CN1046921A - Tandem quench - Google Patents
Tandem quench Download PDFInfo
- Publication number
- CN1046921A CN1046921A CN90102031A CN90102031A CN1046921A CN 1046921 A CN1046921 A CN 1046921A CN 90102031 A CN90102031 A CN 90102031A CN 90102031 A CN90102031 A CN 90102031A CN 1046921 A CN1046921 A CN 1046921A
- Authority
- CN
- China
- Prior art keywords
- effluent
- raw material
- carbon black
- method described
- reduces
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000010791 quenching Methods 0.000 title claims description 88
- 239000006229 carbon black Substances 0.000 claims abstract description 90
- 238000000034 method Methods 0.000 claims abstract description 68
- 239000002994 raw material Substances 0.000 claims abstract description 48
- 239000000567 combustion gas Substances 0.000 claims abstract description 27
- 230000002776 aggregation Effects 0.000 claims abstract description 14
- 238000004220 aggregation Methods 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims description 33
- 238000000197 pyrolysis Methods 0.000 claims description 14
- 230000009467 reduction Effects 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 42
- 230000008569 process Effects 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 4
- 230000000171 quenching effect Effects 0.000 description 60
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 20
- 230000008859 change Effects 0.000 description 15
- 238000002347 injection Methods 0.000 description 12
- 239000007924 injection Substances 0.000 description 12
- 238000002485 combustion reaction Methods 0.000 description 9
- 239000012530 fluid Substances 0.000 description 9
- 239000004215 Carbon black (E152) Substances 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 229930195733 hydrocarbon Natural products 0.000 description 7
- 150000002430 hydrocarbons Chemical class 0.000 description 7
- 238000000605 extraction Methods 0.000 description 6
- LTUJKAYZIMMJEP-UHFFFAOYSA-N 9-[4-(4-carbazol-9-yl-2-methylphenyl)-3-methylphenyl]carbazole Chemical compound C12=CC=CC=C2C2=CC=CC=C2N1C1=CC=C(C=2C(=CC(=CC=2)N2C3=CC=CC=C3C3=CC=CC=C32)C)C(C)=C1 LTUJKAYZIMMJEP-UHFFFAOYSA-N 0.000 description 5
- 238000003672 processing method Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 241000872198 Serjania polyphylla Species 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000000446 fuel Substances 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 230000009183 running Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000007669 thermal treatment Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 241000276498 Pollachius virens Species 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000003738 black carbon Substances 0.000 description 2
- 230000003139 buffering effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013569 fruit product Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/56—Treatment of carbon black ; Purification
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/50—Furnace black ; Preparation thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Carbon And Carbon Compounds (AREA)
- Beans For Foods Or Fodder (AREA)
- Telephone Function (AREA)
- Confectionery (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
A kind of control is by the aggregation size of the carbon black of oven process carbon black reactor production and the method for structure, promptly when being about 0.0-0.002 second (beginning to calculate from the raw material decanting point in downstream), reduces the residence time effluent (mixture of combustion gases and raw material, have pyrolytic reaction to take place therein) temperature, but do not stop pyrolytic reaction wherein, temperature be reduced to many about 800 °F better.
Description
The present invention relates to a kind of size of carbon black focusing and method of structure controlled.
Usually the production method of carbon black is that the combustion gases with heat make the hydrocarbon raw material pyrolysis contain the products of combustion of particulate state carbon black with generation in kiln type reactor.
In one type oven process carbon black reactor (as described in the United States Patent (USP) 2785964 of people's such as Kester United States Patent (USP) 3401020 or Pollock, be referred to as " Kester " and " Pollock " below respectively), with a kind of fuel (hydrocarbonaceous better) and a kind of oxygenant (air is better) injection first district, and react the generation combustion gases.Hydrocarbon feed with gas, steam or liquid form injects first district simultaneously, makes it to begin pyrolysis here.Here, pyrolysis is meant the hydrocarbon decomposes.Resulting combustion gas mixt (wherein having pyrolytic reaction to take place) feeds reaction zone, in this district, finishes the reaction that generates carbon black.
In the type of furnace carbon black reactor of another kind of type, make a kind of liquid or geseous fuel in first district, generate hot combustion gas with oxygenant (air is better) reaction.These hot combustion gas come out from first district, and are dirty in reactor, enter beyond the reaction zone.In order to produce carbon black, on one or more points of hot burning gas circulation flow path, inject hydrocarbon feed.This hydrocarbon feed can be liquid, gas or steam, and can be with producing combustion gases stream used fuel is identical or different.First (or burning) district and reaction zone can have the suppression mouth or the suppression of undergauge to distinguish with one, and its cross-sectional diameter is less than combustion zone or reaction zone.The raw material inlet can be in the hot combustion gas passage in upstream, downstream and/or the undergauge section of undergauge section.Such oven process carbon black reactor is issued in patent 28974 and the United States Patent (USP) 3922335 in the U.S. again general narration.
Though narrated two types oven process carbon black reactor and processing method, should understand, the present invention can be used in any other oven process carbon black reactors or processing method by hydrocarbon pyrolysis and/or incomplete combustion production carbon black.
In above-mentioned two types processing method and reactor, and in other common known reactor and processing method, hot combustion gas is in is enough to make the hydrocarbonaceous raw material generation pyrolytic temperature of injecting combustion gas flowing.In one type reactor (disclosed in as Kester), raw material promptly generates in same district on one or more points in district of combustion gases and injects.In the reactor or processing method of other type, raw material is to have formed on later one or more points at combustion gases stream to inject.In this reactor of two types, because hot combustion gas stream is downward through reactor continuously, along with raw material and the combustion gas mixt reaction zone of flowing through, pyrolytic reaction takes place continuously.The raw material and following all be called in whole application " effluent " of mixing of combustion gases thing of pyrolytic reaction take place therein.The time that effluent stops in the reaction zone of reactor is competent, under conditions suitable, can generate carbon black." residence time " has been meant between hot combustion gas and raw material institute's elapsed time amount since the initial contact.After carbon black with desired properties formed, the temperature that further reduces effluent was to stop pyrolysis.Thisly can finish by any currently known methods, for example in effluent, inject quench liquid by a quenching apparatus for stopping the operation that pyrolysis reduces effluent temperature.Usually know as the common skilled person in this area, when having generated required carbon black product in the reactor, pyrolysis is stopped.A method determining to stop the pyrolytic time is sampling and measure its methylbenzene extraction level from effluent.The methylbenzene extraction level is measured with ASTM D1618-83 " Carbon Black Extractables-Toluene Discoloration " method.Quenching apparatus is installed in usually and reaches on that of acceptable level the required carbon black that the methylbenzene extraction level of effluent produces in reactor.After pyrolysis stopped, effluent separated through a bag shape filtration unit usually and collects carbon black.
Usually use single quenching apparatus, be to use two quenching apparatus but Kester is disclosed, with some performance of control carbon black.Kester relates to tax mould (modulus-imparting) performance by the thermal treatment control carbon black.This thermal treatment is to realize by the flow velocity of the water of two water spray quenching apparatus regulating the assembled in series that feeds in carbon black stove effluent smog.The modulus of carbon black relates to the usefulness of carbon black in rubber product.As Schaeffer and Smith. at " Effect of Heat Treatment on Reinforeing Properties of Carbon Black " (industry and engineering chemistry, 47 volumes, No. 6; June nineteen fifty-five, 1286 pages; Be called " Schaeffer " later on) explained in the article, know that usually thermal treatment will influence the tax mould performance of carbon black.But Schaeffer further explains again, and the tax mould changes of properties of the carbon black by treatment production is because due to the black carbon surface chemical transformation.Therefore, quenching apparatus is installed so that combustion gases stream bears the tax mould performance that different temperature condition influences carbon black by the mode that Kester advised, obviously be because the variation of black carbon surface chemistry, rather than because can discernible mode to influence the form of carbon black.Moreover in the Kester method, two quenching apparatus all are installed in and have obviously taken place in the raw material pyrolytic reaction zone.So as can be seen, in the Kester method, when effluent flow to first quenching apparatus, character such as the CTAB of carbon black, tone, DBP and Stokes diameter limited.This point is supported following conclusion, and promptly composing the mould changes of properties in the Kester method is not because due to the change of properties of carbon black morphology aspect.In addition, with respect to the raw material decanting point or the residence time, Kester does not emphasize any importance of the position of first quenching apparatus, and does not openly select the method for first quenching apparatus.
The United States Patent (USP) 4230670(of Forseth is to call Forseth in the following text) advise using two quenching apparatus to stop pyrolytic reaction.These two quenching apparatus are spaced from each other several inches, are installed on the position that single quenching apparatus should be installed.Using the purpose of two quenching apparatus is to be full of reaction zone more completely with quench liquid, so that more effectively stop the heat energy reaction.But in the Forseth method, when arriving quenching apparatus to effluent, character such as the CTAB of carbon black, Tint, DBP and Stokes diameter limit.
People's such as Mills United States Patent (USP) 4265870 and 4316876 suggestions in the somewhere, downstream of first quenching apparatus again with one second quenching apparatus to prevent damage to filtering system.In these two patents, first quenching apparatus stops pyrolytic reaction fully, and is mounted on the common known position, this area, and when effluent arrived first quenching apparatus, performances such as the CTAB of carbon black, Tint, DBP and Stokes diameter limited.Second quenching apparatus further reduces the temperature of combustion gases stream, the protection filtering unit.
The United States Patent (USP) 4358289(of Austin is to call Austin in the following text) also relate to after the chilling with heat exchanger and prevent damage filtering system.In this patent, also be to stop pyrolytic reaction fully, and quenching apparatus is installed on the common known position, this area by chilling.In Austin, when effluent arrived first quenching apparatus, performances such as the CTAB of carbon black, Tint, DBP and Stokes diameter limited.
The United States Patent (USP) 3615211(of Lewis is to call Lewis in the following text) relate to homogeneity and the extension reactor method of life of improving the carbon black that reactor generates.In order to improve homogeneity and extension reactor life-span, a plurality of quenching apparatus that are installed in the entire reaction district are used in the Lewis suggestion, to keep the temperature that is in substantially constant in the reaction zone.The quenching apparatus of installing from farthest, reactor upstream injects a certain amount of quench liquid, after each downstream quench device in the relatively large quench liquid of injection.The quenching apparatus that is positioned at the farthest, downstream stops pyrolytic reaction.By keeping the steady temperature in the reaction zone, the Lewis device just can promote the homogeneity by the carbon black of this device production.But multiple quenching apparatus can not be controlled the form of the carbon black of device production thus.
But hope can be controlled the form of carbon black usually, comes so that can produce the carbon black that can adapt to its concrete end-use.Also wish to increase the carbon black aggregation size and the structure of given surface-area, this is (to show as higher DBP value, lower Tint value and bigger Stokes diameter) because aggregation size that increases and structure can make carbon black be suitable for some end-use better.
Therefore, an object of the present invention is to provide a kind of aggregation size of carbon black and method of structure controlled.
Another object of the present invention is to produce to have given surface-area and assemble big, the higher carbon black of structure.
We have found the method that reaches these purposes.Discovery can be controlled the form of the carbon black of producing with oven process carbon black production method, method is in the specified residence time (about at the most 0.002 second, calculate toward the downstream from the raw material decanting point in downstream), do not stop the pyrolytic reaction of effluent and its temperature is reduced (about at the most 800 °F better).Reducing temperature can install first quenching apparatus and inject quench liquid by being no more than about 4 feet place at the raw material decanting point from downstream toward the downstream.According to the present invention, can control the working condition of carbon black, so that produce the carbon black that has given surface-area (CTAB) but have specific modality performance (as assembling big and the structure increase, it is higher to show as the DBP value, and the tint value increases than low and Stokes diameter).We also find, by changing the amount that effluent temperature reduces, and/or change raw material decanting point from downstream to the residence time the reduction effluent temperature, can further control the form performance of carbon black.
In more detail, the present invention relates to the aggregation size of the carbon black that a kind of control produced by the oven process carbon black reactor and the method for structure, i.e. reduction effluent (combustion gases of pyrolytic reaction and the mixture of raw material take place therein) temperature but do not stop wherein pyrolytic reaction when residence time of about 0.0-0.002 second (about 0.0-0.0015 is better second) (from the raw material decanting point in downstream toward downstream calculating).In the above-mentioned specified residence time, effluent temperature reduces, about at the most 800 °F better, about 50-800 °F is better.The reduction of effluent temperature can be by being installed in certain point in the reactor quenching apparatus (preferably injecting the quenching apparatus of quench liquid in the effluent) realize, the installation site of quenching apparatus should be able to make effluent be subjected to chilling when about 0.0-0.002 second (about 0.0-0.0015 is better second, is calculated toward the downstream by the raw material decanting point in downstream).Usually, specifying in the residence time by chilling in order to make effluent, the raw material decanting point that quenching apparatus should be installed in from downstream is no more than 4 feet place.This quenching apparatus reduces the temperature of effluent, about at the most 800 °F better, about 50 to about 800 °F better, but do not stop pyrolytic reaction.According to the present invention, the residence time when effluent temperature reduction amount and effluent temperature reduce can change independently or side by side, to control the aggregation size and the structure of the carbon black that this reactor produces.So that reduce the reactor of effluent temperature in the appointment residence time, the change of the residence time when effluent temperature reduction amount and effluent temperature reduce can realize from the amount of the quench liquid of quenching apparatus injection and the position of change quenching apparatus by change respectively at use quenching apparatus, injection quench liquid.After the carbon black with desired properties forms, stop the heat energy reaction.
According to the present invention, the carbon black product that has bigger gathering and structure in the time of can producing than the carbon black of producing by similar approach (not specifying the residence time to reduce effluent temperature) at given surface-area.
Aggregation size and structure that an advantage of the inventive method is a carbon black can be controlled.
Another advantage of the inventive method is to produce the carbon black that has bigger gathering and structure (show that the DBP value is higher, the tint value is lower, and the Stokes diameter increases) for given surface-area (showing on the CTAB value).
From following narration and claim, can obviously find out other advantage of the present invention.
Accompanying drawing is the sectional view of an embodiment of reactor of the present invention, shows the position of first and second quenching apparatus.
Accompanying drawing has been described a possible embodiment of the present invention.Though described the part of one type of carbon black reactor among the figure, as explained earlier, the present invention can be used for any oven process carbon black reactor of producing carbon black by hydrocarbon pyrolysis and/or incomplete combustion.In addition, though following content interpret use a quenching apparatus, inject quench liquid to reduce one embodiment of the invention of effluent temperature, but ordinary skill those skilled in the art should be appreciated that, present invention resides in and specify in the residence time any method that (beginning to calculate from the raw material decanting point near reaction zone) reduces effluent temperature (it is better to reduce specified amount).Similarly, though following content description stop pyrolytic reaction with second quenching apparatus, ordinary skill those skilled in the art should be appreciated that, the present invention includes any method that stops pyrolytic reaction.
In the accompanying drawing, at point 60 places first quenching apparatus 40 is housed in the part of carbon black reactor 10 (for example containing reaction zone 12 and reduced district 20), second quenching apparatus 42 is equipped with at 62 places at point, so that inject quench liquid 50.For each quenching apparatus, its quench liquid 50 can be identical or different.Hot combustion gas stream flow through reactor 10 and 12 and 20 o'clock flow direction represent with arrow.Quench liquid 50 can inject by opposite with the combustion gases flow path direction or preferably identical direction with second quenching apparatus 42 by first quenching apparatus 40.Point 14 is downstream decanting points of raw material 30.The ordinary skill personnel of this area will be understood that the raw material decanting point in downstream can change.Represent with L-1 from the distance raw material decanting point 14 to the first quenching apparatus positions 60, downstream, represent with L-2 from the distance raw material decanting point 14 to the second quenching apparatus positions 62, downstream.
According to described embodiment of the present invention, first quenching apparatus 60 is in order to reduce the temperature of effluent in earlier than 0.002 second (0.0-0.0015 is better second, is calculated by the raw material decanting point in downstream) retention time.Usually, be subjected to chilling in order to make effluent in specifying retention time, first quenching apparatus should be positioned at from downstream raw material decanting point and be no more than 4 feet place.Therefore L-1 should be about 0.0-4 foot.Inject quench liquid so that effluent temperature is reduced to many 800 °F (preferred amounts) by first quenching apparatus 60, reduce about 50-800 °F better, but will satisfy such condition: promptly the quench liquid that is injected by first quenching apparatus 60 can not stop pyrolytic reaction.
In addition, according to the present invention, from the raw material decanting point in downstream to the effluent (mixture of combustion gases and raw material, pyrolytic reaction takes place therein) residence time and the effluent temperature amount that reduce of temperature between beginning to reduce, can change individually or simultaneously, with aggregation size and the structure of control by the carbon black of reactor production.In embodiment of the present invention shown in the drawings, change L-1 and will change the residence time (from the time of downstream raw material injection length when effluent temperature reduces).By changing the amount of the quench liquid that is injected, can change the reduction amount of effluent temperature.
As what explain the last period, in embodiment of the present invention shown in the drawings, according to needed aggregation size and structure, the scope of L-1 is about the 0.0-4 foot usually.Quench liquid 50 with effluent temperature be reduced to many about 800 °F better, reduces about 50-800 °F better, but the condition that will satisfy is not stop pyrolytic reaction at first quenching apparatus, 60 place's quench liquids 50.
After the carbon black with desired properties has generated, just stop pyrolytic reaction by quenching apparatus 42 at 62 places.62 this point are to produce the position with desired properties carbon black by reactor.Release as the front, in order to select the position in order to the quenching apparatus that stops pyrolytic reaction, available any method known in the art is determined the position of 62 this point.In order to a kind of method of the position of determining to stop the quenching apparatus that pyrolytic reaction uses is position when determining that carbon black product that reaction generates has reached acceptable methylbenzene extraction level.Method described in the available ASTM Test of the methylbenzene extraction level D1618-83 " Carbon Black Extractables-Toluene Discoloration " is measured.L-2 will change according to the position of point 62.
Effect of the present invention and advantage will further specify by following embodiment.
In order to show effect of the present invention, with two quenching apparatus, and change the residence time being lowered to effluent temperature from downstream raw material decanting point and change the amount that effluent temperature reduces, the carbon black production method is tested.Change this residence time by changing L-1.The parameter of two groups of carbon black production operations and result are summarised in the following table in the experiment.The I group comprises that experiment 1,2 and 3, the II groups comprise experiment 4,5 and 6.
I group: preheating=900; Gas=7.2kscfh; Air=80kscfh;
Air=11.11; Primary combustion=123%; Combustion zone volume=0.85ft
3;
Injection zone diameter=4.2 inch; Injection zone length=12 inch;
Injection zone burning gas flow velocity=2000ft/ second; Oil=125gph;
Inject oil pressure=230psig; # oil nozzle=4; Oil nozzle diameter=0.042 inch;
Reaction zone diameter=13.5 inch.
Liquid starting material is formed: H/C is than=91; Hydrogen=6.89Wt%, 7.00Wt%;
Carbon=91.9Wt%, 90.8Wt%; Sulphur=1.1Wt%; API
Proportion 15.6/15.6C(60F)=5.0; BMCI(viscosity proportion)=141
II group: preheating=1100; Gas=7.5kscfh; Air=80kscfh;
Air=10.6; Primary combustion=118%; Combustion zone volume=0.85ft
3;
Injection zone diameter=4.2 inch; Injection zone length=12 inch;
Injection region burning gas flow velocity=2300ft/ second; Oil=136gph;
Inject oil pressure=270psig; # oil nozzle=4; Oil nozzle diameter=0.042 inch;
Reaction zone diameter=6 inch.
Liquid starting material (oil) is formed: H/C=1.06; Hydrogen=7.99%(weight),
7.99%(weight); Carbon=89.7%(weight), 89.5%(weight); Sulphur=0.5%(weight);
Api gravity 15.6/15.6C(60F)=0.5; BMCI(viscosity proportion)=123
In I and II group, used fluid fuel is a Sweet natural gas in the combustion reactions, and methane content is 95.44%, and wet calorific value is 925 BTU/SCF.
Those of ordinary skills will appreciate that generally listed processing parameter is represented the parameter of a point in the reactor in the table, and available common known method is measured.Each is organized carbon black production experiment and is being similar to United States Patent (USP) 3,922, carries out in the disclosed reactor among 335 embodiment 1, and difference is dated in table.
Q is meant quenching apparatus in the table, a Q(foot) be meant L-1, i.e. distance from downstream raw material decanting point to first quenching apparatus.Temperature (before the Q) is meant effluent temperature before first quenching apparatus, and temperature (behind the Q) and temperature (behind the 2nd Q) refer to behind first quenching apparatus temperature of raw material and combustion gas mixt behind the effluent temperature and second quenching apparatus respectively.All relate to the temperature of chilling all by known conventional thermodynamics technique computes.In the table residence time be meant from after the raw material decanting point in downstream to the time quantum that is consumed before effluent temperature begins to reduce.The 2nd Q(foot) be meant L-2, it is rule of thumb measured with the methylbenzene extraction level.After the experiment, all collects the carbon black of being produced and performs an analysis each time, with mensuration CTAB, tint, Dst(Stokes median diameter), CDBP, free-running property DBP and toluene decolorization.Each result of experiment is shown in the table.
CTAB measures according to ASTM methods of test D3765-85.The Tint value is measured according to ASTM methods of test D3265-85a.The DBP value of loose carbon black is measured according to the method that ASTM D-2414-86 proposes.The CDBP value is measured according to the method that ASTM D3493-86 proposes.The toluene decolorization is measured according to ASTM methods of test D1618-83.
The Dst(Stokes median diameter) measures with the centrifugal photoelectricity deposition instrument of disc type (disc centrifuge photosedimentometry) according to the method for introducing below.Following method is the improvement of method described in the JoyceLoebl disc type centrifuging Guide Book, case DCF4.008, and on February 1st, 1985 published, the distribution of Joyce-Loebl company, (Marquisway, Team Valley, Gateshead, Tyne ﹠amp; Wear, England), this technology is drawn herein as a reference.Method is as follows: weigh up 10 milligrams of carbon black samples with weighing machine, add 50 milliliter of 10% dehydrated alcohol and the 90% distilled water solution of (containing 0.05%NONIDET P-40 tensio-active agent) then, NONIDET P-40 is the registered trademark of the tensio-active agent of Shell chemical company produce and market.This suspension is with Sonifier(model W 385, by Heat Systems Ultrasonics company produce and market, Farmingdale, New York) disperse to make in 15 minutes suspension by ultrasonic energy.Before the disc type centrefuge experiment, following data are imported in order in the data computing machine of record from disc centrifuge.
1. carbon black proportion is taken as 1.86 grams per milliliters;
2. carbon black is scattered in the liquor capacity in water and the ethanolic soln, and this example is 0.5 milliliter;
3. rotating fluid volume, this example is 10 ml waters;
4. rotating fluid viscosity, this example is 0.933 centipoise (23 ℃);
5. the density of rotating fluid, this example is 0.9975 grams per milliliter (23 ℃);
6. dish is fast, and this example is 8000 rev/mins;
Data sampling at interval, this example is 1 second.
Disc type is centrifugal 8000 rev/mins of runnings down, makes the running of flash of light velometer simultaneously.10 ml distilled waters are injected rotating disk as rotating fluid.Turbidity is set at 0; The solution of 1 milliliter of 10% dehydrated alcohol and 90% distilled water is injected as buffering liquid.The operation-plate type whizzer dam and the supercharging knob to produce the level and smooth concentration gradient between rotating fluid and the buffering liquid, this gradient monitors with appearance method.When this gradient variable gets smoothly, when not having distinguishable boundary between these two kinds of fluids, inject 0.5 milliliter of carbon black that is dispersed in aqueous ethanolic solution in rotating disk, and begin to collect data immediately.If produce liquid stream, shut down immediately.Be scattered in after the carbon black of aqueous ethanolic solution this disc spins 20 minutes in injection.Rotate after 20 minutes, dish is stopped, measuring the temperature of rotating fluid, the mean value of measured rotating fluid temperature was input in the record disc centrifuge data computing machine when when beginning running and running were finished.According to these data of Stokes formula analysis of standard, and represent with following definitions:
Carbon black gathering-a kind of isolating rigidity colloidal entity, promptly I discrete units; It is by a large amount of bonded granulometric composition;
The diameter of sedimentary globe in the resisting medium in centrifugal field or gravity field of Stokes diameter-meet Stokes formula.Be considered to and have and density that this non-globe is same and the level and smooth rigidity globe of sedimentation velocity have identical behavior as the non-globe in the fruit product, then non-globe (as carbon black aggregate) also can be expressed with this term of Stokes diameter.Common unit is nm.
A point on Stokes median diameter (using Dst in the report)-Stokes diameter distribution curve has 50%(weight on this aspect) the diameter of sample or greater or lesser.Therefore its represents the intermediate value of mensuration.
As shown in Table, produce carbon black that contrast method (1 and 4, use single quenching apparatus) produces relatively with carbon black, CDBP value, free-running property DBP value and the increase of Dst value of the carbon black of producing with the inventive method, and the tint value reduces.This result shows that carbon black of the present invention is characterised in that has increased aggregation size and structure.In addition, shown in second group result, for relative constant CTAB value, can produce CDBP value, free-running property DBP value and Dst value with the inventive method increases, and the carbon black that the tint value reduces.This shows, the carbon black that the present invention can produce aggregation size and structure when given CTAB all increase.
Shown in I group result, producing contrast method 1 with carbon black compares, when using the inventive method, adopt the different residence time (effluent temperature initial reduce identical amount) at this moment to produce to have CDBP, free-running property DBP and the increase of Dst value and carbon black that the tint value reduces.
Because the present invention relates to control the method for carbon black aggregation size and structure, in above-mentioned carbon black production method, clearly, can carry out a lot of flexible the present invention that do not break away from revising.Therefore, it should be clearly understood that the form of the present invention with shown in the figure of narration just illustrates scope of the present invention here, and be not intended to limit it.The present invention includes all modification in the following claims.
Claims (20)
1, a kind of method of controlling carbon black aggregation size and structure comprises;
Hot combustion gas stream is passed through a reactor;
In hot combustion gas stream, inject raw material by one or more points, form a kind of effluent, and the raw material in the effluent begins pyrolysis;
In 0.002 second time, first point that calculates toward the downstream at the raw material decanting point from downstream reduces effluent temperature, and does not stop the pyrolysis of raw material in the effluent.
2, the method described in the claim 1, wherein effluent temperature reduction amount is about 800 °F at the most.
3, the method described in the claim 1, wherein effluent temperature reduces about 50-800 °F.
4, the method described in the claim 1 wherein reduces the temperature of effluent at about 0.0-0.0015 in the time of second (calculating from the raw material decanting point in downstream).
5, the method described in the claim 3, the time when wherein effluent temperature reduces is about 0.0-0.0015 second (beginning calculating from the raw material decanting point in downstream).
6, the method described in the claim 1 wherein reduces effluent temperature by injecting quench liquid.
7, the method described in the claim 6, the time when wherein effluent temperature reduces is about 0.0-0.0015 second (beginning calculating from the raw material decanting point in downstream).
8, the method described in the claim 6, wherein quench liquid is reduced to many about 800 °F with effluent temperature.
9, the method described in the claim 6, wherein quench liquid reduces about 50-800 °F with effluent temperature.
10, the method described in the claim 7, wherein quench liquid reduces about 50-800 °F with effluent temperature.
11, a kind of production has the method for the carbon black of in check aggregation size and structure, comprising: hot combustion gas stream is passed through reactor;
In hot combustion gas stream, inject raw material by one or more points, form a kind of effluent, and the raw material in the effluent begins pyrolysis;
In 0.002 second time, first point that calculates toward the downstream at the raw material decanting point from downstream reduces effluent temperature, and does not stop the pyrolysis of raw material in the effluent;
At second point, in the downstream of first point, further reduce the temperature of effluent, with pyrolysis and separation and the collection carbon black product that stops raw material in the effluent.
12, the method described in the claim 11, wherein effluent temperature is reduced to many about 800 °F.
13, the method described in the claim 11, wherein effluent temperature reduction amount is about at the most 50-800 °F.
14, the method described in the claim 11, the time when wherein effluent temperature reduces is about 0.0-0.0015 second (beginning calculating from the raw material decanting point in downstream).
15, the method described in the claim 13, the time when wherein effluent temperature reduces is about 0.0-0.0015 second (beginning calculating from the raw material decanting point in downstream).
16, the method described in the claim 11 wherein reduces effluent temperature by injecting quench liquid.
17, the method described in the claim 16, the time when wherein effluent temperature reduces is about 0.0-0.0015 second (beginning calculating from the raw material decanting point in downstream).
18, the method described in the claim 6, wherein quench liquid is reduced to many about 800 °F with effluent temperature.
19, the method described in the claim 16, wherein quench liquid reduces about 50-800 °F with effluent temperature.
20, the method described in the claim 17, wherein quench liquid reduces about 50-800 °F with effluent temperature.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US33414489A | 1989-04-06 | 1989-04-06 | |
| US334,144 | 1989-04-06 | ||
| US37072389A | 1989-06-23 | 1989-06-23 | |
| US370,723 | 1989-06-23 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1046921A true CN1046921A (en) | 1990-11-14 |
| CN1050855C CN1050855C (en) | 2000-03-29 |
Family
ID=26989058
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN90102031A Expired - Fee Related CN1050855C (en) | 1989-04-06 | 1990-04-06 | Tandem quench |
Country Status (22)
| Country | Link |
|---|---|
| JP (1) | JPH0749541B2 (en) |
| KR (1) | KR930005684B1 (en) |
| CN (1) | CN1050855C (en) |
| AR (1) | AR245477A1 (en) |
| AU (1) | AU625117B2 (en) |
| BE (1) | BE1002548A3 (en) |
| BR (1) | BR9001575A (en) |
| CA (1) | CA2012627C (en) |
| CZ (1) | CZ284688B6 (en) |
| DE (1) | DE4010776A1 (en) |
| ES (1) | ES2020713A6 (en) |
| FR (1) | FR2645542B1 (en) |
| GB (1) | GB2232409B (en) |
| HU (1) | HUT55316A (en) |
| IT (1) | IT1240745B (en) |
| NL (1) | NL9000500A (en) |
| PE (1) | PE3991A1 (en) |
| PL (1) | PL163727B1 (en) |
| PT (1) | PT93676A (en) |
| RO (1) | RO113148B1 (en) |
| SE (1) | SE9001090L (en) |
| TR (1) | TR24400A (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004281293A (en) * | 2003-03-18 | 2004-10-07 | Tokai Rubber Ind Ltd | Hose material for fuel cell system and hose for fuel cell system using the same |
| JP5027989B2 (en) * | 2004-03-25 | 2012-09-19 | 旭カーボン株式会社 | Manufacturing method of carbon black for tire tread |
| JP5697304B2 (en) * | 2008-12-17 | 2015-04-08 | 旭カーボン株式会社 | Production method of carbon black |
| JP2010144011A (en) * | 2008-12-17 | 2010-07-01 | Asahi Carbon Kk | Carbon black to be compounded with tire tread rubber, rubber composition for tire using the same and tire for automobile |
| JP2010144003A (en) * | 2008-12-17 | 2010-07-01 | Asahi Carbon Kk | Method of manufacturing carbon black, carbon black obtained by the method, and rubber composition containing the carbon black |
| JP5887096B2 (en) * | 2011-10-06 | 2016-03-16 | 旭カーボン株式会社 | Production method of carbon black |
Family Cites Families (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2785964A (en) * | 1953-08-17 | 1957-03-19 | Phillips Petroleum Co | Process, apparatus, and system for producing, agglomerating, and collecting carbon black |
| US3211532A (en) * | 1962-03-12 | 1965-10-12 | Phillips Petroleum Co | Carbon black furnace |
| US3376111A (en) * | 1964-08-17 | 1968-04-02 | Phillips Petroleum Co | Production of high structure furnace carbon black |
| US3401020A (en) * | 1964-11-25 | 1968-09-10 | Phillips Petroleum Co | Process and apparatus for the production of carbon black |
| AU1991967A (en) * | 1967-04-05 | 1968-10-10 | Union Carbide Corporation | Manufacture of carbon black |
| DE1592864C3 (en) * | 1967-08-11 | 1975-05-22 | Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler, 6000 Frankfurt | Method of making FurnaceruB |
| US3615211A (en) * | 1968-01-12 | 1971-10-26 | Ashland Oil Inc | Method and apparatus for manufacture of carbon black |
| DE2106912C2 (en) * | 1970-02-19 | 1986-06-05 | Cabot Corp., Boston, Mass. | Device for the production of furnace black |
| US3663172A (en) * | 1970-06-29 | 1972-05-16 | Cities Service Co | Carbon black production process |
| US3734999A (en) * | 1971-10-21 | 1973-05-22 | Phillips Petroleum Co | Control of carbon black quality |
| JPS5413233A (en) * | 1977-07-01 | 1979-01-31 | Toshiba Corp | Non-volatile semiconductor memory unit |
| DE2944855C2 (en) * | 1979-11-07 | 1986-10-16 | Degussa Ag, 6000 Frankfurt | Process for the production of furnace blacks with a lowered structure |
| EP0175327B1 (en) * | 1984-09-21 | 1990-11-22 | Mitsubishi Kasei Corporation | Process for producing carbon black |
-
1990
- 1990-02-27 ES ES9000566A patent/ES2020713A6/en not_active Expired - Fee Related
- 1990-03-02 NL NL9000500A patent/NL9000500A/en not_active Application Discontinuation
- 1990-03-13 PE PE1990166237A patent/PE3991A1/en unknown
- 1990-03-20 CA CA002012627A patent/CA2012627C/en not_active Expired - Fee Related
- 1990-03-26 SE SE9001090A patent/SE9001090L/en not_active Application Discontinuation
- 1990-04-02 CZ CS901615A patent/CZ284688B6/en not_active IP Right Cessation
- 1990-04-04 AU AU52568/90A patent/AU625117B2/en not_active Ceased
- 1990-04-04 PL PL90284616A patent/PL163727B1/en unknown
- 1990-04-04 JP JP2088402A patent/JPH0749541B2/en not_active Expired - Fee Related
- 1990-04-04 DE DE4010776A patent/DE4010776A1/en not_active Withdrawn
- 1990-04-04 BR BR909001575A patent/BR9001575A/en unknown
- 1990-04-05 RO RO144735A patent/RO113148B1/en unknown
- 1990-04-05 BE BE9000384A patent/BE1002548A3/en not_active IP Right Cessation
- 1990-04-05 GB GB9007714A patent/GB2232409B/en not_active Expired - Fee Related
- 1990-04-05 TR TR90/0358A patent/TR24400A/en unknown
- 1990-04-05 PT PT93676A patent/PT93676A/en not_active Application Discontinuation
- 1990-04-05 HU HU902100A patent/HUT55316A/en unknown
- 1990-04-05 FR FR9004388A patent/FR2645542B1/en not_active Expired - Fee Related
- 1990-04-06 AR AR90316579A patent/AR245477A1/en active
- 1990-04-06 CN CN90102031A patent/CN1050855C/en not_active Expired - Fee Related
- 1990-04-06 KR KR1019900004712A patent/KR930005684B1/en not_active IP Right Cessation
- 1990-04-06 IT IT19959A patent/IT1240745B/en active IP Right Grant
Also Published As
| Publication number | Publication date |
|---|---|
| PL163727B1 (en) | 1994-04-29 |
| SE9001090D0 (en) | 1990-03-26 |
| IT1240745B (en) | 1993-12-17 |
| IT9019959A0 (en) | 1990-04-06 |
| GB2232409B (en) | 1992-10-14 |
| NL9000500A (en) | 1990-11-01 |
| JPH0749541B2 (en) | 1995-05-31 |
| HUT55316A (en) | 1991-05-28 |
| FR2645542B1 (en) | 1994-02-11 |
| CN1050855C (en) | 2000-03-29 |
| GB2232409A (en) | 1990-12-12 |
| JPH0362858A (en) | 1991-03-18 |
| KR930005684B1 (en) | 1993-06-24 |
| BE1002548A3 (en) | 1991-03-19 |
| GB9007714D0 (en) | 1990-06-06 |
| HU902100D0 (en) | 1990-07-28 |
| PT93676A (en) | 1990-11-20 |
| ES2020713A6 (en) | 1991-09-01 |
| SE9001090L (en) | 1990-10-07 |
| AR245477A1 (en) | 1994-01-31 |
| IT9019959A1 (en) | 1991-10-06 |
| BR9001575A (en) | 1991-04-30 |
| CA2012627A1 (en) | 1990-10-06 |
| AU625117B2 (en) | 1992-07-02 |
| CZ284688B6 (en) | 1999-02-17 |
| CA2012627C (en) | 1995-08-08 |
| RO113148B1 (en) | 1998-04-30 |
| PE3991A1 (en) | 1991-03-06 |
| TR24400A (en) | 1991-09-01 |
| KR900016395A (en) | 1990-11-13 |
| FR2645542A1 (en) | 1990-10-12 |
| AU5256890A (en) | 1990-10-11 |
| DE4010776A1 (en) | 1990-10-11 |
| CZ161590A3 (en) | 1998-11-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Font et al. | Kinetics of the pyrolysis of almond shells and almond shells impregnated with cobalt dichloride in a fluidized bed reactor and in a pyroprobe 100 | |
| RU2118974C1 (en) | Carbon black, composition containing carbon black | |
| US5879650A (en) | Tandem quench | |
| CN1050855C (en) | Tandem quench | |
| CN1125459A (en) | Process for producing carbon blacks | |
| CN104540929B (en) | Novel fuel composition | |
| US3175888A (en) | Apparatus for producing low structure carbon black | |
| JPH0153978B2 (en) | ||
| CN101165085A (en) | Carbon black for functional rubber component | |
| US4640822A (en) | Apparatus for producing bulk mesophase | |
| US3574547A (en) | High structure,high surface area carbon black | |
| AU8338887A (en) | A method for upgrading of waxy oils to products that can be used as light fuel oils, diesel fuel and other upgraded oils, the products so obtained and an application of the products as substitutes | |
| CN111393878A (en) | Method for producing carbon black by mixing raw oil | |
| CN1206032A (en) | Furnace process for producing conductive carbon black | |
| CN210657532U (en) | Carbon fiber precursor oiling device | |
| US3636148A (en) | Carbon black pelleting | |
| CN1580192A (en) | Methd for on-line monitoring coke burning-off process | |
| CN101712895B (en) | Compounds for fuel oil additives, preparation method and application thereof | |
| CN1030205C (en) | Synthetic diesel oil ued for cold area | |
| CN2547391Y (en) | Loop reactor with up and down double discharge functions | |
| CN1026493C (en) | Automatic feeding device for catalyst and its technology | |
| CN101733132B (en) | Catalyst system for producing diesel oil and method for producing diesel oil by using system | |
| CN210915941U (en) | Petroleum purification device | |
| US2806348A (en) | Bismuth triphenyl jet fuel compositions and process of using same | |
| GB2213477A (en) | Process for producing carbon black |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C15 | Extension of patent right duration from 15 to 20 years for appl. with date before 31.12.1992 and still valid on 11.12.2001 (patent law change 1993) | ||
| OR01 | Other related matters | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |