JP3349249B2 - Apparatus and method for producing carbon black - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention can control not only the oil absorption of compressed dibutyl phthalate (24M4DBP), the size distribution of aggregates, the particle size distribution, etc. of carbon black, but also the fragility of aggregates. In addition, a wide range of quality
The present invention relates to a carbon black manufacturing apparatus and a manufacturing method capable of manufacturing bon black using the same manufacturing apparatus.

[0002]

2. Description of the Related Art Carbon black is a compressed dibutyl phthalate (24M4D) required according to each application field.
BP) Since the characteristics such as oil absorption, aggregate size distribution, and particle size distribution are slightly different, carbon black maker uses the structure of manufacturing equipment or the flow conditions of raw materials, combustion gas, etc., reaction conditions, etc. Carbon black of the required quality is manufactured by devising the manufacturing method and the like. Regarding the shape and structure of the manufacturing apparatus, Japanese Patent Publication No. 47-1005 discloses a method of injecting raw material hydrocarbon into a throttle section following a combustion chamber.
No. 563 discloses a method of injecting a raw material hydrocarbon into a cylindrical narrowed portion (the narrowest portion).
Discloses a method of injecting a raw material hydrocarbon into each of the cylindrical portions having different inner diameters, and various other techniques are disclosed. Regarding the flow conditions and reaction conditions of the raw material, combustion gas, etc., for example, in the above-mentioned Japanese Patent Application Laid-Open No. 4-304271, the reaction time is adjusted by selecting the injection location of the raw material hydrocarbon, or the raw material hydrocarbon is passed through the cylindrical portion. Various techniques have been disclosed, including a technique for adjusting the gas flow rate to a specific range, and others.

[0003] However, it is not always easy to control all the characteristics of the above-described carbon black to appropriate conditions according to these conventional techniques. In particular, it is intended to specify an effective index for the fragility of carbon black aggregates, which is one of the factors having an important effect on the properties of a rubber composition, and to produce carbon black having the conditions. There are no sufficient disclosure examples of the technology related to the apparatus and method. The present inventors studied the relationship between the fragility of the carbon black aggregate and the properties of the rubber composition, and newly defined an index of the fragility of the carbon black aggregate, The inventors have invented an improved apparatus and method for producing carbon black, centering on the establishment of a technique for arbitrarily adjusting the index value of black.

[0004]

SUMMARY OF THE INVENTION According to the present invention, it is possible to control not only the oil absorption of compressed dibutyl phthalate (24M4DBP), the size distribution of aggregates, and the particle size distribution of carbon black, but also the fragility of aggregates. It is another object of the present invention to provide an apparatus and a method for producing carbon black capable of producing various kinds of carbon black of a wide variety of quality using the same apparatus.

[0005]

According to the present invention, there is provided (1) a first region in which a mixture of an oxygen-containing gas and a fuel is burned to obtain a high-temperature gas flow; In a carbon black producing apparatus comprising a second region in which hydrogen is supplied and reacted, and a third region in which cooling water is sprayed on the product gas in the second region to stop the reaction, the latter stage of the first region is A reduction taper section, a rectifying section in which a cylindrical section and a subsequent narrowing section are combined in multiple stages, and the second area is a combination of a cylindrical section and a cylindrical section narrower than that. The third region is a carbon black production apparatus characterized by being a cylinder portion that is wider than the cylinder portion following the second region, and (2) the third region is following the cylinder portion that follows the second region. Enlarged taper section in the range of 2 to 20 degrees half-width, followed by cylinder Mosquito above (1), wherein it is a combination of - carbon black production apparatus, (3)
The apparatus for producing carbon black according to the above (1) or (2), wherein the reduced taper portion at the latter stage of the first area is in a range of 3 to 30 degrees in half angle. The connecting portion between the cylindrical portions comprises a reduced taper portion having a half angle of 20 to 90 degrees,
And the ratio of the diameter of the upstream cylindrical part / the diameter of the downstream cylindrical part is 1.3 to
(1) to (1), which are in the range of 1.5.
(3) The apparatus for producing carbon black as described in (3), (5) Supply of the raw material hydrocarbon in the axial direction at at least one or more locations in each of the cylindrical portion of the second region and the enlarged taper portion of the third region. The carbon black producing apparatus according to any one of the above (1) to (4), characterized by having a mouth, and (6) the carbon black producing apparatus according to the above (5), wherein a raw material hydrocarbon supply port is selectively used. Carbon black production method.

Hereinafter, the present invention will be described in detail. The dispersibility of carbon black when used in a rubber composition is one of the main indices. An important means of improving the carbon black is to increase the size of aggregates, that is, to absorb dibutyl phthalate (DBP) oil. Or this DBP
Control of these indices and the like has been conventionally performed by focusing on the difference between the oil absorption and the DBP oil absorption (24M4DBP oil absorption) after compressing the oil four times and breaking the fragile cohesive portion. On the other hand, the present inventors have studied the effective aggregate index for the purpose of improving the balance between the dispersibility of the carbon black and other properties such as tan δ. The aggregate destruction coefficient (Ds) specified by the method has been set as a new index. Ds represents the natural logarithm of the number of compressions at a pressure of 24000 psi on the horizontal axis, and the natural logarithm of the DBP oil absorption at the number of compressions on the vertical axis.
The results of six measurements of the DBP oil absorption are plotted and are the absolute values of the slopes of the straight lines obtained by simple regression. In this case, for example, a large Ds value means that the aggregate is easily broken under pressure. The present inventors have aimed to control this Ds in addition to one of the main characteristics of carbon black, together with other characteristics such as particle diameter, and a suitable apparatus and method for producing carbon black. Was developed.

In the first area, the rear part is reduced by a taper.
Section and a rectifying section composed of a combination of a multi-stage cylindrical section and a subsequent throttle section, the rectifying and piston flowing effects are exhibited regardless of the flow state of the combustion gas in the preceding section. This is a prerequisite for controlling the various properties of carbon black in the second and subsequent regions. For example, when the combustion gas in the front stage is a strong swirling flow, an appropriate rectification effect can be obtained by appropriately increasing the number of stages of the combination of the cylindrical portion and the subsequent throttle portion. In this case, it is more desirable that the half angle of the reduced taper portion is in the range of 3 to 30 degrees. In the second area,
By combining the cylindrical portion with a narrower cylindrical portion, the distribution of the particle size and the aggregate size is sharpened by the mixing action of the throttle, the 24M4DBP is increased, and Ds is increased.
Can be reduced. In this case, it is more preferable that the connecting portion between the two cylindrical portions is a reduced taper having a half angle of 20 to 90 degrees, and the ratio of the diameters of the two cylindrical portions is in the range of 1.3 to 1.5. The third region needs to be a cylinder that is wider than the cylinder following the second region. In this case, the third region is a combination of the enlarged taper portion in the range of half an angle of 2 to 20 degrees following the cylindrical portion subsequent to the second region and the cylindrical portion following the cylindrical portion. −
It is more desirable to make the It is necessary for the production apparatus that the raw material hydrocarbon supply port is provided at least at one or more locations in each of the cylindrical portion of the second region and each of the enlarged taper portions of the third region in the axial direction, In addition, it is necessary to selectively use these as a manufacturing method. Thus, for example, it is possible to increase the Ds and to make each distribution of the aggregate diameter into a brode, and it is possible to arbitrarily adjust these values in combination with the effect of the manufacturing apparatus. On the other hand, the selective use of the raw material hydrogen supply port in the present production apparatus also enables a wide range of quality carbon black to be produced by the same production apparatus.

FIG. 1 shows an example of the structure of the carbon black producing apparatus of the present invention.

[0009]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Specific embodiments of the present invention will be described below.
The examples all show the characteristics of carbon black produced by the production apparatus and production method of the present invention. Specific conditions of each embodiment are as shown in Table 1. Coal oil was used as the raw material hydrocarbon. In the second embodiment, the ratio of the amount of air to the amount of the base oil is increased as compared with the first embodiment, and in the third embodiment, the feed position of the base oil is set to the upstream side as compared with the first embodiment. In the fourth embodiment, a feed oil supply position is provided further upstream than in the third embodiment. In Comparative Example 1, the half angle of the reduced taper portion of the first area was 38 degrees,
The conditions are the same as those of the embodiment except for the conditions shown in FIG. Comparative Example 2 is the same as the Example except that there is no aperture portion (reduced taper portion) in the second area, and other conditions are the same as those shown in Table 1. The properties of the carbon blacks of these comparative examples are also shown in Table 1.

The test method used at this time is as follows. [Nitrogen adsorption specific surface area (N ₂ SA)] N ₂ SA, which is a measure of the particle size of carbon black, is ASTM D 3037.
Performed according to. [Compressed dibutyl phthalate (24MnDBP) oil absorption]
ASTM D 3493 Compressed DBP Oil Absorption (CDB
According to the measuring method of P), the value of the number of compressions n = 1 to 6 was measured. [Particle size distribution] An electron micrograph of carbon black was taken, and the photograph was taken as a particle size distribution analyzer TG manufactured by Zeiss.
Through A10, the number-based average particle diameter and the standard deviation of the particle diameter distribution were determined. [Aggregate size] Disk Confridge (D
(CF) (manufactured by JOYCE LOEBEL). Was determined by a conventional method, the most frequently strike - a box-equivalent diameter and Dst, the half-width [Delta] D ₅₀ and defined, was calculated.

When Examples 1 and 2 are compared with each other, it is understood that each characteristic of carbon black can be controlled by changing the amount of the raw material oil and the like. Comparing Examples 1, 3, and 4, it can be seen that each characteristic of carbon black can be controlled by selecting the feedstock supply position. When Example 1 and Comparative Example 1 are compared, carbon black D due to the difference in the half angle of the reduced taper in the first area is obtained.
It can be seen that the balance of s value, particle size distribution, etc. can be changed. Comparing Example 1 with Comparative Example 2, it can be seen that each characteristic value of carbon black can be controlled by the presence or absence of the aperture in the second area.

[0012]

[Table 1]

[Brief description of the drawings]

FIG. 1 is a longitudinal sectional view of an essential part showing an example of a carbon black producing apparatus of the present invention.

[Explanation of symbols]

 DESCRIPTION OF REFERENCE NUMERALS 1 First region 2 First region 3 Second region 4 Third region 5 Reduced taper portion 6 Cylindrical portion 7 Reduced taper portion 8 Cylindrical portion 9 Reduced taper portion 10 Cylindrical portion 11 Enlarged Taper section 12 Cylindrical section 13 Fuel oil supply port 14a, b Air supply port 15a-i Raw oil supply port 16 Cooling water supply port

Continued on the front page (72) Inventor Shinyasu Tanaka 4-7-3-304 Nakai, Kokurakita-ku, Kitakyushu-shi, Fukuoka (72) Inventor Isao Sumimoto 7-17-13, Nishiizumi, Yukihashi-shi, Fukuoka (56) References JP-A-4-304271 (JP, A) JP-A-3-68665 (JP, A) JP-A-2-308868 (JP, A) JP-A-2-232269 (JP, A) JP-A-4-178470 (JP, A) JP-A-4-103670 (JP, A) JP-A-3-146568 (JP, A) JP-A-4-277565 (JP, A) JP-A-60-1556764 (JP, A) Kaihei 3-223367 (JP, A) (58) Fields investigated (Int. Cl. ⁷ , DB name) C09C 1/48 C09C 1/50

Claims (6)

(57) [Claims] 1. A first region in which a mixture of an oxygen-containing gas and a fuel is burned to obtain a high-temperature gas flow, a second region in which a raw material hydrocarbon is supplied to and reacted with the high-temperature gas flow obtained in the first region. In the apparatus for producing carbon black comprising a third region in which cooling water is sprayed on the generated gas in the second region and the reaction is stopped, a reduction taper portion and a cylindrical portion are provided at the latter stage of the first region. The subsequent narrowing portion is a rectifying portion that is combined in multiple stages, the second region is a combination of a cylindrical portion and a cylindrical portion that is narrower than that, and the third region is a cylindrical portion that is subsequent to the second region. An apparatus for producing carbon black, characterized in that it is a cylindrical part which is further expanded than that. 2. The method according to claim 1, wherein the third region is a combination of an enlarged taper portion in the range of half an angle of 2 to 20 degrees following the cylindrical portion subsequent to the second region and a cylindrical portion subsequent thereto. An apparatus for producing carbon black as described above. 3. The reduced taper portion at the subsequent stage of the first area has a half-width of 3 to
The carbon black producing apparatus according to claim 1 or 2, wherein the angle is in a range of 30 degrees. 4. The connecting portion between the cylindrical portions of the second region is formed by a half angle of 20 to
4. The method according to claim 1, wherein the taper comprises a tapered portion of 90 degrees, and the ratio of the diameter of the upstream cylindrical portion to the diameter of the downstream cylindrical portion is in the range of 1.3 to 1.5. Carbon black production equipment. 5. A raw material hydrocarbon supply port is provided in each of the cylindrical portion of the second region and the enlarged taper portion of the third region in at least one position in the axial direction. An apparatus for producing carbon black according to any one of claims 1 to 4. 6. The method for producing carbon black according to claim 5, wherein a raw material hydrocarbon supply port is selectively used.