JPH09316356A - Method for controlling properties of carbon black and apparatus therefor - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method and apparatus for controlling properties of a carbon black to a homogeneous quality with a required level on a process for producing a carbon black esp. from an org. polymer waste such as waste tires. SOLUTION: In a process for producing a carbon black by thermally decomposing and gasifying an org. polymer material and subjecting the resultant gas to dehydrogenation and polycondensation, the properties of the carbon black produced are controlled by controlling the gas temp. and gas dwell time in both the dehydrogenation and the polycondensation. The gas temp. is varied by adjusting the amt. of an oxidizing agent supplied to the reaction zone, and the gas dwell time, by changing the amt. of quenching water supplied and the position of the quenching water supply in the reaction zone.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to an organic polymer material,
In particular, the present invention relates to a method for controlling the properties of carbon black when producing carbon black from an organic polymer waste such as a waste tire, and an apparatus for carrying out the method.

[0002]

2. Description of the Related Art Generally, carbon black is produced by burning a raw material oil such as creosote oil and ethylene bottom oil, partially gasifying it to generate gas phase carbon, and growing it by a condensation reaction.
It has been carried out by precipitating and quenching to form a liquid phase and a solid phase. On the other hand, the inventors of the present invention recycle waste tires, and as an effective utilization technology, pyrolyze and gasify organic hydrocarbons such as rubber and volima in waste tires, and dehydrogenate them by raising the temperature of this pyrolyzed gas.・ We proposed a technology to stop the reaction by carbonization by condensation reaction and quenching to produce carbon black (Japanese Patent Application No. 6-1
68061, Japanese Patent Application No. 6-298187).

Carbon black properties are generally required to have properties such as particle size (specific surface area), particle structure and surface activity for each purpose of use. Particularly, properties required for reinforcing tires are particle size and particle size. It is a structure, and this property also serves as a quality control standard, and the basics of carbon black property control are reduction of particle size, (increasing specific surface area), and particle structure control.

Generally, the basic operation of this property control is to control the gas temperature and the reaction residence time in the carbon black formation reaction process. For this reason, many inventions relating to the method and apparatus for controlling the gas temperature and the reaction residence time have been proposed in the related art, but basically, the control and reaction of the combustion temperature (air ratio, air introduction method) in the reaction furnace are performed. There are many things related to the position of feeding quenching water for stopping, the method, and the furnace structure for effectively performing these. However, in these methods, the raw material oil is injected into the high temperature field where the fuel oil is burned, pyrolyzed and partially burned, and the pyrolysis gas generation, dehydrogenation and condensation reaction are performed in the reaction furnace, and Since the quenching water is injected to stop the reaction, the control of the reaction gas temperature and the control of the gas retention time until the reaction stop are non-uniform.

For this reason, the required characteristics of the carbon black production furnace are such that the furnace type, the feedstock oil injection hole position and the cooling water injection position are regulated. Therefore, carbon black of different properties can be produced in the same production furnace. It is difficult to manufacture. This is because combustion of fuel oil and thermal decomposition of raw material oil, partial combustion and subsequent reactions occur simultaneously and it is difficult to control each reaction because the reactions are performed in the same furnace. by.

[0006]

In the method for producing carbon black, which is the object of the present invention, since the organic polymer substance is homogeneously pyrolyzed and gasified, and the pyrolysis gas is manipulated,
Compared with the conventional method for producing carbon black, it has the feature that the properties of carbon black can be controlled easily. That is, the present invention provides a method and apparatus for controlling the properties of carbon black to a required level in order to produce homogeneous carbon black from organic polymer waste such as waste tires. To aim.

[0007]

SUMMARY OF THE INVENTION The above objects of the present invention are as follows.
(1) Synthetic rubber obtained from styrene, butadiene, etc.,
In the method of pyrolyzing and gasifying an organic polymer substance such as polymer hydrocarbons such as polymers and plastics, dehydrogenating the resulting pyrolysis gas, and producing carbon black by a high condensation reaction, dehydrogenation And the properties (particle size, structure, surface activity) of the carbon black produced by controlling the gas temperature and the gas residence time of each reaction of the high condensation reaction. Control of the properties of carbon black, characterized in that it is changed by adjusting the supply amount of the oxidant of the carbon black, and the gas retention time is changed by changing the input amount and position of the quenching water in the reaction section. Method,
(2) Oxygen ratio = (supply oxygen amount / combustion equivalent oxygen amount of pyrolysis gas) is 0.3 to 0.6, and the gas temperature is in the range of 1200 to 1700 ° C. The property of the carbon black described in (1) above, characterized in that the amount and position of the quenching water in the reaction section are controlled so as to control the gas retention time to 0.1 to 1 second. And (3) Pyrolysis furnace for organic polymer, pyrolysis gas combustion and dehydrogenation / polycondensation reaction apparatus obtained from the pyrolysis furnace, apparatus for supplying an oxidant to the reaction apparatus, It is achieved by an apparatus for carrying out the method for controlling the property of carbon black according to the above (1) or (2), which comprises an apparatus for measuring the temperature of the reaction apparatus and a quenching water supply apparatus connected to the reaction apparatus. be able to.

[0008]

BEST MODE FOR CARRYING OUT THE INVENTION In the present invention, the following means are adopted to carry out the above method for controlling the properties of carbon black. That is, the homogeneous pyrolysis gas is mixed with the oxidizer and the pyrolysis gas and led to the carbon immobilization reaction section which is composed of the reaction section for high temperature combustion reaction and the reaction section for dehydrogenation and polycondensation reaction, and the mixed high temperature combustion reaction The oxidant supply device and the combustion temperature measuring device (for example, an optical pyrometer) are provided in the section, and the oxidant supply amount is controlled by the measured value. The oxidant (air or oxygen) supply amount is controlled by the pyrolysis gas property. Depending on the oxygen ratio of 0.3 to 0.6, quenching water for controlling the reaction residence time in the dehydrogenation and polycondensation reaction section (the reaction gas temperature is lowered to about 500 ° C. or lower to stop the reaction). ) Plural supply devices are arranged along the flow direction of the reaction tube so that the supply amount can be controlled, the reaction retention time can be controlled for 0.1 to 1 second, and the oxygen ratio control and the reaction retention can be performed. Hand to control the time control The provided.

The means adopted in the preceding paragraph have the following effects. The oxidant supply device supplies oxygen to the pyrolysis gas and raises the pyrolysis gas temperature by the oxidation reaction. The temperature rise is controlled to an average gas temperature of about 1200 to 1700 ° C. by setting the oxygen ratio in the range of 0.3 to 0.6. The quenching water supply device provided in the dehydrogenation / polycondensation reaction section is used to control the reaction residence time. That is, the reaction residence time up to the reaction stop temperature (<500 ° C.) is controlled by changing the quenching water input position and the amount of input water according to the temperature of the pyrolysis gas and the desired reaction residence time. Here, dehydrogenation means a reaction in which hydrogen is desorbed from a hydrocarbon compound, and condensation reaction means a reaction in which two or more molecules or two or more moieties in the same molecule form a new bond, and high condensation (polycondensation) ) Is a reaction in which these reactions occur repeatedly.

The connection control of the oxygen ratio and the reaction residence time is controlled by the production conditions (gas temperature,
(Reaction retention time), the oxygen ratio and reaction retention time are set, the pyrolysis combustion temperature is measured, and the gas temperature and gas retention time are adjusted by finely adjusting the setting conditions and adjusting the injection position and injection amount of quenching water. Control.

Here, the oxygen ratio means the ratio (molar ratio) of the supply oxygen amount to the combustion equivalent oxygen amount of the pyrolysis gas. For example, when the pyrolysis gas composition is 100% CO, the amount of oxygen required for complete combustion ( The combustion equivalent oxygen amount becomes CO + 1 / 2O ₂ → CO ₂ (1 mol 28 kg) + (1/2 mol 16 kg) → (1 mol 44 kg), and the combustion equivalent oxygen amount is 16 kg. An example of an embodiment suitable for carrying out the method of the present invention will be described below with reference to the system configuration diagram of FIG. In FIG. 1, 1 is a pyrolysis furnace for organic polymer substances, 2 and 3 are combustion and dehydrogenation / polycondensation reaction sections, 4, 5 and 6 are air supply fans for supplying oxidants to the combustion reaction sections, respectively. A flow control valve and a gas thermometer are shown, and 7, 8 and 9 are a pump of a quenching water supply device, a flow control valve and a regulating valve and an outlet gas thermometer which are respectively installed in the dehydrogenation / polycondensation reaction section. Show. The solid line shows the flow of pyrolysis gas, the chain line shows the flow of oxidant, and the broken line shows the flow of quenching water.

The homogeneous pyrolysis gas generated in the pyrolysis furnace is introduced into the combustion reaction section 2, and the amount of the oxidant corresponding to the temperature of the reaction furnace is adjusted and supplied from the air supply fan 4 by the flow control valve 5. This oxidant undergoes a combustion reaction with a part of the pyrolysis gas to give a high temperature condition necessary for dehydrogenation and polycondensation reaction. This temperature is detected by the gas thermometer 6, and the oxidant flow rate is finely adjusted so as to reach a predetermined temperature. The pyrolysis gas that has reached a high temperature is introduced into the dehydrogenation / polycondensation reaction section 3 and the residence time in this reaction section is adjusted. The means is such that the injection supply position of the quenching water supplied from the pump 7 is set by the adjusting valve 8 corresponding to the gas temperature measured by the gas thermometer 6 and the predetermined set residence time, and the amount of supplied water is measured by the outlet gas thermometer 9. The gas temperature is adjusted to a predetermined temperature (generally 500 ° C. or lower) by the adjusting valve 8 of 8.

[0013]

EXAMPLES The present invention will now be specifically described with reference to examples, but the invention is not limited thereto. Example 1 A waste tire was used as an organic polymer waste, which was cut into chips and supplied to the pyrolysis furnace 1 of FIG. 1 for pyrolysis gasification. This pyrolyzed gas was used as an oxidant together with air, and was supplied to the combustion reaction section 2 while changing the oxygen ratio to bring it to a predetermined high temperature. The pyrolyzed gas having a high temperature was introduced into the dehydrogenation / polycondensation reaction section 3 to adjust the residence time. In order to obtain the desired carbon black characteristics, the gas temperature, residence time, and quenching water supply position were variously changed to obtain a control diagram as shown in FIG. In the example shown in FIG. 2, when the gas temperature is 1500 ° C. and the residence time is 0.8 seconds, the oxygen ratio is set to 0.45 with respect to the predetermined gas temperature 1500 ° C. and the residence time is 0.8 seconds. Using injection position B, change the quenching water volume to 50
The temperature was set to 0 ° C or lower. Particle size (particle specific surface area), which is a typical characteristic of the properties of carbon black
Then, the relationship between the residence time and the gas temperature was obtained through the relationship of FIG. 2 to obtain the result of FIG. From this result, it can be seen that the specific surface area of the carbon black particles changes almost proportionally depending on the gas temperature and the gas residence time.

[0014]

In the method of the present invention, the organic polymer material is homogeneously pyrolyzed and gasified, and the pyrolyzed gas is operated. Therefore, the combustion, partial gasification and dehydrogenation, and the polycondensation reaction section are in the same furnace. It is easier to control the properties of carbon black than the conventional method for producing carbon black. By changing the gas temperature, residence time, and quenching water supply position variously, it is relatively easy to arbitrarily change the carbon black having the desired characteristics in a single furnace without using a specific furnace type, method, etc. Can be obtained.

[Brief description of drawings]

FIG. 1 is a schematic diagram showing a system configuration used in a first embodiment of the present invention.

FIG. 2 is a control diagram showing a correlation among gas temperature, oxygen ratio, residence time, and quenching water injection position when producing carbon black.

FIG. 3 is a graph showing the relationship between gas temperature and residence time for obtaining a specific carbon black specific surface area.

Claims (3)

[Claims] 1. A method for producing carbon black by pyrolyzing and gasifying an organic polymer substance and dehydrogenating the obtained pyrolyzed gas to produce a carbon black by a high condensation reaction. Controlling the properties of the carbon black produced by controlling the gas temperature and the gas residence time, the gas temperature is changed by adjusting the amount of oxidant supplied to the reaction part, and the gas A method for controlling the properties of carbon black, characterized in that the residence time is changed by changing the amount and position of addition of quenching water in the reaction section. 2. The supply amount of the oxidizing agent in the reaction section is set to the oxygen ratio =
(Supply oxygen amount / combustion equivalent oxygen amount of pyrolysis gas) 0.3
The amount of quenching water and the position of the quenching water in the reaction section are changed so as to control the gas temperature in the range of 1200 to 1700 ° C. and the gas retention time to 0.1 to 1 second. The method for controlling the properties of carbon black according to claim 1, wherein 3. An organic polymer pyrolysis furnace, a pyrolysis gas combustion and dehydrogenation / polycondensation reaction apparatus obtained from the pyrolysis furnace, an apparatus for supplying an oxidant to the reaction apparatus, and the reaction An apparatus for carrying out the method for controlling the properties of carbon black according to claim 1 or 2, which comprises an apparatus for measuring the temperature of the apparatus and a quenching water supply apparatus connected to the reaction apparatus.