US20170037253A1 - Method of making carbon black - Google Patents

Method of making carbon black Download PDF

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Publication number
US20170037253A1
US20170037253A1 US15/229,608 US201615229608A US2017037253A1 US 20170037253 A1 US20170037253 A1 US 20170037253A1 US 201615229608 A US201615229608 A US 201615229608A US 2017037253 A1 US2017037253 A1 US 2017037253A1
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United States
Prior art keywords
carbon black
functional groups
functionalizing agents
particles
density
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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.)
Pending
Application number
US15/229,608
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English (en)
Inventor
Ned J. Hardman
Roscoe W. Taylor
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Monolith Materials Inc
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Monolith Materials Inc
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Publication date
Application filed by Monolith Materials Inc filed Critical Monolith Materials Inc
Priority to US15/229,608 priority Critical patent/US20170037253A1/en
Assigned to Monolith Materials, Inc. reassignment Monolith Materials, Inc. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HARDMAN, NED J., TAYLOR, ROSCOE W.
Publication of US20170037253A1 publication Critical patent/US20170037253A1/en
Pending legal-status Critical Current

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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
    • C09C1/565—Treatment of carbon black ; Purification comprising an oxidative treatment with oxygen, ozone or oxygenated compounds, e.g. when such treatment occurs in a region of the furnace next to the carbon black generating reaction zone
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • 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
    • C09C1/485—Preparation involving the use of a plasma or of an electric arc

Definitions

  • the field of art to which this invention generally pertains is methods for making use of electrical energy to effect chemical changes.
  • a method of making carbon black in a plasma process including subjecting the carbon black particles during and/or after formation to surface functionalizing agents in a controlled manner so as to impart a degree and/or density of functionalization onto the carbon black particles so as to adapt the particles to a particular pre-intended application.
  • Additional embodiments include: the method described above where the functional groups comprise oxygen containing functional groups; the method described above where the functional groups are introduced in the reactor, pelletizer, and/or dryer; the method described above where the functional groups comprise carboxylic acid and/or phenolic groups; the method described above where the density of the functionalization is up to about 30 micromol/m 2 ; the method described above where the carbon black particles are subjected to the functionalizing agents at temperatures up to about 500° C.; the method described above where the functionalizing agents contain one or more oxidizing agents; the method described above where the functionalizing agents contain one or more of H 2 , CO, CO 2 , O 2 , water vapor, nitrogen, N 2 O, NO 2 , ozone, ammonia, amines, methyl amines, hydroxides, H 2 O 2 , acids, HNO 3 , persulfates, hypohalites, halites, halates, perhalates, permanganates, carbonates, bleach, nitric acid, potassium permanganate, sulfur
  • Carbon blacks (CB) made with a particular surface chemistry can impart improved performance in rubber, composite, and other applications.
  • CB Carbon blacks
  • surface functionality can be controlled, carbon blacks with superior performance properties when compared to traditionally produced plasma blacks can be produced, e.g., even out performing some typical oil based furnace blacks.
  • the performance can be improved, for example, through the creation of oxygen functional groups at the carbon surface.
  • functional groups can inherently exist at the surface, for example, due to the existence of a time-temperature profile that can be characterized as having the CB in contact with tail gas composed of water, hydrogen, carbon monoxide, carbon dioxide and various other gases. These gases can be in intimate contact with the CB while the CB is still at high temperature (e.g., about 600° C.) which can enable the formation of surface functional groups.
  • RH relative humidity
  • Controlled oxidation can place specific groups at the surface.
  • the surface of furnace black might be comprised of 60:40 (mole equivalents) phenolic:carboxylic acid groups whereas with a controlled surface the ration could be comprised of 10:90 phenolic:carboxylic acid groups.
  • the carboxylic acid groups will typically be more reactive to rubber or SBR (styrene butadiene rubber) and more likely to form what is known as “bound rubber”. A larger amount of bound rubber could result in lower vibration, hysteresis, treadwear, and/or higher reinforcement, in addition to other possible benefits such as increased vehicle miles per gallon (mpg).
  • the typical atmosphere or tail gas of a furnace reactor that burns oil and possesses a water quench can comprise the following components (according to Donnet's Carbon Black , t2 nd Edition, pub. by Marcel Dekker, 1993, the disclosure of which is herein incorporated by reference (at page 46)).
  • the option exits to fine tune the surface chemistry of the black to the exact parameters of the desired application.
  • the operators of the furnace black process to take advantage of this process, they would have to either surface modify the current non-ideal particles or heat treat (to the point of full oxygen removal) to start with a non-oxygenated surface and then treat with reactive moieties to obtain the more optimized surface.
  • Equation 1 For a pressurized system the left hand side of equation 1 will be favored. CO and CO 2 are released from the surface at lower temperatures (about 250° C.-400° C.) and hydrogen is released at higher temperatures (about 800° C. and greater) where graphitization is taking place
  • the right hand side of equation 1 is favored and this can result in some amount of mass loss. Under pressure and in the correct atmosphere, the left hand side of equation 1 will be favored.
  • the pressurization of the vessel would involve raising the vessel to greater than atmospheric pressure but typically less than 10 bar.
  • the mixture of functional groups at the CB surface from the furnace process is simply the product as it is made. In that regard it is truly an uncontrolled, unoptimized product.
  • the tailoring of the groups is just simple not easily doable with the furnace process. With the process described herein, it is possible to tailor the surface of the CB to the specific application. It is further possible to tailor the performance of the CB within the application. For example, if carboxylic acid groups increase the bound rubber content in SBR polymer composites, then the ability to control the surface characteristics of the CB could allow for the tuning of the amount of bound rubber and thus fine tune or reduce the amount of road noise, vibration, or even improve the in mpg of the tire based upon this improved quality.
  • the functional surface groups at the CB surface could be 50/50 carboxylic acid and phenolic as made similar to what is produced in a conventional furnace process, while the process described herein could allow for tailoring of the surface functional groups at 90:10, 80:20, 70:30. 60:40, 50:50. 40:60. 30:70. 20:80. or 10:90, for example. This does not exclude the possibility of even much more detailed tuning of the surface groups. Some, or even most, of these types of composites would not be accessible through furnace black, gas black, lamp black, thermal black, etc. technology.
  • a more detailed surface composition could comprise epoxy, quinone, carboxylic acid, phenol, ether, anhydride, carbonyl, lactone, among other reactive groups at for instance a ratio of 5:5:35: 30:10: 5:5:5, for example.
  • the amount of functional groups on a typical furnace black could be one micromol/meter (m) 2 . While this has been used in the tire industry in the past, this is simply the amount that is obtained in a typically furnace black process.
  • m micromol/meter
  • a range of densities for example, anywhere from 0 to 30 micromol/m 2 can be obtained. This fine tuning capability can allow for the direct control of the interfacial surface energy between the rubber and particle and also allows for optimal bonding between these materials.
  • chemistry can similarly tailor surface chemistry for superior performance in other applications, reducing viscosity build in inks, improving dispersability in paints, superior color development in masterbatches, and perhaps improved conductivity in plastics through superior dispersion.
  • the chemistry can be tailored not just to an application, but to each compound or vehicle (liquid system) used within an application.
  • furnace black can be better tuned for the final application.
  • Three exemplary methods which can be used to treat the CB surfaces as described herein, can include, for example, the use of: 1—high temperatures and weak reagents; 2—low temperatures and strong reagents; 3—high temperatures and strong reagents.
  • the CB can be preheated and then doused with gas and steam.
  • the CB could be at room temperature or up to 400° C. when doused with reagent gases.
  • a list of less reactive gases is given below: H 2 , CO, CO 2 , O 2 , water vapor.
  • Nitrogen can also be present simply to control the amount of dousing. More reactive gases are listed below: N 2 O, NO 2 , ozone, ammonia, methyl amines, other general amines.
  • More reactive ingredients for the functionalization of the surface can include peroxides such as H 2 O 2 , acids such as HNO 3 , persulfates, hypohalites, halites, halates , or perhalates, permanganates, bleach, which is a hypohalite, is a low-cost example of one of these reagents. Combinations of these reagents can yield especially strong reaction conditions, for example, nitric acid in combination with hydrogen peroxide or potassium permanganate with sulfuric acid.
  • any diazonium salt-based methods include any diazonium salt-based methods. For instance, it may be advantageous to react the diazonium salt of sulfanilic acid with the CB surface in order to obtain sulfonate functionality.
  • This general diazonium based strategy could be used to corporate a wide variety of functional groups at the surface.
  • One advantage over the furnace black process is that the surface tuned by the methods described herein could have only the desired functionality and would not possess the inherent byproducts of the furnace process (e.g., random, uncontrolled deposition of oxygen groups at the surface).
  • any combination of the above could be used to design the optimum particle surface.
  • One of the methods to treat the surface could be to treat in a pressurized vessel to optimize the results based on equation 1.
  • Another method could be to add the reagents to the pelletizer and then dry at moderate temperatures (about 150° C.-250° C.). The latter method would be more amenable to stronger reagents listed above.
  • small amounts of strong reagents in a pressurized vessel might also be employed.
  • the hydrogen from the degas step can be partially removed and the hydrogen in the pores remain.
  • air can be added in such a way as to avoid explosive combinations of hydrogen and oxygen.
  • Another alternative in the case of slow diffusion of heat is to add a substance (reactive A) that will absorb to the surface of the CB followed by a second step of adding reactive B that will react exothermically with reactant A to provide a temperature activated surface and the final reactant.
  • reactive A reactive A
  • An example of this could be H 2 and O 2 to form H 2 O at between about 400° C. and 500° C. H 2 O would then proceed to react with the CB surface and provide oxygen functionality, or an intermediate between elemental hydrogen plus oxygen and the resulting water can react, e.g., an OH radical.
  • WSP water spreading pressure
  • R is the gas constant
  • T is the temperature
  • A is the N 2 surface area (SA)—(ASTM D6556) of the sample
  • H 2 O is the amount of water adsorbed to the carbon surface at the various RH's.
  • P is the partial pressure of water in the atmosphere and Po is the saturation pressure and g is gram.
  • the equilibrium adsorption is measured at various discrete RH's and then the area under the curve is measured to yield the WSP value.
  • Samples are measured at 25° C. using the 3Flex system from Micromeritics.
  • the region being integrated is from 0 to saturation pressure.
  • the d has it's normal indication of integrating at whatever incremental unit is after the d, i.e., integrating at changing natural log of pressure.
  • the process described herein is an in situ (in reactor) method of tuning the surface chemistry of CB to form ideal particles for the intended application.
  • the method itself can also be employed outside of the reactor, however, optimal efficiencies, e.g., such as cost savings, can be obtained within the reactor.
  • Dimensions such as WSP and density of groups at the surface are controlled. The ratios of the functional groups and the WSP tunability are of particular importance as this will enable performance in key applications such as the tire and rubber industry, among others. The implications are across all market segments which can be a crucial dimension in application performance.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Developing Agents For Electrophotography (AREA)
US15/229,608 2015-08-07 2016-08-05 Method of making carbon black Pending US20170037253A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US15/229,608 US20170037253A1 (en) 2015-08-07 2016-08-05 Method of making carbon black

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201562202498P 2015-08-07 2015-08-07
US15/229,608 US20170037253A1 (en) 2015-08-07 2016-08-05 Method of making carbon black

Publications (1)

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Country Status (7)

Country Link
US (1) US20170037253A1 (de)
EP (1) EP3331821A4 (de)
KR (1) KR20180094838A (de)
CN (2) CN118620417A (de)
CA (1) CA2995081C (de)
MX (1) MX2018001612A (de)
WO (1) WO2017027385A1 (de)

Cited By (20)

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Publication number Priority date Publication date Assignee Title
US10100200B2 (en) 2014-01-30 2018-10-16 Monolith Materials, Inc. Use of feedstock in carbon black plasma process
US10138378B2 (en) 2014-01-30 2018-11-27 Monolith Materials, Inc. Plasma gas throat assembly and method
US10370539B2 (en) 2014-01-30 2019-08-06 Monolith Materials, Inc. System for high temperature chemical processing
US10618026B2 (en) 2015-02-03 2020-04-14 Monolith Materials, Inc. Regenerative cooling method and apparatus
US20200305424A1 (en) * 2019-04-01 2020-10-01 Vulpes Agricultural Corp. Bifunctional plant promoter and preparation thereof
US10808097B2 (en) 2015-09-14 2020-10-20 Monolith Materials, Inc. Carbon black from natural gas
CN113292870A (zh) * 2021-05-31 2021-08-24 安徽德瑞新材料科技有限公司 一种纳米级绝缘炭黑的加工工艺
US11149148B2 (en) 2016-04-29 2021-10-19 Monolith Materials, Inc. Secondary heat addition to particle production process and apparatus
CN113652103A (zh) * 2021-07-09 2021-11-16 中国化学工业桂林工程有限公司 一种裂解炭黑的再生方法
US11304288B2 (en) 2014-01-31 2022-04-12 Monolith Materials, Inc. Plasma torch design
US11453784B2 (en) 2017-10-24 2022-09-27 Monolith Materials, Inc. Carbon particles having specific contents of polycylic aromatic hydrocarbon and benzo[a]pyrene
US11492496B2 (en) 2016-04-29 2022-11-08 Monolith Materials, Inc. Torch stinger method and apparatus
CN115537044A (zh) * 2022-09-19 2022-12-30 青岛黑猫新材料研究院有限公司 一种改性裂解炭黑及其制备方法和应用
US11665808B2 (en) 2015-07-29 2023-05-30 Monolith Materials, Inc. DC plasma torch electrical power design method and apparatus
US11760884B2 (en) 2017-04-20 2023-09-19 Monolith Materials, Inc. Carbon particles having high purities and methods for making same
US11926743B2 (en) 2017-03-08 2024-03-12 Monolith Materials, Inc. Systems and methods of making carbon particles with thermal transfer gas
US11939477B2 (en) 2014-01-30 2024-03-26 Monolith Materials, Inc. High temperature heat integration method of making carbon black
US11987712B2 (en) 2015-02-03 2024-05-21 Monolith Materials, Inc. Carbon black generating system
US12030776B2 (en) 2017-08-28 2024-07-09 Monolith Materials, Inc. Systems and methods for particle generation
US12119133B2 (en) 2015-09-09 2024-10-15 Monolith Materials, Inc. Circular few layer graphene

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CN108774415A (zh) * 2018-07-20 2018-11-09 宁波德泰化学有限公司 一种节能环保炭黑的制造方法
CN109233350A (zh) * 2018-10-09 2019-01-18 乌海黑猫炭黑有限责任公司 一种应用于化纤的色素炭黑的生产方法
CN109796791A (zh) * 2019-04-18 2019-05-24 山东耐斯特炭黑有限公司 一种电缆屏蔽料用导电炭黑的生产方法
CN111410855A (zh) * 2019-12-31 2020-07-14 宁波德泰化学有限公司 一种高表面活性/高亲水性分散型炭黑的制备方法
CN112724711A (zh) * 2021-01-11 2021-04-30 北京化工大学 一种高色素炭黑的制备方法
CN112940542B (zh) * 2021-01-21 2022-02-25 山东联科科技股份有限公司 一种具有电磁屏蔽性能的炭黑生产方法
CN113150579A (zh) * 2021-03-24 2021-07-23 茂名环星新材料股份有限公司 一种去除炭黑中杂质的方法及其应用

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US20140000488A1 (en) * 2011-03-10 2014-01-02 Tokai Carbon Co., Ltd. Method for producing aqueous dispersion of surface-treated carbon black particles and aqueous dispersion of surface-treated carbon black particles
WO2015051893A1 (de) * 2013-10-09 2015-04-16 Ralf Spitzl Verfahren und vorrichtung zur plasmakatalytischen umsetzung von stoffen
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Cited By (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11939477B2 (en) 2014-01-30 2024-03-26 Monolith Materials, Inc. High temperature heat integration method of making carbon black
US10138378B2 (en) 2014-01-30 2018-11-27 Monolith Materials, Inc. Plasma gas throat assembly and method
US10370539B2 (en) 2014-01-30 2019-08-06 Monolith Materials, Inc. System for high temperature chemical processing
US11591477B2 (en) 2014-01-30 2023-02-28 Monolith Materials, Inc. System for high temperature chemical processing
US10100200B2 (en) 2014-01-30 2018-10-16 Monolith Materials, Inc. Use of feedstock in carbon black plasma process
US11866589B2 (en) 2014-01-30 2024-01-09 Monolith Materials, Inc. System for high temperature chemical processing
US11203692B2 (en) 2014-01-30 2021-12-21 Monolith Materials, Inc. Plasma gas throat assembly and method
US11304288B2 (en) 2014-01-31 2022-04-12 Monolith Materials, Inc. Plasma torch design
US10618026B2 (en) 2015-02-03 2020-04-14 Monolith Materials, Inc. Regenerative cooling method and apparatus
US11987712B2 (en) 2015-02-03 2024-05-21 Monolith Materials, Inc. Carbon black generating system
US11998886B2 (en) 2015-02-03 2024-06-04 Monolith Materials, Inc. Regenerative cooling method and apparatus
US11665808B2 (en) 2015-07-29 2023-05-30 Monolith Materials, Inc. DC plasma torch electrical power design method and apparatus
US12119133B2 (en) 2015-09-09 2024-10-15 Monolith Materials, Inc. Circular few layer graphene
US10808097B2 (en) 2015-09-14 2020-10-20 Monolith Materials, Inc. Carbon black from natural gas
US11492496B2 (en) 2016-04-29 2022-11-08 Monolith Materials, Inc. Torch stinger method and apparatus
US11149148B2 (en) 2016-04-29 2021-10-19 Monolith Materials, Inc. Secondary heat addition to particle production process and apparatus
US12012515B2 (en) 2016-04-29 2024-06-18 Monolith Materials, Inc. Torch stinger method and apparatus
US11926743B2 (en) 2017-03-08 2024-03-12 Monolith Materials, Inc. Systems and methods of making carbon particles with thermal transfer gas
US11760884B2 (en) 2017-04-20 2023-09-19 Monolith Materials, Inc. Carbon particles having high purities and methods for making same
US12030776B2 (en) 2017-08-28 2024-07-09 Monolith Materials, Inc. Systems and methods for particle generation
US11453784B2 (en) 2017-10-24 2022-09-27 Monolith Materials, Inc. Carbon particles having specific contents of polycylic aromatic hydrocarbon and benzo[a]pyrene
US11653646B2 (en) * 2019-04-01 2023-05-23 Vulpes Agricultural Corp. Bifunctional plant promoter and preparation thereof
US20200305424A1 (en) * 2019-04-01 2020-10-01 Vulpes Agricultural Corp. Bifunctional plant promoter and preparation thereof
CN113292870A (zh) * 2021-05-31 2021-08-24 安徽德瑞新材料科技有限公司 一种纳米级绝缘炭黑的加工工艺
CN113652103A (zh) * 2021-07-09 2021-11-16 中国化学工业桂林工程有限公司 一种裂解炭黑的再生方法
CN115537044A (zh) * 2022-09-19 2022-12-30 青岛黑猫新材料研究院有限公司 一种改性裂解炭黑及其制备方法和应用

Also Published As

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CN108350280A (zh) 2018-07-31
CN118620417A (zh) 2024-09-10
MX2018001612A (es) 2018-05-28
EP3331821A1 (de) 2018-06-13
CA2995081C (en) 2023-10-03
CA2995081A1 (en) 2017-02-16
KR20180094838A (ko) 2018-08-24
EP3331821A4 (de) 2018-12-26
WO2017027385A1 (en) 2017-02-16

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