquid state, which is mentioned after the first login,

- the first output, equipped with means for removing solid products p�of rolisa, associated with the means of collecting the solid products of pyrolysis, and

- the second output is equipped with means for removing gas phase obtained during pyrolysis.

"Pyrolysis chamber" should be understood as a closed environment in which pyrolysis occurs. Preferably the pyrolysis chamber is vertical so that the second entrance, equipped with means for supplying water in liquid state, was lower than the first input, equipped with means for supplying rubber granulates. Thus, the rubber granulate is converted, in particular in the hydrocarbon during pyrolysis, and the hydrocarbon is lowered along the reactor to the level of the second inlet of the pyrolysis chamber, where liquid water enters, "quenching" the reaction of pyrolysis.

The pyrolysis chamber is equipped with external heating means. Heat is obtained than from products introduced into the chamber (rubber granules and water).

The pyrolysis chamber is heated by external heating, which allows to reach the pyrolysis temperature. Typically, the pyrolysis chamber contains a Central shaft, which is usually too hot. Preferably the Central shaft equipped with blades for mixing.

In the private embodiment, the heating system external heating occurs at least partially from the combustion of the enriched gas and/or light oil yielding�required by the method in accordance with the present invention.

Preferably, means for feeding rubber granules, which are equipped with the first inlet of the pyrolysis chamber include means of water supply simultaneously with the filing of rubber granulates (input rubber granules "wetted"). Under the "concurrent filing" means submission of rubber granulates together with water. Typically means feeding rubber granules contain tubular portion equipped with an inclined auger which allows to deliver a mixture of water/granulate in the first entry.

Pyrolysis chamber comprises a second inlet, equipped with means of supplying water in liquid state. Typically, the bulk of the water flows through this second entrance.

Thus, water is introduced into the pyrolysis chamber through two entrances: on the one hand, via a first input and concurrent with rubber pellets, which are fed into the pyrolysis chamber in the wet state, on the other hand, via a second input designed specifically for water.

The pyrolysis chamber has no special means for the intake and/or removal of heated water vapor. Indeed, water is introduced into the pyrolysis chamber in liquid form. During pyrolysis the water that is converted to water vapor under the action of heat released in the gas phase, and water vapor is removed, thus, means for removing gas phase.

In an embodiment in�EUcasino install the tool feed rubber granules, which is equipped with the first inlet of the pyrolysis chamber, contain the device pre-mix granules and water, allowing to obtain a preliminary mixture of water and rubber granules, essentially not containing air.

In the private embodiment, in the above setting means feed rubber granules, which are equipped with the first inlet of the pyrolysis chamber, contain the device pre-mix granules and water, allowing to obtain a preliminary mixture containing no air.

The premixing device may be a conical tank that contains rubber granules and water, and the lower end of which is connected to an inclined auger, which feeds into a pyrolysis chamber granulate and water, as shown in Fig.2.

This device preferably prevents the entrance of air and thus oxygen in the pyrolysis chamber, which allows the pyrolysis in an atmosphere with low oxygen content.

In another embodiment, the above setting is made with recycled rubber granulates in carbonizate with simultaneous production of heavy oil and further comprises a distillation column, hydraulically communicating with means for removing gas phase, wherein said distillation column is designed�ena with the possibility of separation from the gas phase compounds which have a boiling point below 300 º C, and the said distillation column contains an output that is equipped with means of collection mentioned heavy oil.

In this embodiment, the effluent from the pyrolysis chamber the gas phase is sent to distillation column.

Thus, the distillation column allows the separation of heavy oil from the other components of the gas phase.

In a preferred embodiment, the distillation column is made with the possibility of selection:

connections mentioned gas phase, which have a boiling point above 300º, which receive the first liquid composition, called heavy oil,

connections mentioned gas phase, which have a boiling point above ambient temperature and below 300º, thereby getting the second liquid composition, called light oil,

connections mentioned gas phase, which have a boiling point below ambient temperature, thereby getting gas composition, called enriched gas, and the said distillation column comprises a first output, equipped with means of collection mentioned heavy oil, the second output, equipped with means of collection mentioned light oil, and the third exit, equipped with means of collection mentioned enriched gas.

In ecomarine perform distillation column allows the separation of the components from the gas phase and has three phases: enriched gas in the head part of the column, light oil in the middle column and heavy oil at the bottom of the column. To use enriched gas, light oil and heavy oil can be stored in storage tanks.

In a preferred embodiment, the plant comprises a water cooler, hydraulically communicating with enriched gas, wherein said water cooler being configured to separate water from other components of the enriched gas.

In a more preferred embodiment, the apparatus further includes a means of collecting water in liquid form and means of re-supplying the collected water in the pyrolysis chamber.

This embodiment provides recycle of water. Thus, water enters the pyrolysis chamber in which it is converted into steam. This steam leaves the reactor together with the gaseous phase. After separation of the gas phase in the distillation column water vapor is a component of the enriched gas. Water cooler allows you to condense water and separating the water from the other components of the enriched gas. When this water is returned to the pyrolysis chamber through a water recirculator.

Under the "distillation column" should be understood separator installation, which allows you to isolate the components contained in the gas phase, by distillation.

The advantage of the installation according to the�AI with the present invention is its energy self-sufficiency, that is, it allows you to produce at least as much energy as is required to supply (in particular for heating the pyrolysis chamber).

Other features and embodiments of the invention presented below with reference to the accompanying drawings, in which:

Fig.1 and 2 - view of the apparatus in accordance with the present invention.

Fig.3 is a sectional view of the device used to implement the examples below.

Fig.1 shows an installation containing:

- pyrolysis chamber 10 is equipped with means 20 external heating and containing:

the first inlet 30 is equipped with means 40 feed rubber granules,

- a second input 50 is equipped with means 60 of water in the liquid state, which is mentioned after the first login,

- the first output 70, equipped with 80 removal of solid products of pyrolysis, associated with means 90 collection of solid pyrolysis products, and

- the second output 100 is equipped with means 110 removal of the gas phase obtained during pyrolysis.

Means 20 allow external heating heating chamber 10 to a temperature of 400-500º.

The moistened granules come in via the first input 30 of the chamber, and the water enters through the second inlet 50 of the camera. A second input 50, equipped with means for supplying water is after (below) the first WMOs�and 30, equipped with means for supplying granules. Rubber granules are subjected to a pyrolysis reaction and is converted to hydrocarbon, moving down the camera. The pyrolysis reaction "extinguished" liquid water flowing through the second entrance.

Pyrolysis occurs in the pyrolysis chamber.

The gas phase generated during the pyrolysis are removed via a second outlet 90, and solid products (hydrocarbon) is removed from the chamber via the first output 70, and they fall in funds 90 collection of solid products of pyrolysis, for example, in the storage tanks solid pyrolysis products.

Fig.2 shows (in cross section) installation, comprising a pyrolysis chamber 10 is equipped with means 20 external heating, which contains:

the first inlet 30 is equipped with means 40 feed rubber granules and containing;

- tubular portion 120 containing an inclined auger 130, and

device 140 pre-mix granules and water, in particular, conical tank 150, the lower end of which is connected to the tubular part 120,

- a second input 50 is equipped with means 60 of water in the liquid state, which is mentioned after the first login,

- the first output 70, equipped with 80 removal of solid products of pyrolysis, associated with means 90 collection of solid pyrolysis products, and

- the second output 100 is equipped with means 110�Alenia gas phase, produced during pyrolysis,

- the Central shaft 160, equipped with mixing blades 170.

The tubular portion 120 containing an inclined auger 130, sends the mixture of water/granules to a first input 30.

The device 140 pre-mix granules and water contains rubber granules and water and allows to obtain a preliminary mixture of water and rubber granules, essentially not containing air.

Fig.3 shows (in cross section) set containing:

- tank storage 180 connected to the pyrolysis chamber 10,

- pyrolysis chamber 10 is equipped with means 20 external heating, which contains:

the first inlet 30 is equipped with means 40 feed rubber granules,

- a second input 50 is equipped with means 60 of water in the liquid state, which is mentioned after the first login,

- the first output 70, equipped with 80 removal of solid products of pyrolysis, associated with means 90 collection of solid pyrolysis products, and

- the second output 100 is equipped with means 110 removal of the gas phase during the pyrolysis

- distillation column 190, hydraulically communicating with the means 110 removal of the gas phase during the pyrolysis of rubber granulates, on the second output 100 of the pyrolysis chamber, wherein said distillation column 190 ODS�RIT:

- first 200, equipped with 210-collection of heavy oils, in particular, the storage tanks of heavy oil,

- the second output 220, equipped with 230 collection of light oil, in particular, the reservoir storage of light oil

- the third exit 240,

- means of collecting water in liquid form, in particular:

- water cooler 250, hydraulically communicating with the head part of the distillation column 190 through the third opening 240 and equipped with means 260 collection enriched gas, in particular, the reservoir storage of enriched gas,

- water recirculator 270, and

- means 280 re-submission of the collected water in the pyrolysis chamber.

Tank storage 180 contains rubber granules and water.

Water cooler cools 250-enriched gas coming from the head portion of the distillation column 190.

Distillation column 190 separates the connection of the gas phase obtained in the pyrolysis of three phases:

connection mentioned gas phase, which have a boiling point above 300º, which receive the first liquid composition, called heavy oil, wherein said heavy oil is removed from the distillation column via the first output 200,

connection mentioned gas phase, which have a boiling point above ambient temperature and below 300º, by che�about getting a second liquid composition, called light oil, wherein said light oil is removed from the distillation column via the second output 220,

connection mentioned gas phase, which have a boiling point below ambient temperature, thereby getting gas composition, called enriched gas, and this enriched gas is removed from the distillation column through the third opening 240.

Water recirculator 270 returns water enriched gas in the pyrolysis chamber 10.

EXAMPLES

EXAMPLE 1

2 kg/h of rubber granules (granules size 1,0-4,0 mm (% textiles: ≤1,5% sand: 1% - metal ≤0,1%) - ABC RECYCLING®) and 0.25 liters of water per hour is introduced into the pyrolysis chamber heated to 495º. Collect 0.8 kg of hydrocarbon per hour. The gas phase formed during pyrolysis is separated into enriched gas (0.3 kg/h), heavy oil (0,5 kg/h) and light oil (0.4 kg/h).

Table 2 presents the characteristics of the semi-active hydrocarbon in comparison with the characteristics of carbon black N-330®, characterized by norm ASTM to make it as a semi-active carbon black.

Table 2
Comparison of carbon black N-330® and the obtained hydrocarbon
TESTS SOOTNORM N-330®Semi-active hydrocarbon
Indicator of iodine (g/kg)ASTM D 151082,6105,7
Absorption (dibutyl phthalate DBP) (cm3/100 g)ASTM D 2414Of 101.7-
Adsorption (setitimer ammonium bromide BECOMING), (m2/g)ASTM D 376584,7
Ink capacity, (%)ASTM D 3265102,159,2
Mass loss during drying at 125°C (%)ASTMD15090,150,75
Ash content, (%)ASTMD15060,3112,0
Sulphur content (%)ASTMD16190,392,43

It is noted that the obtained hydrocarbon characterized by a high content of substances that can be reused.

Carbonizate in with�according to the present invention contains a large amount of ash: 12%, almost half of which consists of zinc oxide (ZnO) (table 3). Hydrocarbon in accordance with the present invention also contains a significant amount of sulfur.

Table 3
The composition of the ash obtained from the combustion of hydrocarbon in accordance with the present invention
ComponentContent (%)
Na2O0,486602
Li2O0,001213
K2O0,175399
ZnO49,61224
Fe2O31,34167
AS2O30,00225
CrO30,032389
CdO0,000218
PbO0,022657
CoO0,182031
NiO0,009114
CuO 0,088711
HgO6,55 E -05
SiO229,9
CaO6,124958
MgO4,129356
Al2O32,886896

Table 4 shows the specifications of two shipments of heavy oil obtained by the method in accordance with the present invention.

Table 4
Technical characteristics of two shipments of heavy oil, obtained by the claimed method
No.FeatureTest 1Test 2
1.Density at a temperature of 15 ° C, kg/m3917,2920.5
2.Sulfur content, %1,361,73
3.Kinematic Vascos�ü at 40 ° C, mm2/s (measured using a glass capillary viscometer)63,8 (80ºC)29,6 (90 ° C)
4.The solidification temperature, ºC1028

EXAMPLE 2

Hydrocarbon, obtained in example 1 was used as a reinforcing filler for the preparation of rubber mixtures. In particular, in a mixture of 50% carbon black N-330®, classically used by manufacturers of rubber as a reinforcing filler, replaced by hydrocarbon.

For comparison, table 5 presents the composition of mixtures 1 and 2, when the mixture of 1 (control) contains as reinforcing filler 100% carbon black N-330®, and a mixture of 2 contains as reinforcing filler 50% carbon black N-330® / 50% of the hydrocarbon in example 1.

Table 5
The composition of mixtures 1 and 2
RAW materialsA mixture of 1A mixture of 2
Synthetic rubber (KER®N-9 from Synthos Dwory®)53,153,1
Synthetic rubber (KER®8512 from Synthos Dwory®) 7,77,7
Carbon black N-330® (Bvdgovskie zakłady Przemyslu Gumovego
"STOMIL" S. A.)
22,411,2
Carbon black No. 539® (Bvdeovskie zakłady Przemyslu Gumovego "STOMIL" S. A.)4,44,4
Hydrocarbon example 1-11,2
Zinc oxide (zinc white)3,12,4
Stearic acid0,80,8
Accelerator TMTD (disulfide tetramethyl thiuram)0,10,1
Accelerator CBS (n-cyclohexyl-2-benzothiazol a sulfonamide)1.31,3
Powdered sulfur0,70,7
Rosin0,40,4
Oil Nytex® (plasticizer)66
Kaolin- 0,7

Table 6 presents the physical and chemical properties of rubber mixtures obtained after vulcanization.

Table 6.
Results of physical and mechanical testing of mixtures 1 (control) and 2
The type of testA mixture of 1 (control)A mixture of 2
Hardness (+-5)[ºSh] (measured by the tester, dynamic hardness shore A ASTM D 2240)7067
Specific gravity (ton/m) or density1,101,11
Abrasion (mm3) (by norm111124
NFT 46 012 under load 1st Dan
The tear resistance (kN/m) (notched corner samples) (norm NF T 46-007)10,711.3
Tensile strength (MPa) (according to the norm NF T46002) (modulus 300%)19,420,5
Elongation (relative to the original length of the sample) or deformation at rupture (%)547700

The rubber mixture, containing 50% carbon black N-330® and 50% of the hydrocarbon as a reinforcing filler, has properties similar to rubber mixtures obtained from uterine mixture containing 100% carbon black N-330®. Replacement of all or part of carbon black N-330® hydrocarbon of interest from an economic point of view as carbon black N-330® is an expensive product.

1. Method of processing rubber granules with average size of 2 to 10 mm, in hydrocarbon, containing the following stages:
(a) carry out the pyrolysis of rubber granulates at a temperature of from 400 to 500°C, adding during the pyrolysis of liquid water, to thereby produce a hydrocarbon and a gas phase,
(b) collecting the hydrocarbon obtained in step (a).

2. A method according to claim 1, wherein stage a) is carried out at atmospheric pressure.

3. A method according to claim 1 or 2, further comprising the following steps:
(c) is isolated by distillation of the connection of the gas phase obtained in step a) that have a boiling point above 300°C, whereby liquid composition, called heavy oil,
(d) collecting heavy oil obtained in stage (C).

4. A method according to claim 1 or 2, in which�'om the mass content of water relative to the weight of rubber granules in step (a) ranges from 5% to 20%.

5. A method according to claim 1 or 2, carried out in a cyclic mode, in which all water or part of the water present in the gas phase obtained in step a), produced water is separated and reused in step a).



 

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FIELD: machine building.

SUBSTANCE: device for processing rubber waste comprises a hopper with crushed rubber waste, the loading chamber with the container filled with waste which is moved into the thermolysis reactor and overturned, the thermolysis reactor is designed as a chamber with gas flues for discharge and supply of steam-gas mix, the device is fitted with the branch pipe of supply of gases in the container connected to the steam-gas mix supply flue. Using the fan through the layer of waste in the container and pipes of the heat exchanger the gas medium is pumped over, performing the circulation of the gas medium along the circuit: the layer of waste in the container - thermolysis reactor - heat exchanger - fan, the thermolysis reactor is also fitted with the system of unloading of solid products, the system of unloading of solid products is connected to the screw placed in the cylindrical housing which is installed on an axis of the cylindrical furnace with a possibility of rotation and further is connected to the screw placed in the cylindrical housing with a cooling shirt which is connected to the mill connected to the magnetic separator, from where solid products via the batcher are fed to the mixer which by means of another batcher is connected to the storage of liquid fraction, the mixer is fitted with the ultrasonic dispenser and electrodes connected to the electric impulse generator, mixer-processed mix of solid products of thermolysis of waste in liquid fraction is poured into the vessel, the device contains the mixing heat exchanger which is connected through its inlet to the gas flue for discharge of steam-gas mix from the thermolysis reactor, and below the inlet of steam-gas mix into the mixing heat exchanger the shell-and-tube heat exchanger is installed, the outlet of which is connected to the storage of liquid fraction which is connected to nozzles for dispersion of liquid fraction in the mixing heat exchanger. The branch pipe for discharge of gases from the mixing heat exchanger is connected to the steam-gas mix condenser where hydrocarbons are condensed from gases, and non-condensible gases fed to the torch for burning, the condensed hydrocarbons are poured into the liquid fraction separator for separation into water and light hydrocarbons.

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FIELD: engines and pumps.

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FIELD: chemistry.

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21 cl, 10 dwg, 1 tbl

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FIELD: machine building.

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2 cl, 2 tbl

FIELD: chemistry.

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5 cl, 2 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to method for thermal processing polymer components of worn-out car tyres, involving their loading into a reactor, pyrolysis in a gas medium with subsequent separation of pyrolysis products and unloading the solid residue. Crushed polymer components of worn-out car tyres are treated with an aqueous solution of cobalt chloride in amount of cobalt chloride of 2% of the weight of polymer components and subsequent drying of the treated material at room temperature. Pyrolysis is carried out in a nitrogen medium at atmospheric pressure at 450-460°C for 1.0-1.5 hours.

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3 cl, 1 ex, 2 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to processing rubber-containing wastes, particularly to recycling worn-out tyre casings and industrial rubber articles. The method of processing waste industrial rubber articles involves dissolving rubber crumbs in a naphthalene fraction of coal-tar resin by mixing a mixture of the components in a sealed container at 220-230°C for 15-30 minutes using microwave radiation at frequency of 2450 MHz and power of 450 W, in the following ratio of components of the mixture in wt %: rubber crumbs 10-40, naphthalene fraction of coal-tar resin - the rest.

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2 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to chemical engineering and equipment, particularly for processing solid household and industrial wastes, as well as other carbon-containing feed stocks into fuel gas by gasification and to methods for pyrolysis and downdraft gasification process. The gasification apparatus includes an elongated external reservoir, an elongated internal reservoir, said internal reservoir located inside said external reservoir to form a cavity between said internal reservoir and said external reservoir, a loading mechanism which includes an elongated housing of the loading mechanism and a feed stock feeding device for moving said feed stock along said elongated housing of the loading mechanism, a gas generator housing with an external surface and an internal surface, a combustion chamber, a gas outlet and a slag offloading mechanism.

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27 cl, 34 tbl, 3 dwg

FIELD: chemistry.

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EFFECT: inventions provide the complete recycling of fine fractions of processing products, enable producing high-calorie gas and increasing yield and quality of the finished products.

6 cl, 1 dwg, 2 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: method of thermocatalytic processing of industrial and solid household wastes includes milling wastes and their thermal processing in air medium at 550-750°C and pressure 1.2-2.0 atm, catalytic thermodestruction of gaseous products in presence of transition metals of iron subgroup, characterised by the fact, that catalytic thermodestruction is realised at temperature 500-550°C, weight ratio of catalyst and wastes 0.01-0.05, air consumption 1.5-4.0 m3 per 1 kg of solid raw material, as catalyst transition metals of iron subgroup, applied on artificial zeolite ZSM-5 in quantity 1-15 wt %, are applied.

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5 tbl, 6 ex

FIELD: chemistry.

SUBSTANCE: invention relates to field of application of renewable sources of raw material - biomass. Claimed is method of catalytic gasification of biomass with obtaining gaseous fuels. Method includes milling biomass and its thermal processing in air medium at 600÷800°C and pressure 1.2-2.0 atm, catalytic thermal degradation of gaseous products in presence of transition metals, method differs by the fact that catalytic thermal degradation is realised at temperature 500÷550°C, weight ratio of catalyst and biomass is 0.01÷0.05 and air consumption 1.0÷2.5 m3 per 1 kg of biomass, and as catalyst is applied mixture of oxides of chrome and vanadium, applied on natural aluminosilicate in quantity 1÷20 wt % and 1÷5 wt % respectively, or as catalyst applied is mixture of oxides of molybdenum and manganese, applied on natural aluminosilicate in quantity 1÷10 wt % and 10÷30 wt % respectively, or as catalyst applied is mixture of cobalt and nickel oxides, applied on natural aluminosilicate in quantity 5÷25 wt % and 1÷40 wt % respectively.

EFFECT: increased output of flammable hydrocarbons, achievement of good efficiency of gasification.

6 tbl, 6 ex

FIELD: agriculture.

SUBSTANCE: invention can be used in preparation of enhanced fuel from wastes of poultry farms. The method of processing poultry farm litter comprises granulating the wet raw material in the granulator. The granules obtained are dried in a drying chamber at a temperature of 150°C and heated in the pyrolysis chamber without access of air at a temperature of 550°C in the presence of gaseous coolant with the transfer of the pyrolysis products to the solid product and steam-gases with their subsequent partial condensation into the liquid fuel.

EFFECT: inventions enable to increase the yield of liquid fuel from organic material to 31,6% with a decrease of water content in it to 5%, to increase the calorific value by 15-20%, and to reduce energy consumption per 1 kg of the obtained solid and liquid fuel, to obtain the solid carbon-mineral product with a yield of up to 15%, which can be used as fuel and as fertiliser.

8 cl, 7 dwg, 5 tbl, 1 ex

FIELD: process engineering.

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22 cl, 2 dwg

FIELD: process engineering.

SUBSTANCE: invention relates to chemical industry and can be used in processing of coal shale and peat. Proposed plant comprises bin (1) with fuel and equipped with feeder (2), fuel mixer (3) and solid heat carrier cyclone (4), drum-type pyrolysis reactor (5) with horizontal shaft, dust separation chamber (6) with dust separation cyclone (9). Outlet of cyclone (9) is connected with compartment (10) of fluid condensation from vapour-gas mix. Bottom of dust separation chamber (6) is connected with inlet of flash firebox (8) its outlet being connected via gas-dust flow splitter (11) with cyclone (4), its ash discharge outlet being connected with fuel and solid heat carrier mixer (3). Outlet of flash firebox (8) is connected with ash separator (12), its ash discharge being connected with ash heat exchange (13) while gas pipe being connected to waste-heat boiler (15). Dust separation chamber (6) is furnished with flow splitter plate (17). One part of plate (17) is arranged in outlet pipe (18) of pyrolysis reactor (5) above solid material layer at the angle of its natural slope. Second part of said plate (17) is arranged in dust separation chamber (6) horizontally to cover is cross-section with slot formation.

EFFECT: higher quality of fluids, simplified dust separation and condensation.

2 dwg

FIELD: chemistry.

SUBSTANCE: method of processing lipids and lignins involves exposing a suspension of lignins in liquid or molten lipids to ionising radiation and temperature action at volatilisation temperature of the methoxyphenol fraction. The decomposition products are removed from the exposure area by gaslift with gaseous products of decomposition of the material. Alkanisation of the reaction mixture, use of ultrasound, catalysts or mineral sorbents can be additional controlling factors depending on composition of the starting material.

EFFECT: invention widens the range of natural material for producing fuel, increases output of products for fuel purposes, increases stability of the obtained products and simplifies their fractional separation, and also lowers the processing temperature of the material.

6 cl, 2 tbl, 10 ex

FIELD: process engineering.

SUBSTANCE: invention relates to thermal depolymerisation of natural and secondary organic stock, for example, solid domestic wastes. Proposed method comprises stock loading with preliminary separation and grinding with drying. In differs from know processes in that drying is carried out jointly with catalyst low-cal natural fuel. Then, paste is prepared from ground material and solvent, i.e. distillate obtained in liquid products distillation. Note here that further step depolymerisation of reaction mass is performed at 200-400°C and normal barometric pressure at the cascade of to pairs of series reactors. Whereat depolymerisation temperature reaches 200°C in said first pair and 200-300°C in said second pair combined by circulating flows: gaseous flow forming in said reaction medium a reducing medium in the form of synthesis gas (CO and H2) formed by vapor catalytic conversion of hydrocarbon gases escaping from depolymerisation reactors and displaced by gas pump via heater of reducing gases from reaction system. Synthesis gas is discharged to produce motor fuels, i.e. methanol, dimethyl ether or gasoline. Liquid hydrocarbon phase is separated from solid unreacted components to allow their yield of 40% of total initial mass of solid wastes to be discharged from the system by circulation pumps and directed for production of oil briquettes and/or combustible capsules. Note here that said liquid reaction hydrocarbon mix is directed, after solid residue separation therefrom to hot separation, cooling and distillation. Besides, smaller portion of distillate is retuned to mixer for making paste at appropriate stage. While smaller portion is separated into target fractions: one with boiling point of up to 200°C and second with boiling point above 200°C but not over 310°C.

EFFECT: wasteless, non-polluting and efficient process.

1 cl, 1 dwg, 2 tbl, 2 ex

FIELD: chemistry.

SUBSTANCE: invention relates to investigation of processes of thermal decomposition of solid fuels and can be used in chemical and fuel industry. The method of determining the dependency of output of polyfractional solid fuel semicoking products on heating temperature involves placing the starting fuel in an annular reaction volume between two heat-conducting surfaces; external and internal heating of the solid fuel through the heat-conducting surfaces without access to oxygen to a given final temperature; measuring heating temperature at different points on the cross-section of the annular volume at a different depth; recording the given final heating temperature of the fuel as the average arithmetic value of readings of all heat sensors; heat-insulating the collector; maintaining temperature higher than 200°C in the top part of the reaction volume and keeping final temperature of the process constant until the release of gas stops completely; and removing the formed gaseous products through the collector into a condensation system; insulating the inner volume of the vessel from the condensation system and determining output of semicoking products.

EFFECT: invention increases accuracy of determining output of semicoking products.

3 cl, 6 dwg, 3 ex

FIELD: process engineering.

SUBSTANCE: invention relates to processing of wastes and can be used in chemical and rubber-textile industry for production of rubber mix ingredients from wastes of petrochemical industry wastes, fuel analogs and rubber mix ingredients. Proposed method comprises feeding the wastes into reactor, their thermolysis in the medium of heat carrier forced through the bed of wastes to form gas and fluid phases, discharge of gas phase therefrom, discharge of solid phase from reactor by displacing the container with solid phase from reactor into first chamber, discharge of solid phase and its electromagnetic processing, extraction of liquid phase from gas by cooling, extraction of water from fluid phase, compression of gas phase, process reiteration whereat wastes are fed into reactor in movable container from second chamber to allow displacement of the container from reactor to second chamber after thermolysis termination.

EFFECT: lower power consumption and emissions, higher quality of target products.

1 dwg

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