CN112852189B - Preparation method of carbon black - Google Patents
Preparation method of carbon black Download PDFInfo
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- CN112852189B CN112852189B CN202110080352.2A CN202110080352A CN112852189B CN 112852189 B CN112852189 B CN 112852189B CN 202110080352 A CN202110080352 A CN 202110080352A CN 112852189 B CN112852189 B CN 112852189B
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C1/50—Furnace black ; Preparation thereof
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Abstract
The invention relates to a preparation method of carbon black, which comprises the following steps: (1) pretreatment of tar: taking tar as a raw material, adding a dispersing agent and a structure inhibitor into the tar to prepare the treated tar; (2) performing correlation on the tar obtained in the step (1) by adopting a high-pressure jet device in the opposite direction, forming a turbulent fluid system after correlation, forming nano atomized liquid drops, blowing the nano atomized liquid drops into a combustion chamber along with hot air to perform carbonization reaction quickly, and then entering the reaction chamber to perform pyrolysis; (3) after pyrolysis, introducing quenching water for cooling, collecting the generated carbon black, granulating, and drying to obtain the final product. The invention adopts the impinging stream technology, disperses and exerts energy to the maximum by the action of shearing force, and continuously shears to form tiny tar droplets, thereby efficiently utilizing the energy of natural gas, simultaneously, the eddy shearing force generated by the impinging stream can reduce the aggregation of carbon black, and the conversion rate is improved.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a preparation method of carbon black, in particular to a method for preparing carbon black by adopting an impinging stream method in a production process.
Background
Carbon black is widely used as an inorganic chemical raw material in daily life of people. Due to the rapid development of world economy and transportation, people increasingly demand high-grade products such as automobiles and the like, so that the rubber industry mainly based on tires is developed vigorously, and the consumption of carbon black in the rubber industry accounts for 89.5 percent of the total output, wherein the carbon black mainly serves as a reinforcing agent and a filling agent in the rubber field. Although the carbon black market is wide, the current carbon black production technology faces serious pollution and energy consumption problems. The worldwide production of carbon black can be roughly divided into three categories: contact processes, thermal cracking processes, and oil furnace processes. The former two are gradually eliminated due to factors such as large energy consumption, heavy pollution, shortage of natural gas raw materials, fierce market competition and the like, and oil furnace production currently accounts for more than 95% of the production field and is the current most important production method. The oil furnace method is mainly characterized in that the oil furnace method is arranged in front of a reaction furnaceThe fuel oil is burnt in the air to form a high temperature of over 1800 ℃, the tar is cracked at high temperature to generate carbon black, and simultaneously, the quenching water is injected to cool rapidly. Because the temperature of the generated carbon black is high, the carbon black is collected after entering the bag-type dust collector after heat exchange with air through the heat exchanger, and hot air formed after the heat exchange enters the front part of the reaction furnace for combustion, so that energy is saved. However, the research of PVT international carbon black limited has revealed that only 50% or less of sensible heat is directly used for carbon black production in the oil furnace process, and nitrogen oxides and sulfur oxides are generated in the reaction. Taking the oil furnace method of Qingdao Yingchuang chemical Co Ltd for preparing carbon black as an example, the nitrogen oxide in the front tail gas of a waste heat boiler can reach 1150mg/m3The oxysulfide can reach 650mg/m3The above.
In recent years, several innovative carbon black production techniques have evolved. For example, professor jopperstdongtou, milus university, france, and frankataltado engineers, Trellebory corporation, developed two entirely new carbon black preparation techniques: the plasma method and the gamma ray method use high-density energy flow to break carbon-hydrogen bonds, and obtain the carbon black through separating force. Although the two processes have technical advantages, the yield is low, the unit energy consumption is higher, and the two processes are not suitable for large-scale industrial production.
On the whole, innovative production technology does not appear in the world, but researches are mainly carried out around the problems of single-furnace yield improvement, pre-improvement of different forms of injection ports, heat recovery and consumption reduction, emission reduction and environmental protection of an oil furnace method. The method for preparing the carbon black by using the tar with large yield and complex components meets the requirements of energy conservation and consumption reduction, and is urgent to seek a new technology for sustainable development in economy. The impinging stream process production technique was first proposed by Elperin and was subsequently greatly developed in the Tamir study. The principle is that the fluids colliding with each other not only have a large relative movement speed, but also can generate a mixing zone with high turbulence intensity at the collision position, the principle is that two opposite phase fluids collide at high speed, so that a high-speed turbulent collision area is formed between accelerating tubes, the axial speed of the fluids on a collision surface approaches zero and is converted into radial flow, particles can penetrate into the opposite flow through coherence, the relative speed reaches a maximum value at the moment of starting penetration, and then under the action of turbulence, through the formation, interaction and extinction of vortexes, the energy is dispersed from the maximum size to the minimum size. In short, the orderly fluid flow forms individual vortices that interact to break up into smaller vortices, which then continue to interact, and so on, which has the benefit of constantly spreading the energy points all around into the mass, allowing mechanical or other forms of energy to be fully applied to microscopic dimensions, resulting in internal transfer of energy. Through research for many years, the impinging stream technology is applied to various fields such as powder drying, gas absorption, liquid-liquid extraction, particle preparation and the like. In industrial application, the equipment for impinging stream has simple structure, convenient operation and wide application prospect. A method for preparing ultrafine barium sulfate by using an impinging stream is reported in patent CN 202010128216.1; patent CN201920397326.0 reports that chitosan antibacterial nano-microspheres are prepared by adopting impinging stream reinforcement; patent CN201710177813.1 reports extraction of collagen by impinging stream method. It has been proved that impinging stream is one of the most effective methods for strengthening the phase-to-phase transfer, especially the outer diffusion transfer process, and the transfer coefficient can be improved by several times to dozens of times compared with the common method, and the characteristic is in general concern. In recent years, the use of this characteristic for the preparation of ultrafine powders and the like has shown great potential applications, and research in this field is rapidly growing.
Disclosure of Invention
In order to solve the problems that carbon black produced in the process of producing the carbon black by an oil furnace method is easy to be aggregated into an integrated block, the energy utilization rate is not high in the production process, and single gun head sector jet particles are large and uneven, a high-pressure jet device is adopted, an impinging stream technology is utilized, turbulent flow is generated through impinging stream, the energy is dispersed and exerted to the maximum by utilizing the shearing force of the turbulent flow, micro tar droplets are formed through continuous shearing, so that the natural gas energy is utilized efficiently, and the carbon black with different sizes is prepared most. In the invention, liquid tar is atomized in an impinging stream mode in the process of preparing carbon black by an oil furnace method, tar liquid drops with corresponding sizes are obtained by control, and the energy of natural gas is utilized at high efficiency; meanwhile, the aggregation of the carbon black can be reduced by the vortex shearing force generated by the impinging stream, and the aggregated carbon black can be damaged by the vortex energy, so that a carbon black product with good dispersibility is finally prepared.
The problem solved by the invention is realized by the following steps:
a method of making a carbon black, the method comprising the steps of:
(1) pretreatment of tar: taking tar as a raw material, adding a dispersing agent and a structure inhibitor into the tar to prepare the treated tar;
(2) performing correlation jetting on the tar obtained in the step (1) by using a high-pressure jet device, forming a turbulent fluid system after correlation jetting to form nano atomized liquid drops, blowing the nano atomized liquid drops into a combustion chamber along with hot air for carbonization reaction, and then feeding the nano atomized liquid drops into a reaction chamber for pyrolysis;
(3) after pyrolysis, introducing quenching water for cooling, collecting the generated carbon black, granulating, and drying to obtain the final product.
According to the invention, the high-pressure jet device with two high-pressure gun heads or three high-pressure gun heads is adopted to control a certain pressure, and during opposite injection, because the rifling of the gun heads enables jet flow to be injected in a spiral shape, the impulse is increased, two spiral jet flows are subjected to energy conversion after collision, and two liquid flows are emitted outwards in a turbulent flow mode to form atomized nano liquid drops, so that carbon black products with different properties are finally prepared, and the generated carbon black is not easy to aggregate and has good dispersibility.
In some embodiments, in the step (1), the dispersant is selected from any one of methyl carbonate, ethyl acetate and isobutyl acetate, and the dispersant is added in an amount of 1.7-2.6% by volume of the tar.
In some embodiments, the structural inhibitor is selected from any one of hydroquinone and dopamine, and the addition amount of the structural inhibitor is 3-18 per mill of tar volume fraction.
In some embodiments, in the step (2), the high-pressure jet apparatus comprises two high-pressure gun heads, and the high-pressure gun heads are 180 ° or the high-pressure jet apparatus comprises three high-pressure gun heads, and the three high-pressure gun heads are 120 °.
In some embodiments, in the step (2), the caliber of the muzzle of the high-pressure jet device is 1-2mm, and the muzzle distance is 1-4 mm. In some embodiments, in the step (2), the injection pressure of the high-pressure jet device is 1 to 4 MPa. In some embodiments, in the step (2), the pyrolysis temperature of the reaction chamber is 1600-1700 ℃.
In some embodiments, the conductivity of the quench water in step (3) above is between 1 and 10 us/cm.
Compared with the prior art, the invention has the advantages that:
(1) compared with the traditional oil furnace method for producing carbon black, the temperature required by the reaction furnace can be reduced by 100-200 ℃, and the energy consumption is greatly reduced.
(2) For the production of hard carbon black, the operation flexibility is wider.
(3) According to the invention, turbulent flow is generated by collision of impinging streams, and the kinetic energy of the tar solution is converted into shearing force by cascade energy transfer to continuously act on tar droplets, so that carbon black products with different properties are finally prepared, and the generated carbon black is not easy to aggregate and has good dispersibility.
(4) The tar is pretreated, a small amount of dispersant and structural inhibitor are added, and the impinging stream technology is combined, so that the turbulent flow effect and the reaction activity in the impinging stream can be increased, and the conversion rate is further improved.
Drawings
FIG. 1 is an electron micrograph of a prior art soot prepared by spray;
FIG. 2 is an electron micrograph of carbon black prepared in example 1 of the present invention;
FIG. 3 is a schematic view of a high-pressure fluidic apparatus tip according to the present invention;
fig. 4 is a schematic diagram of the normal impact correlation of two high-pressure gun heads of the high-pressure jet device.
Detailed Description
The present invention will be described in detail below with reference to examples and drawings, but the following examples should not be construed as limiting the scope of the present invention.
Example 1
Preparing tar containing methyl carbonate and hydroquinone, wherein the content of the methyl carbonate is 1.7 percent (volume fraction), and the content of the hydroquinone is 3 per mill (volume fraction). And carrying out correlation on the prepared tar by adopting a high-pressure jet device in the opposite direction, forming a turbulent fluid system after correlation to form nano atomized liquid drops, sending the nano atomized liquid drops into a combustion chamber together with preheated hot air for combustion, and controlling the distance between two correlation tar nozzles to be 1mm and the injection pressure to be 1 MPa. After the combustion reaction is finished, the carbon black is sent to a reaction chamber and pyrolyzed to form carbon black under the condition of 1700 ℃, and the generated carbon black is cooled by quenching water with the conductivity of 1 us/cm. And (4) collecting the cooled flue gas in a cloth bag filter, and granulating and drying to finally obtain the finished product of carbon black.
Example 2
Preparing tar containing ethyl acetate and hydroquinone, wherein the ethyl acetate content is 2.6% (volume fraction), and the hydroquinone content is 18 ‰ (volume fraction). And carrying out correlation on the prepared tar by adopting a high-pressure jet device in the opposite direction, forming a turbulent fluid system after correlation to form nano atomized liquid drops, sending the nano atomized liquid drops into a combustion chamber together with preheated hot air for combustion, and controlling the distance between two correlation tar nozzles to be 2mm and the injection pressure to be 2 MPa. After the combustion reaction is finished, the carbon black is sent to a reaction chamber and pyrolyzed to form carbon black under the condition of 1600 ℃, and the generated carbon black is cooled by quenching water with the conductivity of 2 us/cm. And (4) collecting the cooled flue gas in a cloth bag filter, and granulating and drying to finally obtain the finished product of carbon black.
Example 3
Preparing tar containing ethyl carbonate and dopamine, wherein the content of the ethyl carbonate is 2.1 percent (volume fraction), and the content of the dopamine is 13 per mill (volume fraction). And carrying out correlation on the prepared tar by adopting a high-pressure jet device in the opposite direction, forming a turbulent fluid system after correlation to form nano atomized liquid drops, sending the nano atomized liquid drops into a combustion chamber together with preheated hot air for combustion, and controlling the distance between two correlation tar nozzles to be 2mm and the injection pressure to be 3 MPa. After the combustion reaction is finished, the carbon black is sent to a reaction chamber and pyrolyzed to form carbon black under the condition of 1600 ℃, and the generated carbon black is cooled by quenching water with the conductivity of 6 us/cm. And (4) collecting the cooled flue gas in a cloth bag filter, and granulating and drying to finally obtain the finished product of carbon black.
Example 4
Preparing tar containing isobutyl acetate and dopamine, wherein the content of methyl carbonate is 2.4 percent (volume fraction), and the content of hydroquinone is 10 per mill (volume fraction). And carrying out correlation on the prepared tar by adopting a high-pressure jet device in the opposite direction, forming a turbulent fluid system after correlation to form nano atomized liquid drops, sending the nano atomized liquid drops into a combustion chamber together with preheated hot air for combustion, and controlling the distance between two correlation tar nozzles to be 1mm and the injection pressure to be 4 MPa. After the combustion reaction is finished, the carbon black is sent to a reaction chamber and pyrolyzed to form carbon black under the condition of 1600 ℃, and the generated carbon black is cooled by quenching water with the conductivity of 10 us/cm. And (4) collecting the cooled flue gas in a cloth bag filter, and granulating and drying to finally obtain the finished product of carbon black.
Comparative example 1 (Tar not pretreated)
The tar is injected oppositely by a high-pressure jet device, a turbulent fluid system is formed after the injection, nano atomized liquid drops are formed, the nano atomized liquid drops are sent into a combustion chamber together with preheated hot air for combustion, the distance between two injection tar nozzles is controlled to be 1mm, and the injection pressure is controlled to be 1 MPa. After the combustion reaction is finished, the carbon black is sent to a reaction chamber and pyrolyzed to form carbon black under the condition of 1700 ℃, and the generated carbon black is cooled by quenching water with the conductivity of 1 us/cm. And (4) collecting the cooled flue gas in a cloth bag filter, and granulating and drying to finally obtain the finished product of carbon black.
Comparative example 2 (Tar pretreatment with dispersant only)
A tar was prepared which contained methyl carbonate having a methyl carbonate content of 1.7% (volume fraction). And carrying out correlation on the prepared tar by adopting a high-pressure jet device in the opposite direction, forming a turbulent fluid system after correlation to form nano atomized liquid drops, sending the nano atomized liquid drops into a combustion chamber together with preheated hot air for combustion, and controlling the distance between two correlation tar nozzles to be 1mm and the injection pressure to be 1 MPa. After the combustion reaction is finished, the carbon black is sent to a reaction chamber and pyrolyzed to form carbon black under the condition of 1700 ℃, and the generated carbon black is cooled by quenching water with the conductivity of 1 us/cm. And (4) collecting the cooled flue gas in a cloth bag filter, and granulating and drying to finally obtain the finished product of carbon black.
Comparative example 3 (Tar pretreatment with structural dispersant only)
Preparing tar containing hydroquinone, wherein the content of the hydroquinone is 3 per mill (volume fraction). And carrying out correlation on the prepared tar by adopting a high-pressure jet device in the opposite direction, forming a turbulent fluid system after correlation to form nano atomized liquid drops, sending the nano atomized liquid drops into a combustion chamber together with preheated hot air for combustion, and controlling the distance between two correlation tar nozzles to be 1mm and the injection pressure to be 1 MPa. After the combustion reaction is finished, the carbon black is sent to a reaction chamber and pyrolyzed to form carbon black under the condition of 1700 ℃, and the generated carbon black is cooled by quenching water with the conductivity of 1 us/cm. And (4) collecting the cooled flue gas in a cloth bag filter, and granulating and drying to finally obtain the finished product of carbon black.
Through experiments, the carbon black prepared in the examples of the application has the advantage that the conversion rate is obviously improved compared with that of comparative examples 1, 2 and 3.
The prior art usually adopts the conventional spraying technology, a single gun head sector is adopted, the sprayed particles are large, the prepared carbon black is not uniform, and agglomeration is easy to occur, as shown in figure 1. In the invention, a high-pressure jet device is adopted, the impact flow is utilized to generate turbulence, the kinetic energy of the tar solution is converted into shearing force by cascade energy transfer, the shearing force continuously acts on tar droplets, and finally carbon black products with different properties are prepared, as shown in figure 2, compared with the prior art, the carbon black prepared by the method is not easy to aggregate and has good dispersibility.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention in any way, and any person skilled in the art can make any simple modification, equivalent replacement, and improvement on the above embodiment without departing from the technical spirit of the present invention, and still fall within the protection scope of the technical solution of the present invention.
Claims (6)
1. A method for preparing carbon black, which is characterized in that: the preparation method comprises the following steps:
(1) pretreatment of tar: taking tar as a raw material, adding a dispersing agent and a structure inhibitor into the tar to prepare the treated tar; the dispersing agent is selected from any one of methyl carbonate, ethyl acetate and isobutyl acetate, and the structure inhibitor is selected from any one of hydroquinone and dopamine;
(2) performing correlation on the tar obtained in the step (1) by using a high-pressure jet device, forming a turbulent fluid system after correlation to form nano atomized liquid drops, blowing the nano atomized liquid drops into a combustion chamber along with hot air to perform carbonization reaction, and then entering a reaction chamber to perform pyrolysis, wherein the pyrolysis temperature of the reaction chamber is 1600-; the injection pressure of the high-pressure jet device is 1-4 MPa;
(3) after pyrolysis, introducing quenching water for cooling, collecting the generated carbon black, granulating, and drying to obtain the final product.
2. The method for producing carbon black according to claim 1, characterized in that: in the step (1), the addition amount of the dispersing agent is 1.7-2.6% of the volume fraction of tar.
3. The method for producing carbon black according to claim 1, characterized in that: in the step (1), the addition amount of the structural inhibitor is 3-18 per mill of the volume fraction of the tar.
4. The method for producing carbon black according to claim 1, characterized in that: in the step (2), the high-pressure jet device comprises two high-pressure gun heads, the two high-pressure gun heads are 180 degrees or the high-pressure jet device comprises three high-pressure gun heads, and the three high-pressure gun heads are 120 degrees.
5. The method for producing carbon black according to claim 1, characterized in that: in the step (2), the caliber of the muzzle of the high-pressure jet device is 1-2mm, and the muzzle distance is 1-4 mm.
6. The method for producing carbon black according to claim 1, characterized in that: in the step (3), the conductivity of the quenching water is between 1 and 10 us/cm.
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