CZ2015570A3

CZ2015570A3 - Method for producing carbon black using extender fluid

Info

Publication number: CZ2015570A3
Application number: CZ2015-570A
Authority: CZ
Inventors: Chad J. Unrau; David O. Hunt; David M. Matheu; Serguei Nester
Original assignee: Cabot Corporation
Priority date: 2013-03-15
Filing date: 2014-02-26
Publication date: 2015-11-18
Also published as: CZ309755B6

Abstract

Řešení se týká způsobů výroby tuhy s využitím plnivové tekutiny nebo plnivových tekutin, stejně jako způsobů ovládání jedné nebo více vlastností částic tuhy s využitím plnivových tekutin a jiných technik.The present invention relates to methods for producing graphite using filler fluid or filler fluids, as well as methods for controlling one or more graphite particle properties using filler fluids and other techniques.

Description

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PV 2015-570 01-1430-15-Eng

Process for the Production of Graphite with the Use of Filling Fluid Technical Field [0001]

The invention relates to graphite and to methods for producing graphite.

The invention further relates to controlling the properties of one or more graphite particles.

BACKGROUND OF THE INVENTION In the production of graphite, variations in the control of the graphite production process and / or the arrangement of the device are usually required when the production line is converted to produce different graphite grades or to adapt to different types of processed raw material, these changes touching the continuous and / or efficient production line operation.

An operational setting that is effective to change the properties of the particles can be utilized when the change in particle properties (e.g., structure or surface area) of graphite is required for manufacturing reasons. 2

Such adjustments result in a cessation of the graphite production reactor, which may even include a total shutdown, whereby the jet nozzles used to feed the graphite feedstock to be processed are replaced in order to change the flow or dynamics of the fluid, which may provide hue or other properties. .

It should be noted that shutting down the reactor and replacing the nozzles can be time consuming and costly.

[0003]

In addition, in the production of graphite, some of the raw materials processed may be more problematic than others, such as the use of the raw coal-based feedstock as well as the resulting degree of nozzle tip wear.

This may also apply to other processed raw materials, which are considered as raw materials with a higher amount of small particles, such as ash, which may be problematic for the production of graphite and / or problematic in using small tip sizes for feedstock feedstocks due to clogging concerns or clogging.

In fact, clogging or clogging can be caused by particles coming from the raw material being processed, sintered, due to the potassium, water content, to mention at least several causes.

For purposes of this invention, the terms "jet nozzle" and "jet nozzle" are used for the purposes of this invention. or "nozzle" or "peak " the same part.

[0004]

It would also be desirable to improve the methods of making graphite by using a preheated feedstock as described in International Publication WO 2011/103015. In this known process, the preheated feedstock was used to obtain graphite advantageous properties as well as economically.

It would be advantageous to further refine this process in order to achieve much higher efficiency.

[0005]

Therefore, it would be advantageous to develop methods for producing graphite to provide one or more of the above tasks.

SUMMARY OF THE INVENTION It is therefore an object of the present invention to provide methods for controlling at least one feature of graphite particles, without any process interruption or reactor downtime.

It is a further object of the present invention to provide a method for controlling at least one feature of graphite particles without the need to replace nozzles at feed points for the feedstock being processed.

[0008]

It is a further object of the present invention to provide the possibility of further increasing the preheating temperatures of the feedstock to be processed in the production of graphite, by providing control for clogging or clogging caused by heat in the pipelines of the feedstock at elevated temperatures of the feedstock being processed.

[0009]

It is a further object of the present invention to provide a process for the production of graphite with the use of high particle content raw materials such as ash.

[0010]

Other features and advantages of the present invention will be set forth in part in the description which follows, and will be apparent from the description, or may be learned by practice of the present invention. The objects and other advantages of the present invention will be realized and attained by means of elements and combinations particularly pointed out and set forth in the description and appended claims.

In order to achieve these and other advantages, as well as in accordance with the objects of the present invention, as detailed below, the present invention relates in part to a process for producing graphite.

This method involves feeding a stream of heated gas to a graphite reactor.

The method further comprises mixing at least one filler fluid with at least one processed feedstock providing a solid to form a mixture of fluid and feedstock.

The mixing is preferably carried out such that at least one filler fluid enhances the momentum of the at least one graphite-providing feedstock in a direction that is substantially axial (within 10 ° of the axial direction) or axial to at least one feed point of the feedstock being processed into the production reactor. solid.

The mixture of fluid and feedstock is fed to at least one point for feeding the feedstock (preferably to several locations) to the graphite reactor.

The method further comprises mixing at least one feed and fluid feed through at least one feed point into a gas stream reactor to produce a heated gas stream to form a solid in the graphite reactor.

The method further comprises recovering the graphite in the reaction stream.

According to this method, the filler fluid may be chemically inert, and is preferably chemically inert to the feedstock to be treated.

[0012]

Instead of or in addition to mixing at least one filler fluid with at least one graphite-providing feedstock to form a mixture of fluid and feedstock, the mixture of fluid and feedstock can be generated in the reactor.

In other words, at least one filler fluid can be fed into the reactor, and at least one feedstock can be fed to the reactor in such a way that the feed points for each of these materials are arranged such that the filler fluid increases the momentum of the feedstock to be treated. .

The present invention further includes a method of controlling at least one property of graphite particles, such as structure and / or surface area.

The method comprises mixing at least one filler fluid with at least one solid treated feedstock to form a mixture of fluid and feedstock and supplying the fluid and feedstock mixture to a graphite reactor. The feed of the fluid / feed mixture is carried out in the form of one or more streams. 7 • · Μ • ·

The method further comprises controlling the amount of filler fluid present in the fluid mixture and the feedstock to control at least one property of the particles, such as hue.

Other particle properties may include a surface area (measured, for example, by BET, CTAB, and / or STSA (ASTM D6556)) or a structure such as OAN or DBP.

In the methods of the present invention, the graphite-providing feedstock may be formed or may contain processed high-content raw materials from 0.01% by weight to 0.5% by weight based on the weight of the raw material being processed, such as ash, since the invention provides possibilities for processing these types of processed raw materials without side effects, as will be described later.

[0015]

It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only, and are intended to provide further explanation of the present invention as claimed.

The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate aspects of the present invention, and together with the description, serve to explain the principles of the invention.

Similar reference numerals used in the drawings show similar features or features. BRIEF DESCRIPTION OF THE DRAWINGS [0017]

FIG. 1 to 5 are schematic illustrations of a portion of various types of furnace graphite reactors that can be used in the process of the present invention to produce graphite.

This graphite reactor is merely illustrative of the reactors that can be used in the present invention.

[0018]

FIG. 6 is a schematic representation of one exemplary embodiment of an injector showing injection of filler fluid into a ground feedstock prior to entering the graphite reactor and prior to primary ignition.

[0019]

FIG. Figures 7 and 8 are schematic illustrations showing possibilities for supplying filler fluid and raw material to be treated without prior mixing prior to entering the reactor, both as an annulus and as a side-by-side embodiment. Best Mode for Carrying Out the Invention The present invention relates to methods for producing graphite. The present invention also relates to methods for controlling at least one property of graphite particles. Further, the present invention also relates to the possibility of using high-particle processing raw materials without plugging any of the feed points into the reactor. Further, the present invention also relates to methods for further increasing the preheating temperatures of the feedstock to be treated in the production of graphite, by controlling the fouling or deposition of the feed of the feedstock due to heat at elevated temperatures of the feedstock being processed.

In the production of graphite, fuel is combusted to produce a stream of hot gases that flow at high speed through a transition region where the graphite feedstock provided is supplied and mixed with the hot gas stream.

The mixture is continued at a high speed into a hot reactor where the feedstock is pyrolyzed to obtain graphite particles, whereupon the reaction is quenched, the reactants are cooled, and the graphite product is collected. ·

In general, one aspect of the present invention relates to the production of graphite by mixing at least one filler fluid with at least one processed feedstock providing a feedstock prior to feed of the feedstock (or feedstock) to the reactor via one or more feed points. In the use of filler fluid, which will be described in more detail below, the filler fluid or filler fluid has the ability to provide various advantages that include one or more of the following advantages:

The ability to work with different types of graphite-providing raw materials, including those considered as high-particle (e.g., ash) raw materials, such as coal tar raw materials to produce graphite, the possibility of pre-heating the graphite feedstock to even a higher temperature than previously described, the possibility of controlling one or more graphite particle properties, the possibility of using lower pressures to feed the feedstock, and / or other advantages.

[0023]

The filler fluid may be a gas or a liquid. Preferred examples are gases.

The filler fluid may be chemically inert to the feedstock to be treated, preferably chemically inert to the feedstock to be treated.

The filler fluid may be at least one inert gas (e.g., argon, neon, helium, and the like).

The filler fluid may be nitrogen, alone or with other gases.

The filler fluid may be steam, water, air, carbon dioxide, carbon monoxide, hydrogen, residual graphite gases, natural gas, or nitrogen, one or more inert gases, or any combination thereof.

Generally, the gas or liquid has a purity of at least 95% by weight (for example at least 97% by weight, at least 98% by weight, at least 99% by weight, at least 99.5% by weight or at least 99.9% by weight) of the gas or liquid.

For example, if nitrogen (alone or with other gases or liquids) is used, nitrogen gas is at least 95% by weight gas.

[0024]

The filler fluid, when mixed with at least one graphite-providing feedstock to form a mixture of fluid and feedstock, may optionally be evenly distributed in the graphite-providing feedstock to be treated.

Mixing the filler fluid or filler fluids with the at least processed solids feedstock results in a mixture of fluid and feedstock, wherein the filler fluid is distributed (uniformly or non-uniformly) in the feedstock to be treated.

Before mixing the filler fluid with the graphite-providing feedstock to be treated, the graphite-providing feedstock can be comminuted or at least partially comminuted.

Optionally, the filler fluid is not utilized as a grinding agent for the graphite-providing feedstock of the present invention.

Preferably, the filler fluid provides momentum for the graphite feedstock being treated, after it has been mixed with the graphite-providing feedstock. The term "momentum" refers to momentum as understood in fluid mechanics. Optionally, the filler fluid upon mixing with the treated feedstock feedstock provides momentum to form a columnar stream of the fluid / feedstock mixture when the mixture leaves the nozzle and enters the graphite reactor.

The filler fluid has the ability to control the momentum of the feedstock being processed. 13 • ·

The fluid / feedstock mixture is directed in the injector so that the forward momentum of the fluid / feed mixture mixture after entering the reactor continues in a direction that is axial to the centerline of the injector (or substantially axial to the center axis of the injector, e.g., within 10 ° axial with respect to the center axis).

The fluid / feed mixture is further guided preferably to be perpendicular (or substantially perpendicular, i.e. within 10) to the primary fire or combustion stream, and / or is preferably perpendicular (or substantially perpendicular, i.e. at 10 °) to the wall of the graphite reactor.

Optionally, the mixture of fluid and feedstock or inverter used to inject a mixture of fluid and feedstock may be at any angle relative to the primary fire or combustion stream (e.g., perpendicular (90 °), substantially perpendicular (80 ° to 110 °), or below) other angles (such as from 20 ° to 79 °, 20 °, 30 °, 40 °, 45 °, 50 °, 55 °, 60 °, 65 °, 75 ° and the like)).

One example of mixing a filler fluid and a graphite-providing feedstock is shown in Figure 6.

As shown in Fig. 6, the graphite processing material 100 being processed enters the opening 102 and exits the opening 102 as a pulverized graphite processing material 104.

The filler fluid 106 is fed through channel 108 and is mixed with the pulverized graphite processing material 104 to form fluid mixture 110 and material to be processed.

The composition 110 has increased momentum compared to the momentum that existed prior to feeding the filler fluid.

This fluid / material mixture 110 leaves the injector through a nozzle or channel 112 in the reactor wall 117 as a columnar stream of fluid / material mixture having high momentum 114, penetrating into the combustion stream or primary fire 116 of high speed.

Thus, preferably according to the invention, mixing of at least one filler fluid with at least one processed graphite material to form a fluid / material mixture is such that at least one filler fluid provides an increase in momentum of at least one processed material to produce graphite in a direction that is axial or substantially axial with respect to the at least one feed point of the material being processed into the graphite reactor.

[0026]

The amount of filler fluid or filler fluids that is mixed with the graphite-providing feedstock is adjustable.

The amount of filler fluid that is mixed with the graphite-providing feedstock can be adjustable when the process is performed on-line and graphite is produced.

In other words, the amount of filler fluid can be changed "on the go". • 15 • * 9 · ψ * * ··· ·

Thus, since the amount of filler fluid can be mixed with the feedstock providing the graphite providing in an adjustable manner, this can be done without interrupting operation and shutting down the reactor.

Thus, continuous graphite production can be maintained even if the reactor conditions are set to obtain graphite of different quality or to optimize the quality of graphite produced or to adjust or change the quality of graphite produced and / or in other settings that are carried out in the process or reactor during manufacture solid.

[0027]

Generally, the filler fluid may be fed to the feedstock provided to provide a solid at any pressure, but generally high pressures are preferred to provide the desired mixing of the filler fluid with the graphite-providing feedstock, especially when the filler fluid is gas.

For example, suitable pressures may be from about one pound per inch to about 350 pounds per square inch, or from about 50 pounds per square inch to about 175 pounds per square inch, or from about 50 pounds per inch to about 200 pounds per inch. a square inch or more, or from about 100 pounds per square inch to about 200 pounds per square inch or higher.

16 · 16

These pressures, as well as other pressures, can be used to feed the filler fluid to the graphite-providing feedstock.

The pressure may be sufficient to penetrate the graphite-providing feedstock to form a mixture of fluid and feedstock, preferably when the filler fluid is uniformly distributed in the graphite-providing feedstock being processed.

[0029]

Any amount of filler fluid may be present in the fluid / feedstock mixture.

For example, the filler fluid may be present in the fluid / feedstock mixture in an amount of from about 0.1 wt% to about 400 wt% (or higher) based on the weight of the graphite-providing feedstock being processed.

Other amounts include, for example, from about 0.1% by weight to about 100% by weight or more, based on the feedstock being processed, or from about 5% by weight to about 15% by weight or more, based on the feedstock being processed or from about 0.1 to .50 to about 50

about 0% by weight or more, based on the feedstock being processed, or from about 1% by weight to about 40% by weight or more, based on the feedstock being processed.

The supply of the fluid mixture and the feedstock can be carried out in the form of one or more streams.

Based on the type of filler fluid and / or the amount of filler fluid, the flow of the fluid / feedstock stream into the heated gas stream can be adjusted.

As mentioned above, by using a mixture of fluid and feedstock that is fed in the form of one or more streams, the flow of the fluid and feedstock stream into the heated gas stream can be adjusted based on the amount of filler fluid and / or the type of filler fluid. any change in the nozzle and / or without any need to interrupt the process or shut down the graphite reactor.

[0031]

As an option, the filler fluid may be mixed with the feedstock to be treated to provide a solid at a point which is located upstream of the point of introduction of the fluid / feedstock mixture into the graphite reactor.

The fluid may be fed in such a way that the fluid and the feedstock are mixed together prior to exiting the injector or nozzle. 18

The filler fluid may be mixed with the feedstock provided to give the graphite at a location that is more than or less than 0.5 inches, such as at least 0.75 inches, at least 1 inch, at least 2 inches, at least 4 inches, or at least 6 inches before the reactor feed point.

[0032]

As an option, the filler fluid may be mixed with the feedstock provided to give the graphite after the respective feedstock to a graphite reactor.

In other words, the filler fluid can be fed to the graphite reactor separately and independently of the feedstock provided.

Any geometry for obtaining a separate feed of the filler fluid and the feedstock feedstock provided to the reactor such that the two fluids are adjacent to each other or contacting each other in the reactor can be utilized.

For example, as shown in FIGS. 7 and 8, the feed of the filler fluid and the graphite-providing feedstock separately may be accomplished by means of a conduit having a hollow structure with an annulus so that one of the liquids surrounds the second fluid. 19

Another geometry that can be utilized is the arrangement of the fill points for the filler fluid and the feedstock providing the stiffener. In such a design, one of the inlet locations may be located in front of the second supply point at a slight distance, for example, one-half inch or one inch or more.

If the filler fluid and the graphite-providing feedstock are fed to the reactor separately, the geometry is such that the filler fluid contacts the liquid-treated feedstock providing the solid, wherein the filler fluid increases the momentum of the feedstock feed fluid to the combustion stream (or cross-stream).

There is no geometry limitation that can be used to provide this double separate feed of the filler fluid and the graphite-providing feedstock.

Again, one or more feed points may be used, for example around the reactor periphery, such as a neck region.

[0033]

For each feed point of the graphite-providing feedstock to be processed, either a premixing of the filler fluid with the feedstock to be treated can be provided prior to feeding the feedstock to the graphite reactor and / or the respective filler feed point for each feed point of the feedstock provided .

[0034]

The manner in which a mixture of fluid and feedstock is fed to a graphite reactor, such as at a process transition point, may be in the form of one or more streams or jet nozzles, or a combination thereof, or alternatively one or more lances.

When jet nozzles are used, these jet nozzles are typically positioned in a radial position around the reactor periphery, for example, as shown in Figure 1.

When a lance is used, the lance is typically located more in the axial center of the reactor site.

[0035]

According to the present invention, for any process, the graphite-providing feedstock may comprise or contain any liquid hydrocarbon having a specific gravity of from about 0.9 to about 1.5 or greater (such as from 0.9 to 1.3, or from 1 to 1). , 2 or the like) or any combination thereof.

The graphite-providing feedstock may have a boiling point of from about 160 ° C to about 600 ° C, for example from about 160 ° C to about 500 ° C, or from about 200 ° C to about 450 ° C, or

from about 215 ° C to about 400 ° C and the like. 21 ·· · · · ·

The graphite-providing feedstock can be any commonly known graphite-providing feedstock to form a solid.

For example, any hydrocarbon material may be utilized.

A suitable feedstock to be treated may be any hydrocarbon feedstock providing a graphite that is readily volatile under reaction conditions.

For example, unsaturated hydrocarbons such as acetylene, olefins such as ethylene, propylene, butylene, aromatics such as benzene, toluene and xylene, certain saturated hydrocarbons, and other hydrocarbons such as kerosines, naphthalenes, terpenes, ethylene tars, aromatic cyclic fractions, aromatic cyclic fractions may be used. etc.

[0036]

The graphite-providing feedstock that can be processed using the present invention may generally include any hydrocarbon liquid or oil-treated feedstock useful for graphite production. 22

Suitable liquid feedstocks include, for example, unsaturated hydrocarbons, saturated hydrocarbons, olefins, aromatics, and other hydrocarbons such as kerosines, naphthalenes, terpenes, ethylene tars, coal tars, cracking residues, and aromatic cyclic fractions, or any combination thereof.

For example, the feedstocks to be treated may include decanted oil, coal tar product, ethylene cracking residues, oil-containing asphaltenes, or any combination thereof.

The type of raw material being processed can affect clogging or settling behavior.

The chemical composition may vary within the different types of raw material being processed and / or within the raw material being processed. 23

For example, decanted oil, coking oil, coal tar, and ethylene cracking residues can be deposited at various temperatures in excess of 300 ° C based on tests and laboratory tests.

For example, ethylene cracking residues (ECRs) may contain high amounts of asphaltenes.

Other types of processed materials may also contain asphaltenes and / or have a chemical composition that causes other fouling or settling mechanisms.

[0037]

The content of asphaltenes in the feedstock can be, for example, from 0 wt% to about 30 wt%, or at least about 0.5 wt%, or at least about 1 wt%, or at least about 2 wt%, or at least about 3 wt%, or from about 1 wt% to about 10 wt%, from about 2 wt%, to about 7.5 wt%, or from about 2.5 wt% to about 5 wt%, based on the total weight of the feedstock being processed. ···· 24

The feedstock to be treated may have an initial boiling point of, for example, from about 160 ° C to about 500 ° C, or from about 180 ° C to about 450 ° C, or from about 200 ° C to about 400 ° C, or from about 225 ° C to about 350 ° c.

The initial boiling point refers to the temperature at which the first component of the feedstock evaporates.

The feedstock to be treated may have a boiling point of the central range, for example, from about 380 ° C to about 800 ° C, or from about 400 ° C to about 500 ° C, or from about 425 ° C to about 470 ° C, or from about 440 ° C. to about 460 ° c.

The boiling point of the center range refers to the temperature at which 50% of the components of the feedstock evaporated.

The feedstock to be treated may have a final boiling point of, for example, from about 600 ° C to about 900 ° C, or from about 625 ° C to about 725 ° C, or from about 650 ° C to about 700 ° C, or from about 670 ° C to about 690 ° C.

The final boiling point refers to the temperature at which 100% of the raw material components were evaporated. • 25 • ·

Other boiling points may be applied, both initial, mid-range and / or final, depending on the choice and chemical composition of the feedstock being processed.

[0038]

The methods of the present invention can be used in furnace reactors to produce graphite with adaptations and modifications disclosed herein.

The methods of the invention can be practically applied, for example, to a modular or modular furnace graphite reactor, also referred to as "stepped".

Stepped furnace reactors that have been modified for practical use have been adapted to the present invention or are described, for example, in U.S. Pat. Nos. 3,922,335, 4,383,973, 5,190,739, 5,877,250, 5,904,762, 6,153,684, US 6,156,837, US 6,403,695, and US 6,485,693 B1, all of which are incorporated herein by reference in their entirety.

[0039]

With respect to the hot gas stream (or the hot gas stream) that is mixed with the graphite-providing feedstock to be treated, the hot gas stream can also be considered as a stream of hot combustion gases or heated gases that can be formed by contacting the solid, liquid and / or hot gases. or a gaseous fuel with a suitable oxidant stream, such as, but not limited to, air, oxygen, air / oxygen mixtures, or the like.

Alternatively, the stream of preheated oxidant may flow without the addition of liquid or gaseous fuel. Examples of fuel suitable for use in contacting with the oxidant stream to produce hot gases include any readily ignitable gas, vapor, or liquid streams, such as natural gas, hydrogen, carbon monoxide, methane, acetylene, alcohol, and the like. «

recycled residual gas or kerosene.

In general, it is preferred to use fuels having a high content of carbon-containing components, especially hydrocarbons.

The air to fuel ratio used to produce the graphite of the present invention may be from about 0.7: 1 to infinity, or from about 1: 1 (stochiometric ratio) to infinity.

In order to promote the formation of hot gases, the oxidant stream can be preheated.

The heated gas stream is essentially formed by ignition or combustion of the fuel and / or oxidant. Thus, temperatures such as from about 1,000 ° C to about 3,500 ° C can be achieved in the case of a heated gas stream.

In the present invention, the penetration of the feed stream of the feedstock can be adjusted by the filler fluid.

For example, the filler fluid has the ability to affect the flow rate or critical velocity, or both one or more streams of fluid and feedstock stream, as it is fed through one or more feed points to the reactor. The higher the amount of filler fluid, the higher the constricted flow rate or the critical mix rate (where the constricted flow rate and the critical velocity relate to the sound velocity for such a mixture). , and therefore there is a more pronounced leakage of current into the stream of heated gas.

[0041]

Another advantage of the present invention is the ability to increase total graphite yield with the use of filler fluid.

According to the present invention, more graphite can be produced using the same amount of feed fluid. For example, the yield may be increased by at least 1%, at least 2%, or at least 5% if the% yield is based on the weight% of graphite. Yields can be further enhanced by utilizing the preheating option (as described) of the filler fluid, the graphite-providing feedstock, or both.

[0042]

A further advantage of the present invention lies in the fact that large sizes of holes or nozzles can be used. In some graphite production processes, large sizes of holes or nozzles are used due to the presence of particles in the graphite-providing material.

Large sizes of holes or nozzles are used to prevent nozzle clogging due to particles present. • »· ·· · *

However, if large nozzle sizes are utilized, sufficient or good penetration of the feedstock fluid into the combustion gas stream of heated gases can be prevented due to reduced pressure and feed rate of the feedstock being processed.

However, in the case of the present invention, the use of filler fluid provides the possibility to increase the momentum of the fluid of the feedstock, even if it is fed from large-sized nozzles, so that penetration is achieved at the same level as using small nozzle sizes to achieve the desired graphite formation.

[0043]

As an option, the graphite-containing feedstock that is mixed with the filler fluid can be heated prior to mixing with the filler fluid. In other words, the graphite-providing feedstock can be preheated. The preheating of the feedstock and the associated techniques may be as disclosed in International Application WO 2001/103 105, the entire contents of which are incorporated herein by reference.

[0044]

According to the present invention, as an option, the graphite-providing feedstock prior to mixing with the filler fluid can be heated to a temperature greater than 300 ° C, or from about 360 ° C to about 850 ° C or higher, or from about 400 ° C to about 600 ° Or other temperatures.

[0045]

According to the invention, as an option, the filler fluid prior to mixing with the treated feedstock providing the graphite can be heated to a temperature of at least 100 ° C, at least 300 ° C, or at least 500 ° C, or at least 750 ° C, or at least 1000 ° C, or at least 1200 ° C or other temperatures.

[0046]

As an optional feature of the present invention, the filler fluid and the graphite-providing feedstock prior to mixing together may be pre-heated separately to the same or different temperature. 31 31

Preheating temperatures may be within the above ranges, and may be about preheating to a temperature of greater than 300 ° C, or from about 360 ° C to about 100 ° C. 850 ° C or higher, or

from about 400 ° C to about 600 ° C for a graphite-yielding feedstock and / or at least 100 ° C, or at least 300 ° C, or at least 500 ° C, or at least 750 ° C, or at least 1000 ° C , or at least 1200 ° C, or other temperatures for the filler fluid.

As a further optional option, the mixture of fluid and feedstock may optionally be heated to a higher temperature, either with or without preheating the feedstock providing the graphite and / or filler fluid.

[0047]

As an option, the graphite-providing feedstock can be heated to a first temperature, such as at least 300 ° C, for example from 300 ° C to about 850 ° C, prior to mixing with the filler fluid to form a mixture of fluid and feedstock, after which it can be The mixture of fluid and feedstock is further heated to a second temperature which is higher than the temperature of the preformed graphite-providing feedstock itself, before being mixed with the filler fluid.

This heating of the fluid / feedstock mixture to a higher temperature may be at least 50 ° C higher than the preheated feedstock, for example at least 75 ° C higher or at least 100 ° C higher or the like.

As an option, the graphite-providing feedstock may be heated or preheated to a first temperature prior to mixing with the filler fluid to form a mixture of fluid and feedstock, and may be further heated to a second temperature that is higher than the first temperature, e.g. 950 ° C.

[0048]

The method may include quenching or cooling the graphite in the reaction stream.

The graphite in the reaction stream may be quenched or cooled in one or more regions.

For example, in FIG. 2, in a quenching point of quenching region 14, quenching fluid is injected, which may contain water and which can be used to completely or substantially complete pyrolysis of the processed graphite-yielding feedstock, or only to partially cool the feedstock without stopping pyrolysis, whereupon followed by a secondary quenching (not shown) used to stop the pyrolysis of the graphite-providing feedstock. 33 ····

Further extinguishing steps that are common in graphite production can be utilized in the methods of the invention.

After quenching the mixture of hot combustion gases and the treated solids providing the graphite, the cooled gases pass further downstream into any conventional cooling and separating means, obtaining graphite.

Separation of the graphite from the gas stream is readily accomplished by known means such as a precipitation device, a cyclone separator or a bag filter.

With regard to the complete extinguishing of the reactions for forming the final graphite product, any known means for quenching the flow downstream of the second graphite-providing feedstock may be utilized and known to those skilled in the art.

For example, the extinguishing fluid may be injected, wherein the fluid may be water or other suitable fluid to stop the chemical reaction.

[0049]

As described above, and as will be described in more detail below, one method may include supplying a stream of heated gases to a graphite reactor. • · 34

The method further optionally comprises supplying at least one graphite-providing feedstock having a first temperature that is less than the desired preheating temperature, such as less than 300 ° C, or less than 275 ° C, such as from 40 ° C to 274 ° c, from 50 ° C to 270 ° C, from 70 ° C to 250 ° C, from 60 ° C to 200 ° C, from 70 ° C to 150 ° C, and the like, to at least one heater (for example at least two heaters, at least three heaters and the like, wherein the heaters may be the same or different from each other).

The at least one filler fluid may be mixed with the feedstock to be treated to provide the graphite at any point before and / or after the feedstock feedstock being fed to the reactor.

Ideally, the greatest advantages are obtained when the filler fluid is mixed prior to feeding into the reactor.

This can be done directly before or at any point after the heating stage described herein for preheating or before the heating stage. · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · ·· ······

The temperature of the feedstock entering the at least one heater is lower than the target preheating temperature or temperature range.

The feedstock to be pre-heated may, as an option, be at a first rate of at least about 0.2 m / s, such as at least about 0.4 m / s, at least about 0.6 m / s, at least about 0.8 m / s, at least about 1 m / s, at least about 1.1 m / s, at least about 1.6 m / s, such as from 0.2 m / s to 4 m / s, from 1.1 m / s to 3 m / s alike.

Other speeds may be employed, provided that the other process conditions are selected to control fouling and / or sintering in the heater or in the heater and in the feed lines to the reactor.

[0050]

The method may include preheating at least one feedstock to provide a solid in at least one heater to a second temperature that is greater than about 300 ° C, for example at least 350 ° C, at least 360 ° C, at least 400 ° C, at least 450 ° C, at least 500 ° C, such as from 300 ° C to 850 ° C, or from 360 ° C to 800 ° C, from 400 ° C to 750 ° C, from 450 ° C to 700 ° C and the like, to form a pre-heated graphite-yielding feedstock wherein (a) the at least one graphite-providing feedstock has a velocity in at least one heater that is at least 0.2 m / s, wherein the velocity is calculated based on the raw material being processed, measured at 60 ° C and 1 atm, and based on the smallest cross-sectional areas of the feedstock present in the at least one heater.

Since it may be very difficult to measure the speed of the feedstock at such an elevated temperature; for purposes of this invention, the rate cited herein is based on these specific measurement conditions.

Wherever a smaller diameter or smallest cross-sectional area is present in an existing heater, this minimum cross-sectional area is used to determine the speed cited herein for purposes of the present invention.

A number of heaters have the same diameter across the entire heater, but if several diameters or cross-sectional areas are present in the heater or heaters, this condition is determined.

The speed is based on the minimum cross-sectional area.

· Ί ί ί ί ί ί ί ί ί ί ί

The actual velocity through the feedstock heater may generally be faster than the velocity measured at 60 ° C and 1 atm.

[0051]

According to the method, the graphite-providing feedstock may have a first residence time of the feedstock being processed in the heater, which is less than about 120 minutes, such as less than 100 minutes, less than 80 minutes, less than 60 minutes, less than 40 minutes, less than 30 minutes. minutes, less than 20 minutes, less than 10 minutes, such as from one second to 119 minutes, from 5 seconds to 115 minutes, from 10 seconds to 110 minutes, from 30 seconds to 100 minutes, from one minute to 60 minutes, from 5 seconds minutes to 30 minutes, and the like.

[0052]

The method may comprise supplying a preformed graphite-providing feedstock (optionally pre-blended with the filler fluid) to at least one feed point of the feedstock being processed into a graphite reactor (e.g., at least one or two or three or four feed points of the feedstock being processed), wherein the preheated feedstock providing the graphite, the second residence time of the raw material being processed, measured from leaving the heater or heaters directly upstream of the graphite reactor feed point, is less than about 120 minutes, e.g., less than 100 minutes, less than 80 minutes, less than 60 minutes, less than 40 minutes minutes, less than 30 minutes, less than 20 minutes, less than 10 minutes, such as from one second to 119 minutes, from 5 seconds to 115 minutes, from 10 seconds to 110 minutes, from 30 seconds to 100 minutes, from one minute to 60 minutes, from 5 minutes to 30 minutes, and the like.

The first residence time of the feedstock to be treated and the second residence time of the feedstock to be processed in its combination is preferably 120 minutes or less, for example less than 100 minutes, less than 80 minutes, less than 60 minutes, less than 40 minutes, less than 30 minutes , less than 20 minutes, less than 10 minutes, such as from one second to 119 minutes, from 5 seconds to 115 minutes, from 10 seconds to 110 minutes, from 30 seconds to 100 minutes, 39 minutes from 60 minutes, from 5 minutes to 30 minutes, and the like.

For example, as shown in the drawings, the second residence time of the raw material being processed may be, for example, the time when the raw material being processed leaves the heater 19 of FIG. 2 or the heater 22 of FIG. Fig. 2 and Fig. 3.

The combination of the first residence time of the raw material to be processed and the second residence time of the raw material to be processed will result in the total residence time of the raw material being processed.

[0053]

As an option, if the feed of the feedstock to the heater has roughly the same cross-section as that of the heater, the graphite feedstock processed may have a heater or heater speed that is about the same or greater, e.g. 2% greater, at least 3% larger, at least 4% larger, at least 5% larger, at least 7% larger, at least 10% larger, at least 100% larger, at least 200% greater than 1% % to 200% larger, or 20% to 100% larger, and the like than the first speed at the entrance to the heater or heaters.

[0054]

The process of the present invention may include pressurizing or increasing the pressure of the feedstock to be treated or the feedstock being treated to provide the solid.

The method may include pressurizing or applying pressure to the feedstock being processed or the solids to be treated, such that pre-heating the graphite-providing feedstock prevents the formation of vapor film in the at least one heater or prior to feeding to the graphite reactor.

The process of the present invention may include pressurizing the feedstock or graphite feedstock being treated to provide a pressure of, for example, greater than about 10 bar prior to entering at least one heater that preheats the feedstock providing the graphite.

This pressure may be at least 15 at least 20 at least 30 at least 40 as from 10 at 15 bar from 20 bar to 25 bar bar, bar, bar, bar to 180 bar or more to 150 bar to 125 bar to 100 bar. bars.

[0055]

According to the present invention, the method of producing graphite may include feeding a stream of heated gas to the graphite reactor.

The method further comprises supplying a graphite-providing feedstock having a first temperature that is less than the target preheat temperature of the feedstock, such as less than 300 ° C or less than 275 ° C, for example from 40 ° C to 274 ° C, from 50 ° C to 270 ° C, from 70 ° C to 250 ° C, from 60 ° C to 200 ° C, from 70 ° C to 150 ° C, and the like, to a heater or heaters at a first pressure that is greater than 10 bar.

This pressure may be at least 15 at least 20 at least 30 at least 40 as from 10 at 15 bar from 20 bar to 25 bar bar, bar, bar, bar to 180 bar or more to 150 bar to 125 bar to 100 bar bars.

42 • ·

The method may include preheating at least one graphite-providing feedstock in a heater or heaters (e.g., at least two heaters, at least three heaters, and the like, wherein the heaters may be the same or different from each other) to a second temperature that is greater than about 300 ° C, for example at least 350 ° C, at least 360 ° C, at least 400 ° C, at least 450 ° C, at least 500 ° C, such as from 300 ° C to 850 ° C, or from 360 ° C to 800 ° C or from 400 ° C to 750 ° C, from 450 ° C to 700 ° C, and the like to form a pre-heated graphite-providing feedstock, wherein (a) the graphite-providing feedstock has a second pressure in at least one heater that is roughly the same or lower, for example at least 1% lower, at least 2% lower, at least 3% lower, at least 5% lower, at least 7% lower, at least 10% lower, at least 15% lower, 43

at least 20% lower, such as 1% to 75% lower, or 3% to 20% lower, and the like than the first pressure, wherein (b) the graphite-providing feedstock has a first residence time of the raw material being processed in the heater of less than about 120 minutes, such as less than 100 minutes, less than 80 minutes, less than 60 minutes, less than 40 minutes, less than 30 minutes, less than 20 minutes, less than 10 minutes, such as from one second to 119 minutes, from 5 seconds within 115 minutes, from 10 seconds to 110 minutes, from 30 seconds to 100 minutes, from one minute to 60 minutes, from 5 minutes to 30 minutes, and the like.

[0057]

As mentioned above, in any of the methods described herein, either sooner or later, the at least one filler fluid may be mixed with the preheated feedstock to provide graphite at any location (prior to preheating, during preheating, 44).

and / or after preheating, and / or before and / or after introduction into the graphite reactor.

[0058]

The method may include supplying a pre-heated graphite-providing feedstock to at least one feed point to feed the feedstock to the graphite reactor, wherein the pre-heated graphite-yielding feedstock has a second residence time of the feedstock from the outlet of the at least one heater to the reactor feed point of the graphite lesser more than about 120 minutes, such as less than 100 minutes, less than 80 minutes, less than 60 minutes, less than 40 minutes, less than 30 minutes, less than 20 minutes, less than 10 minutes, such as from one second to 119 minutes, from From 5 seconds to 115 minutes, from 10 seconds to 110 minutes, from 30 seconds to 100 minutes, from one minute to 60 minutes, from 5 minutes to 30 minutes, and the like, with the first residence time of the raw material being processed and the second residence time of the raw material being processed. the combination is 120 minutes or less, such as less than 100 mi less than 60 minutes, less than 40 minutes, less than 30 minutes, less than 20 minutes, less than 10 minutes, such as from one second to 119 minutes, from 5 seconds to 115 minutes minutes, from 10 seconds to 110 minutes, from 30 seconds to 100 minutes, from one minute to 60 minutes, from 5 minutes to 30 minutes, and the like.

The present invention may relate to a process for producing graphite, which comprises supplying a stream of heated gases to a graphite reactor.

The method further comprises supplying at least one graphite-providing feedstock having a first temperature that is less than the target preheating temperature of the feedstock, such as less than 300 ° C or less than 275 ° C, for example from 40 ° C to 274 ° C. from 50 ° C to 270 ° C, from 70 ° C to 250 ° C, from 60 ° C to 200 ° C, from 70 ° C to 150 ° C, and the like, 46 ° to at least one heaters (e.g., at least two heaters, at least three heaters, and the like, wherein the heaters may be the same or may differ from each other), at a first pressure greater than 10 bar.

As an optional heater, the first one is about 0.2 m / s, for example at least about 0.4 m / s, at least about 0.6 m / s, at least about 0.8 m / s, at least about 1 m / s, at least about 1.1 m / s, at least about 1.6 m / s, such as from 0.2 m / s to 2 m / s, from 0.4 m / s to 1.8 m / s, and the like.

The speed at entry to speed may be at least

The method comprises preheating the graphite-providing feedstock in the preheater or preheaters to a second temperature that is greater than about 300 ° C, for example at least 350 ° C, at least 360 ° C, at least 400 ° C, at least 450 ° C, at least 500 ° C, as from 300 ° C to 850 ° C, or from 360 ° C to 800 ° C, from 400 ° C to 750 ° C, from 450 ° C to 700 ° C, and the like, 47 to form a pre-heated, graphite-providing feedstock wherein (a) the graphite-providing feedstock being processed has a velocity in the heater or heaters which is at least 0.2 m / s, the velocity being calculated based on the density of the feedstock being processed, measured at 60 ° C and at 1 atm, and the smallest cross-sectional area of the feedstock present, present in the at least one heater, and (b) at least one graphite-providing feedstock has a second heater or heater pressure that is roughly the same n or lower, for example at least 1% lower, at least 2% lower, at least 3% lower, at least 5% lower, at least 7% lower, at least 10% lower, at least 15% lower, at least 20% lower lower, such as 1% to 25% lower, or 3% to 20% lower, and the like than the first pressure, wherein the pressure can be calculated based on the assumption of the same cross-sectional area over which the feedstock moves at the first pressure and the second pressure (although the cross-sectional area may be the same or different in actual operation). 48 • 48 • · * · · · · · · * *

This assay procedure can be used to properly compare pressure, although this is not necessary.

[0061]

The method may comprise supplying a pre-heated graphite-providing feedstock (optionally mixed with a filler fluid) to at least one feed point for feeding the feedstock to a graphite reactor, and mixing at least a pre-heated graphite feedstock via a feed point or feed points to a graphite reactor with a hot gas stream for generating a reaction stream in which the graphite is formed in the graphite reactor.

[0062]

According to the present invention, for any method, the predetermined target preheat temperatures are preferably represented by the average temperature of the feedstock being fed to the graphite reactor.

The pre-heating temperatures of the feedstock to be treated can be the maximum temperature of the feedstock to be treated or the minimum temperature of the feedstock to be treated before it is fed to the graphite reactor.

[0063]

According to the present invention, for any method, the determined target pressure is preferably represented by the average pressure of the feedstock being processed.

The prescribed pressure of the feedstock to be treated can be represented by the maximum pressure of the feedstock being processed or the minimum pressure of the feedstock being processed.

[0064]

According to the present invention, for any method, the determined target speed is preferably represented by the average feed rate of the feedstock.

The determined feed rate of the feedstock can be represented by the maximum feed rate of the feedstock or the minimum feed rate of the feedstock being processed.

Preheating can be accomplished by any means, with no limitation on these methods to achieve the target. Preheating can be performed in at least one heater (e.g., one, two, three or more).

The source of heat for the at least one heater can be any source, such as one or more graphite reactors, electric heating, plasma heating, residual gas heating, residual gas combustion, fuel combustion, and / or or heat from other industrial processes, and / or other forms of heating, and / or any combination of the above processes. Preheating can be performed when at least one heater partially or completely heats the feedstock to a target preheating temperature to feed it to the reactor.

One heater may provide partial or total preheating, or two or more heaters may be used sequentially or in another arrangement to provide preheating (partial or complete).

If partial preheating is provided by the at least one heater, then the remaining preheating is provided by an additional or secondary heat source or other heaters for the necessary achievement of the target preheating temperature.

[0066] 51 ···· ··· ··

For example, preheating at least one graphite-providing feedstock may or may be performed by heating the graphite-providing feedstock in at least one heater having a heat exchanger.

The heat exchanger may be operated at an average heat flow greater than about 10 kW / m 2, for example greater than about 10 kW / m 2 greater than about 20 kW / m 2, or greater than about 30 kW / m 2, greater than about 40 kW / m 2, as from about 10 kW / m 2 to about 150 kW / m 2, and the like.

[0067]

As an option, at least a portion of the preheating (or total preheating) is performed in at least one heater that acquires heat at least partially or wholly provided by the heat generated by the graphite reactor to which the preheated feedstock is fed or by another reactor or graphite reactors or both.

At least one heater may exhibit heat exchange with at least a portion of a graphite reactor to which preheated feedstock is fed, or with another graphite reactor or reactors, or both. 52 • «•« • ··· ····· · · · · · · ·····

For example, the at least one heater may contact the reaction stream in the graphite reactor, for example downstream of the arc quencher, wherein the at least one heater may have a heat exchanger whose walls are heated by the reaction stream on the first side (e.g. contacting the feedstock providing the graphite on the opposite side, for example on the inner wall).

As an option, the at least one heater may comprise a heat exchanger which heat exchange with the reaction stream in the graphite reactor, wherein the liquid heat carrier flowing through the heat exchanger is heated, wherein the heat carrier passes through at least one heater located on the outside of the reactor and adapted to transfer heat from the heat carrier to the graphite-providing feedstock.

At least one heater may be at least partially (or completely) supplied with heat from residual gases in the production of graphite (for example, residual gas heat or heat generated by residual gas combustion) from the graphite reactor or other graphite reactor or reactors or both , for heating the graphite-providing feedstock. The preheating may be partially or wholly performed using one or more plasma torches or other burners or heat sources.

Feeding the heated gas stream into the reactor may include plasma heating of the plasma-heatable gas stream in the plasma torch to produce at least a portion of the heated gas stream.

[0069]

According to the present invention, the non-catalytic surface can be used on some or all of the walls of at least one heater coming into contact with the graphite-providing feedstock and / or on the interior walls of at least one feedstock feed line that feeds the preheated feedstock feedstock to the reactor or graphite reactors.

This surface may be non-catalytic due to cracking (e.g., thermal cracking) or hydrocarbon polymerization.

[0070]

According to the present invention, the feeding step may include or comprise feeding a preformed graphite-providing feedstock via at least one feedstock feed line to feed the reactor or graphite reactors, the method optionally further comprising periodically feeding the purge gas or gases, which may be an oxidant for carbon, by means of at least one feed line or multiple feed lines for the feedstock to be treated. 54 • · · ·

The feed line for the feedstock exiting the at least one heater that preheats the feedstock may have a cross-sectional area (e.g., diameter) that is equal to or different from the feed line that feeds the feedstock into at least one heater (e.g. cross-sectional area).

[0071]

According to the present invention, the delivery may include supplying a preformed graphite-providing feedstock through at least one feed line of the feedstock that feeds the reactor or graphite reactors, the method may include injecting a preformed graphite feedstock into a graphite reactor, at least partially (or complete (by, for example) evaporation (for example, evaporation of the feedstock, caused, for example, by a pressure drop) of the feedstock providing the solid.

[0072]

As already mentioned, the feedstock to be treated can be heated to a temperature greater than about 300 ° C, or to other temperatures above 500 ° C, by employing the subject clogging or settling control procedures.

For example, the temperature of the feedstock resulting from the advantages of the present invention may be at least 310 ° C, at least 350 ° C, at least 375 ° C, at least 400 ° C, at least 425 ° C, at least about 450 ° C, or at least about 500 ° C, or at least about 550 ° C, or at least about 600 ° C, or at least about 650 ° C, or at least about 700 ° C, or at least about 750 ° C, or at least about 800 ° C, at least 850 ° C or from about 305 ° C to about 850 ° C, or from about 350 ° C to about 850 ° C, or from about 450 ° C to about 750 ° C, or from about 450 ° C to about 700 ° c, or from about 500 ° C to about 750 ° C, or from about 500 ° C to about 700 ° C.

This temperature of the feedstock represents the temperature of the feedstock to be processed to form the graphite directly after exit from the heater or heaters used to preheat the feedstock and / or directly before feed to the graphite reactor.

The temperature of the feedstock in this respect can be measured or scanned at one or more locations along the feed line of the feedstock from the point where the feedstock temperature was raised to about 300 ° C to the feed end of the feed line where the feedstock is processed. to the reactor.

This feed line of the raw material to be treated includes any length of piping in the raw material heater in which and after which the temperature of the raw material being processed is increased to a value in excess of about 300 ° C, and prior to shipment.

An additional portion of the feed conduit extending from the raw material heater to the reactor is provided.

As an option, the temperature of the preheated feedstock may have an absolute minimum value in the preheated feed line of the feedstock of at least 301 ° C, and / or, as an option, the maximum temperature variation in the preheated feedstock of the feedstock may be ± 20%, or ± 10%, for example. or ± 5%, or ± 2.5%, or ± 1%, or ± 0.5%, taking into account all sites along the feed line of the feedstock.

These temperatures of the feedstock to be treated can be used in combination with the various variables mentioned herein in the clogging or settling process.

[0073]

Regulating clogging or settling by utilizing said feedstock feed rate may at least partially include feeding feedstock or more feedstocks at this rate to the heater and / or through a heater that preheats the feedstock and / or through feedstock feed to the reactor. 57

MM «• ·

For example, the speed may be at least about 0.2 m / s, or at least about 0.5 m / s, or at least about 1 m / s, or at least about 1.6 m / s, or at least about 2 m / s, or at least about 3 m / s, or from about 0.2 m / s to about 10 m / s, or from about 1 m / s to about 7 m / s, or from about 1.5 m / s to about 3 m / s m / s, or from about 2 m / s to about 6 m / s, or from about 3 m / s to about 5 m / s.

The feed rate of the feedstock is a linear velocity relative to the longitudinal axis of the pipe or other feed line design.

The rate of raw material being processed (first speed) is measured at the point of introduction into the heater, which preheats the feedstock to be treated.

The rate of raw material being processed through the heater or heaters and / or after exiting the heater or heaters may be the same as the first velocity or different from the first velocity, and may be, for example, at least 1% greater, at least 2% larger, at least about 1% greater. 3% larger, at least 5% larger, at least 7% larger, at least 10% larger, at least 100% greater, 58 • at least ο 200% greater than ο 1% to 300% larger, or 50% to 200% larger, or the like.

The velocity is measured or calculated based on the density of the feedstock being measured, measured at 60 ° C and 1 atm pressure, and based on the smallest cross-sectional area present in the feed feed line being measured.

This feedstock feed line may include any length of pipe within the feedstock heater in which and / or beyond which the feedstock temperature has been increased to a value in excess of about 300 ° C, and before being transported to an additional feed line portion extending from the feedstock heater into the reactor.

For example, the rate of raw material being processed may have an absolute minimum value in the feed line of the feedstock to be at least 0.2 m / s, and / or as an option, the maximum variation in feedstock feed rate at the feedstock of the feedstock may be ± 20%, or ± 10%, for example or ± 5%, or ± 1%, or + 0.5%, taking into account all sites along the feedstock feed line.

59 [0074] 59 • · · · ·

Regulating clogging or deposition by using pressurized feedstock, at least in part, may include pressurizing or increasing the pressure of the feedstock to provide a solid, for example, to a pressure greater than about 10 bar, or greater than about 20 bar, or greater than about 30 bar, or greater about 40 bar, or greater than about 50 bar, or from about 10 bar to about 180 bar, or from about 20 bar to about 180 bar, or from about 40 bar to about 180 bar, or from about 50 bar to about 180 bar bars or more.

The feedstock pressures referred to herein are given as absolute pressures.

The pressure (first pressure) is the pressure measured at the point before feeding the feedstock into the heater for preheating.

The pressure through the heater or heaters that preheat the feedstock and / or downstream of the inlet or feed points into the reactor may be the same as the first pressure or different from the first pressure, for example lower than the first pressure, e.g. , at least 2% lower, at least 3% lower, at least 5% lower, or at least 7% lower, at least 10% lower, at least 15% lower, at least 20% lower than 1% to 25% % lower, 3% to 20% lower, and the like. The measurement of the pressure by the meter can be set to absolute values in a known manner for comparison with the ranges disclosed herein.

The pressure of the feedstock can be measured or scanned at one or more locations along the feed line of the feedstock from the point at which the feedstock temperature is raised to about 300 ° C to the feed end of the feed line where the feedstock is fed to reactor.

This feedstock feed line can include any length of pipe in the feedstock heater in which and after which the feedstock temperature has been increased to a value in excess of about 300 ° C, and before being transported to an additional feed line section from the feedstock heater to the reactor.

The pressure can be directly related to the temperature of the raw material being processed to control fouling or settling.

For example, a pressure of 10 bar feedstock may be adequate to control clogging or settling at a temperature of 300 ° C of raw material being processed, whereby an increased pressure of more than 10 bar, such as 20 bar or more, can be used to provide the same level controlling clogging or settling if the temperature of the feedstock is raised to 500 ° C, all other facts being the same.

The control of fouling or settling can be utilized by utilizing the low total residence time of the feedstock being processed.

The total residence time of the feedstock to be processed may be a combined time spent in at least one preheater, including the time that the pre-heated graphite feedstock spends before being fed to the reactor.

For example, the total residence time may be less than about 120 minutes, or less than about 90 minutes, or less than about 60 minutes, or less than about 45 minutes, or less than about 30 minutes, or less than 15 minutes, or less than 10 minutes. minutes, or less than 5 minutes, or less than 4 minutes, or less than 3 minutes, or less than 2 minutes, or less than 1 minute, or less than 30 seconds, or less than 15 seconds, or from about 1/60 minutes to about 120 minutes from about 0.5 minutes to about 120 minutes, or • 4 • · • · 62 * ·

From about one minute to about 90 minutes, or from about two minutes to about 60 minutes, or from about 3 minutes to about 45 minutes, or from about 4 minutes to about 30 minutes, or from 5 minutes to 30 minutes, or from 5 minutes to 40 minutes, or from 10 minutes to 30 minutes, or from about 5 minutes to about 15 minutes. The dwell time can be an average value or a maximum value or a minimum value. The residence time of the feedstock to be treated can be determined from the point at which the temperature of the feedstock is increased to above about 300 ° C, to the point where the feedstock is fed to the reactor. The dwell time may be inversely related to the temperature of the raw material being processed.

For example, the residence time of the raw material to be treated up to about 120 minutes can be tolerated without problems in clogging or settling at the temperature of the processed raw material of 310 ° C, wherein the residence time can be advantageously reduced to less than 120 minutes to provide the same level of clogging or settling if the temperature of the feedstock is raised to 500 ° C, all other facts being the same.

[0076]

Controlling fouling or settling during the preheating of the feedstock, for example, in the feedstock heater, may involve the use of a heater operating at an average heat flux that is greater than greater than greater than about 10 kW or about 20 kW / m2, or about 30 kW / m2, or about 50 kW / m2, or about 100 kW / m2, or or or or or 10 kW / m2 to about 150 kW / m2 (or more) 20 kW / m 2 to about 150 kW / m 2 (or more) 30 kW / m 2 to about 100 kW / m 2 (or more) 40 kW / m 2 to about 75 kW / m 2 (or more), 50 kW / m 2 to about 70 kW / m2.

Higher heat flow operation can be considered as a measure of clogging or settling, since a higher heat flux causes the graphite feedstock to be treated to heat faster, and / or allows a shorter residence time in the heater because shorter time to reach the target is needed preheating temperatures.

[0077]

Regulating fouling or deposition using a non-catalytic cracking surface (e.g., thermal cracking and / or polymerization of hydrocarbons on the inner walls of a feedstock feed line, at least partially may include, for example, one or more layers of protective lining such as ceramic lining (e.g., silica) , alumina or chromium trioxide).

Regulating clogging or deposition with the use of periodic direct delivery of purge gas through the feedstock feed line may include injecting oxidants for carbon (e.g., CO 2, oxygen, steam, steam / air mixture) into the feedstock feed of the feedstock at an accessible location or locations along the feedstock feed line. . The scrubbing gas can be fed at a temperature of 150 ° C or higher or above 300 ° C beyond any pumping means for pumping the liquid feedstock.

For example, the vapor velocity through the cleaning line may be at least about 6 m / s.

Any impermeable sites for the feedstock to be treated can be removed so that all the feedstock to be treated is immediately injected into the reactor. The scrubbing gas can be fed upstream of the feedstock heater to further ensure that all feed lines subjected to process temperatures that exceed 300 ° C are treated.

[0079]

As mentioned, regulating fouling or settling by removing carbon deposits with feedstock feed lines may include, for example, crumbling or mechanical scraping.

For example, the crumb may include cooling the deposits with which the tubes are coated, so that at least some of the deposits deposited on the inside of the tubes are peeling or popping or otherwise separating from the inner walls of the tubes when the tubes shrink as a result of cooling.

The released carbon deposits can be blown out or rinsed from the tubes so that the crumbled tube is ready for use again. During crushing or chipping, the feedstock can be diverted from the treated tube, for example by valves, via an alternative feed line or multiple feed lines to the reactor, which are arranged in the plant.

After cleaning, the stripped pipe is ready for use again.

Another method of cleaning deposited carbon deposits from the feedstock tubes may include providing a mechanical scraper to move through the tube to mechanically remove carbon deposits from the inner walls of the tubes. During mechanical scraping, the feedstock can be diverted, for example using valves, via an alternate line or multiple feed lines to the reactor, which are arranged in the apparatus, so that it is temporarily out of service while the tube is out of service for cleaning.

Rolling and / or mechanical scraping, if used, can be performed periodically on the feed lines of the feedstock.

[0080] 66 • ·

FIG. 1 shows a furnace 3 which comprises five regions, the primary combustion region 10, the transition region 13, the first reaction region 31, the neck region 31 and the second reaction region 35, into which the quenching probe 51 is positioned to terminate graphite formation reaction.

[0081]

The combustion region Π) is defined by the front wall 6 and the side wall 4, and terminates at the point 12 where the transition region 13 begins.

A pipe 6 extends through the wall 6 through which fuel is fed to the combustion zone 10.

A pipe 5 through which the oxidizing agent is fed to the combustion region 10 passes through the side wall 4. The pipe 5 is passed through the side wall.

A flame holder 10 is mounted in the combustion region 10 and is attached to a pipe 3 which passes into the combustion region 10 through an opening 7 in the wall 6.

A transitional region 13 is provided downstream of the combustion region K) and a transition region 13 is attached to the combustion region 30, which is defined by a wall 17 which begins at point 12 and ends at a point 14.

A plurality of substantially radially oriented openings 21 (or jet nozzles 21) are disposed circumferentially around the wall 7, through which the fluid mixture 87 and the feedstock can be injected into the transition region 13. 67 • · · · · · · · · · · · · · • · · · · · · · · · · · ·

FIG. 1 also illustrates a filler fluid 85 which is mixed with the feedstock 83 to form a fluid mixture 87 and feedstock prior to feeding (e.g., injection) through one or more openings 21 (or jet nozzles 21).

[0082]

In the direction of flow downstream of the transition region 13, a first reaction region 31, which is delimited by a wall 37, is positioned and fixed to this transition region 30.

The first reaction region 31 may be of varying length and width depending on the desired reaction conditions.

The inner cross-sectional area of the first reaction region 31 may be greater than that of the transition region 13. Preferably, the ratio of the inner cross-sectional area of the first reaction region to the cross-sectional area of the transition region is from 1.1 to 4.0.

The wall 32 then tapers at an angle of 45 ° relative to the central axis of the furnace 1 and passes into the wall 38 at the location 32.

Wall 31. defines the neck area. The inner cross-sectional area of the neck region 33 is smaller than the inner cross-sectional area of the transition region 13. Preferably, the ratio of the inner cross-sectional area of the neck region 33 with respect to the inner cross-sectional area of the transition region 13 is about 0.25 to 0.9. 68 ··· ·

The upstream end 34 of the wall 38 passes into the wall 39. The wall 39 extends at an angle of 30 ° with respect to the center axis of the furnace 1 and defines a second reaction region 35.

The inner cross-sectional area of the second reaction region 35 is greater than the inner cross-sectional area of the neck region 33. Preferably, the ratio of the inner cross-sectional area of the second reaction region 35 to the cross-sectional area of the transition region 131 is about 1.1 to 16.0. A quenching probe 41 passes through the wall 39 to the second reaction region 35. The quenching or cooling medium such as water can be injected through which the quenching or quenching reaction can be injected.

[0083]

As shown in Figures 2 to 5, at least one filler fluid 80 may be a feedstock treated feedstock 15 providing a fluid mixture 7 and a feedstock to be fed to reactor 2, such as a transition zone 12.

As shown in Fig. 2, the graphite-providing feedstock 15 is preheated to a temperature above about 300 ° C before being mixed with the filler fluid 85 and then fed to the reactor 2 as a fluid mixture 10 and feedstock. Preheated feedstock 15 > providing graphite is fed in at least one feed line 11 for the mixture of fluid and feedstock to at least one feed point 16 for supplying feedstock to reactor 2. 69 · ···· ···· · * T · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · ·

Upon introduction, the feedstock is mixed with the heated gas stream to produce a reaction stream in which the graphite is formed in the reactor.

The graphite in the reaction stream may be cooled in one or more regions.

For example, a cooling or quenching fluid is injected in the quenching or quenching quenching or quenching point 18, which may contain water and which can be used to completely or substantially complete the pyrolysis of the processed graphite-yielding feedstock, or only to partially cool the feedstock without stopping the pyrolysis. , which is followed by secondary cooling or quenching (not shown) used to stop the pyrolysis of the graphite-providing feedstock.

[0084]

As also shown in FIG. 2, the raw material heater may comprise a heat exchanger 19 (HXR) which may have heater walls (not shown), as used in known heat exchanger designs, which walls are heated through the reaction stream to their first. side, contacting the feedstock on its opposite side prior to feeding the feedstock into at least one feedstock feed line.

As indicated, the feedstock is heated in the heat exchanger to a temperature above about 300 ° C. Although shown in the downstream direction of the quenching or quenching device, the heat exchanger for the feedstock to be treated can be located in the flow direction. · · · · ···· 'U «« «i ·······« ψ 0 · · · · · ········································ or a quenching device in the reaction stream, provided that the heater is of such a design that it can be operated at high reactor temperatures.

The feedstock heater may be arranged to be in physical contact with at least a portion of the reactor, such as a coil or conduit, positioned inside or against and in contact with the heated wall or reactor walls to heat the feedstock to a temperature greater than about 300 ° C. Although not shown in Figure 2, the heat exchanger may optionally heat the feedstock to an intermediate temperature (e.g., above 250 ° C or from 50 ° C to 350 ° C, or other temperatures below the target preheating temperature) or may be used for achieving a preheating temperature above 300 ° C, whereupon another heat exchanger or heater on the outside or inside of the reactor can be used to heat to the final preheating temperature.

[0085]

The reaction stream in the reactor may have a cooling or quenching temperature of, for example, from about 600 ° C to about 2000 ° C, or from about 800 ° C to about 1,800 ° C, or from about 1,000 ° C to about 1,500 ° C. or may have other high temperatures corresponding to the extreme exothermic reaction occurring in the reactor furnace.

According to the present invention, heat exchange of the processed raw material with high exothermic heat generated by the reactions in the reactor can be provided without problems of fouling or clogging occurring in the feed lines of the feedstock being processed. 71 71 tak ·· · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · improving energy recovery and cost savings of raw materials compared to conventional graphite production, operated at much lower temperatures of the feedstock.

[0086]

Also, as shown in FIG. 2, at least one pump 20 can be installed in the feed line of the feedstock upstream of the feedstock heater 19 used to raise the temperature of the feedstock to a value that exceeds 300 ° C. The pump 20 can be used to increase the pressure of the feedstock before it enters the heater of the feedstock. In this way, the pressure of the feedstock to be processed can already be increased when the temperature of the feedstock is increased to higher values, while the problems of clogging the feed line of the feedstock could otherwise result in no pressurization or other indicated clogging approaches. .

As the raw material is usually depressurized during passage through the raw material heater under normal operating conditions (e.g., a pressure drop from 0 to about 20 bar), depending on, for example, the heat exchanger design and operation mode, and any pressurization , carried out with respect to the feedstock being treated as a clogging control, could compensate for any pressure drop that may or may be expected in the heat exchanger for the processed feedstock, as well as any other pressure drop to which may or may be expected to be in the supply lines or other channels used to convey the preheated feedstock to the reactor, especially when it is necessary to maintain the feedstock pressure within a predetermined range. Although only one feed line for the feedstock and the only feed point for the feedstock to be injected into the reactor is shown in FIG. 2, as well as in the accompanying figures, to simplify the drawing, it is to be understood that the plurality of feed lines of the feedstock and injection molding the reactor can be used, whereby clogging control can also be applied.

[0087]

After the mixture of hot combustion gases and the graphite-yielding feedstock being processed is cooled, the cooled gases pass in the flow direction to any known cooling and separation step where the graphite is recovered.

Separation of the graphite from the gas stream can be readily accomplished by known means such as a precipitation device, a cyclone separator or a bag filter.

Due to the complete extinguishing of the reactions for forming the final graphite product, any known process for extinguishing the flow downstream of the feedstock feedstock provided can be utilized, as is known to those skilled in the art.

For example, a cooling or extinguishing fluid may be injected, which may be water or other suitable fluid to stop the chemical reaction.

[0088]

FIG. 3 shows a portion of another type of furnace graphite reactor that can be used in the process of the present invention to produce graphite, wherein at least a portion of the preheating comprises contacting the heat exchanger 21 with the reaction stream in the reactor, wherein the liquid hot medium or carrier medium 28 such as the steam or nitrogen flowing through the heat exchanger is heated in the reactor, whereupon the heated steam (e.g. superheated steam) then passes out of the heat exchanger and the reactor and is routed through the separate raw material heater 24 located on the outside of the reactor to exchanging heat with the feedstock in the feedstock heater to heat the feedstock to a temperature above about 300 ° C, such as 370 ° C or higher.

[0089]

FIG. 4 illustrates a portion of another type of furnace graphite reactor that can be used in the process of the present invention to produce graphite, wherein at least a portion of the preheating comprises contacting the feedstock heater 23 with the residual gas exiting the reactor to heat the feedstock to the fluid to be treated to a temperature above about 300 ° C (or at least partially to the target temperature). · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · # ·· ··· ·· ·· ······

FIG. 5 depicts another type of furnace graphite reactor that can be used in the process of the present invention, wherein the heated gas stream further comprises at least partially or fully heated gas 2A that has been heated at least partially or entirely using a plasma heater 25.

Plasma gas heating can be carried out, for example, in accordance with known procedures known to those skilled in the art. For example, a plasma torch can be used, as described in U.S. Patent No. 5,486,674, the entire disclosure of which is incorporated herein by reference, reference being made also to plasma heating according to U.S. Pat. Nos. 4 101 639 and 3 288 696, the entire disclosure of which is incorporated herein by reference. here noted in the form of reference.

[0091]

As also shown in FIG. 5, the feedstock to be treated can be indirectly heated by means of a heated medium (e.g., steam) that has exchanged heat with the reaction stream in the heat exchanger 26 in the reactor, or alternatively, the feedstock can be indirectly heated in the heat sink. in the reactor as shown by dashed lines.

[0092]

As shown in Fig. 7, the feedstock (FS) to be treated can be fed separately from the filler fluid using a pipe structure that includes an annulus. 75 • · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · • Fig. 7 and Fig. 8 indicate the combustion stream.

FIG. 8 illustrates an embodiment where the feedstock (FS) for graphite production is separately fed from the filler fluid by means of a structure where the pipe is side by side.

[0093]

The heat exchanger design used to preheat the feedstock inside or outside the reactor of these various process schemes of the present invention may have any known heat exchanger design, such as shell and tube, shell and spiral, plate and frame, or the like.

For example, if the heat exchanger has an internal spiral configuration, a layout of eighty tubes and elbows may be utilized to avoid corrosion or erosion problems in the spiral.

Also, a constant spacing between the tubes can be utilized in the construction of an in-line spiral duct, whereby the spiral can utilize the entire cross section of the flue gas collector.

Heat transfer coefficients for in-line coils can vary significantly for different qualities and for different devices.

[0094]

Also, any processed raw materials for the disclosed process methods may contain additional materials or compositions that are generally used for graphite production. 76

The method of the present invention may further comprise supplying at least one substance that represents or contains at least one element of group ΙΔ and / or group IIA (or iron) of the periodic table. A substance comprising at least one element of Group IA and / or Group IIA (or iron) comprises at least one alkali metal or alkali metal of the earths. Examples include lithium, sodium, potassium, rubidium, cesium, francium, calcium, barium, strontium, or radium, or combinations thereof.

Any mixtures of one or more of these components may be present in the agent. The substance may be solid, may be a solution, dispersion, gas, or any combination thereof. More than one substance having the same or different IA and / or metal group IIA (or iron) may be utilized.

When multiple substances are used, the substances can be added together, separately, sequentially or at different sites of the reaction.

For purposes of this invention, the substance may be a metal (or metal ion), a compound containing one or more of these elements, including a salt comprising one or more of these elements, and the like. · • · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · capable of feeding the metal or metal ion into a reaction which is performed to produce a graphite product.

For purposes of this invention, a substance comprising at least one metal (or ion thereof) of Group IA and / or IIA, if used, may be fed at any point in the reactor, for example, prior to quenching or cooling.

For example, the substance may be added at any point prior to completion of quenching or cooling, including prior to supplying the graphite-providing feedstock in the first stage, during the feed of the graphite-providing feedstock in the first reaction step, after the graphite-providing feedstock is fed in the first reaction stage before, during or immediately after the introduction of any second graphite-yielding feedstock, or at any step after feeding the second graphite-providing feedstock, but before completion of quenching or cooling. More than one substance supply point can be used.

[0095] 78 * * • · · · · · ·

In addition, as previously stated, the present invention relates to a method for controlling at least one property of graphite particles.

The method comprises mixing at least one filler fluid with at least one graphite-providing feedstock (before and / or after entering the reactor) to form a mixture of fluid and feedstock. The method may further comprise supplying the fluid and feedstock mixture to the reactor at solid or feeding the filler fluid and feedstock separately to the reactor. The feed of the mixture of fluid and feedstock can be carried out in the form of one or more streams.

The method includes controlling the amount of filler fluid present in the fluid mixture and the feedstock to control at least one of the portion properties. The terms " filler fluid "," graphite-providing feedstock " and "a mixture of fluid and feedstock" have the same meaning as those terms have been defined and explained in the above description.

[0096]

One example of at least one particle property is a light shade.

The property of the particles may be a surface area property or a structure property.

The present invention will be further elucidated by means of the following examples, which, however, are merely exemplary of the present invention.

EXAMPLES Example 1 In one example of the present invention, a hot gas stream from a high velocity natural gas flame (greater than 200 m / s) was ignited into a transition area (D = 135 mm) of a solid-state reactor as shown in FIG. 1, at a ratio of 0.8.

The decanted feedstock was injected into the transition area using four injectors at a total ratio of 3.33.

The feedstock injectors each had a 0.76 mm aperture, followed by a 76 mm expansion section and 6.5 mm diameter.

The feedstock was preheated to about 500 ° C before entering the injectors. 80 • · · · · · · ·

Nitrogen was added to the feedstock as filler fluid at flow rates of from 0% to 20% by weight (see the following table) of the feedstock stream immediately downstream of the orifice.

Nitrogen was added in such a way that it was mixed with the raw material being processed before entering the transition zone.

[0099]

The penetration of the fluid streams and the feedstock into the transition region was observed visually through the observation hole in the reactor.

Without any filler fluid, the feedstock streams merely penetrated into the transverse flow of the high velocity hot gas stream to a depth equal to about 25% of the transition area diameter (which is about 34 mm of penetration).

When the filler fluid was added to the feedstock, the flow of fluid and feedstock was continuously increased until the opposing fluid streams and the feedstock met at the center of the transition region (about 68 mm of penetration).

It was observed that this occurred at a nitrogen stream of 20% by weight, based on the weight of the feedstock being injected. 81 81 ····

·· · 9 · t? tf · ···· ··

In addition, the graphite hue value was measured using the ASTM D3265 method, with an increase for a given graphite surface area when adding more nitrogen to the feedstock in the fluid / feed mixture. The following table shows how shade and current leakage vary based on the nitrogen flow rate.

Table 1

N2 Current (in% by weight of feedstock) Current Inlet (in% of transition area diameter) Hue in% (ASTM D3265) 0 25% 122 5 35% 127 10 45% 130 20 > Example 2 In the second example of the invention using the same reactor as in Example 1, nitrogen was added to the annulus (as shown in Figure 7) around the feed streams that the annular filler fluid and the fluid to be treated are not mixed prior to entering the transition zone.

The filler fluid was in close proximity to the feedstock being processed so that the momentum of the feedstock to be processed was increased, thereby increasing the flow of the fluid stream and the feedstock being processed.

The same reaction conditions were used as in Example 1, whereby nitrogen was added to the annulus at flow rates of from 0% to 20% by weight of the feedstock stream, based on the weight of the feedstock being injected.

As in the previous example, the penetration of the feedstock stream was only about 25% of the diameter of the transition area, with no fluid flow in the annulus.

The current leakage increased with the filler fluid flow in the annulus up to about 40% of the transition region diameter at 20% by weight, based on the weight of the feedstock being injected.

Accordingly, the addition of the filler fluid in this way increases the penetration of the fluid stream and the feedstock, but not as efficiently as in the previous example.

The shade also increased to some extent when adding the nitrogen in the annulus.

Table 2

N2 Current (in% by weight of feedstock) Current Inlet (in% of transition area diameter) Hue in% (ASTM D3265) 0 ~ 25% 122 5 ~ 30% 123.5 10 ~ 35% 126 20 ~ 4 0% 127, 5 [00101] 83

The present invention includes the following aspects / embodiments / features in any order and / or combination: 1. A process for producing graphite, comprising the steps of: feeding a stream of heated gas to a graphite reactor, mixing at least one filler fluid with at least one graphite-treated feedstock to form a mixture of fluid and feedstock such that at least one filler fluid increases the momentum of at least one graphite-providing feedstock in a direction that is axial or substantially axial to at least one feed point of feedstock to the graphite reactor; feeding the mixture of fluid and the feedstock to at least one point for feeding the feedstock to the graphite reactor, mixing at least one fluid and feedstock mixture through at least one feed point into the lead graphite reactor the heated gas to form a reaction stream in which a graphite is formed in the graphite reactor and recovering the graphite in the reaction stream. A method according to any preceding or following embodiment / feature / aspect, wherein the filler fluid is chemically inert to the graphite-providing feedstock being processed. 84 • · · · · 84

3. A method according to any preceding or following embodiment / feature / aspect, wherein the filler fluid is uniformly distributed to the graphite-providing feedstock. A method according to any preceding or following embodiment / feature / aspect, wherein the supply of the fluid / feedstock mixture is carried out in the form of one or more streams, the one or more streams of fluid / feedstock mixture containing sufficient filler fluid to drive the processed feedstock providing graphite into the inner portion of the heated gas stream. A method according to any preceding or following embodiment / feature / aspect, wherein the filler fluid is at least one inert gas. A method according to any preceding or following embodiment / feature / aspect, wherein the filler fluid is steam, water, air, carbon dioxide, natural gas, carbon monoxide, hydrogen, residual graphite, nitrogen, or any combination thereof. The method of any preceding or following embodiment / feature / aspect, wherein the filler fluid is nitrogen. A method according to any preceding or following embodiment / feature / aspect, wherein the filler fluid is fed to the treated feedstock providing a solid at a pressure sufficient to penetrate into the treated feedstock providing the solid to form a mixture of fluid and feedstock. 9. A method according to any preceding or following embodiment / feature / aspect, wherein the filler fluid is fed to a processed feedstock providing graphite at a pressure of about one pound per inch to about 350 pounds per inch square, to form a mixture of fluid and feedstock. A method according to any preceding or following embodiment / feature / aspect, wherein the graphite-providing feedstock is comminuted prior to mixing with the filler fluid. A method according to any preceding or following embodiment / feature / aspect, wherein the amount of filler fluid that is mixed with the graphite-providing feedstock is adjustable during continuous graphite production. A method according to any preceding or following embodiment / feature / aspect, wherein the supply of the fluid / feedstock mixture is conducted in the form of one or more streams, wherein the flow of the fluid / feedstock stream into the heated gas stream is adjusted by varying the content of the filler fluid in a mixture of fluid and feedstock during continuous graphite production. A method according to any preceding or following embodiment / feature / aspect, wherein the filler fluid is at least partially distributed to the graphite-providing feedstock. 86 • ·

14. A method according to any preceding or following embodiment / feature / aspect, wherein the filler fluid is present in the fluid / feedstock mixture in an amount of from about 0.1% to about 400% by weight based on the weight of graphite-providing feedstock. A method according to any preceding or following embodiment / feature / aspect, further comprising heating the treated feedstock providing a solid prior to mixing with the filler fluid to form a mixture of fluid and feedstock. A method according to any preceding or following embodiment / feature / aspect, further comprising heating the treated feedstock providing the solid to a temperature above about 300 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock. A method according to any preceding or following embodiment / feature / aspect, further comprising heating the treated feedstock providing a temperature of from about 360 ° C to about 850 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock. A method according to any preceding or following embodiment / feature / aspect, further comprising heating the graphite-providing feedstock to a first temperature of from about 300 ° C to about 850 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock, and then heating the fluid / feed mixture to a second temperature that is greater than the first temperature, each of said heating steps prior to feeding to the graphite reactor. A method according to any preceding or following embodiment / feature / aspect, further comprising heating the graphite-providing feedstock to a first temperature of about 400 ° C to about 600 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock, and then heating the fluid / feed mixture to a second temperature that is greater than the first temperature of at least 50 ° C, each of said heating steps prior to being introduced into the graphite reactor. A method according to any preceding or following embodiment / feature / aspect, further comprising heating the graphite-providing feedstock to a first temperature of from about 400 ° C to about 600 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock, and then heating the fluid / feed mixture to a second temperature that is greater than the first temperature of at least 100 ° C, each of said heating steps prior to being introduced into the graphite reactor. A method according to any preceding or following embodiment / feature / aspect, further comprising heating the graphite-providing feedstock to a first temperature prior to mixing with the filler fluid to form a mixture of fluid and feedstock, and then heating the fluid / feedstock mixture to a second temperature, which is higher than the first temperature, and up to about 950 ° C, each of said heating steps being carried out prior to introduction into the graphite reactor. 88 · «··

A method according to any preceding or following embodiment / feature / aspect wherein the setting of the filler fluid is performed to control the constricted flow rate or critical velocity, or both, in one or more fluid and feedstock mixture streams, thereby altering the penetration of the mixture and feedstock to the heated gas stream. A method of controlling at least one property of graphite particles, comprising the steps of: mixing at least one filler fluid with at least one graphite-treated feedstock to form a mixture of fluid and feedstock and supplying said fluid and feedstock mixture to a graphite reactor, the fluid and the feedstock are conducted in the form of one or more streams and the amount of filler fluid present in the fluid / feedstock mixture is controlled to control at least one particle property. A method according to any preceding or following embodiment / feature / aspect, wherein the at least one particle property is a shade. A method according to any preceding or following embodiment / feature / aspect, wherein the filler fluid is chemically inert to the graphite-providing feedstock being processed.

26. A method according to any preceding or following embodiment / feature / aspect, wherein the filler fluid is uniformly distributed to the graphite-providing feedstock. A method according to any preceding or following embodiment / feature / aspect, wherein the supply of a mixture of fluid and raw material is carried out in the form of one or more streams, wherein one or more streams of fluid / feedstock mixture contain sufficient filler fluid to drive the processed feedstock providing graphite into the inner portion of the heated gas stream. A method according to any preceding or following embodiment / feature / aspect, wherein the filler fluid is at least one inert gas. A method according to any preceding or following embodiment / feature / aspect, wherein the filler fluid is steam, water, air, carbon dioxide, natural gas, carbon monoxide, hydrogen, residual graphite, nitrogen, or any combination thereof. A method according to any preceding or following embodiment / feature / aspect, wherein the filler fluid is nitrogen. 31. A method according to any preceding or following embodiment / feature / aspect, wherein the filler fluid is fed to a treated feedstock providing a solid at a pressure sufficient to penetrate into the treated feedstock providing a solid to form a mixture of fluid and feedstock. The method according to any preceding or following embodiment / feature / aspect, wherein the filler fluid is fed to the feedstock being provided, providing a < RTI ID = 0.0 >< / RTI > solids at a pressure of about one pound per inch to about 350 pounds per inch to form a mixture of fluid and feedstock. A method according to any preceding or following embodiment / feature / aspect, wherein the amount of filler fluid that is mixed with the graphite-providing feedstock is adjustable during said graphite production method. A method according to any preceding or following embodiment / feature / aspect, wherein the amount of filler fluid that is mixed with the graphite-providing feedstock is adjustable during continuous graphite production. A method according to any preceding or following embodiment / feature / aspect, wherein the supply of a mixture of fluid and feedstock is carried out in the form of one or more streams, wherein the flow of the mixture of fluid and feedstock into the heated gas stream is adjusted by changing the content of filler fluid in a mixture of fluid and feedstock during continuous graphite production. The method of any preceding or following embodiment / feature / aspect, wherein the filler fluid is present in the fluid / feedstock mixture in an amount of from about 0.1% to about 400% by weight based on the weight of graphite-providing feedstock. 91

37. The method of any preceding or following embodiment / feature / aspect, wherein the filler fluid is present in the fluid / feedstock mixture in an amount of about 0.1% to about 50% by weight based on the weight of the graphite-providing feedstock. 38. A method according to any preceding or following embodiment / feature / aspect, further comprising heating the graphite-providing feedstock prior to mixing with the filler fluid to form a mixture of fluid and feedstock. 39. A method according to any preceding or following embodiment / feature / aspect, further comprising heating the treated feedstock providing the solid to a temperature above about 300 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock. 40. The method of any preceding or following embodiment / feature / aspect, further comprising heating the treated feedstock providing a temperature of from about 360 ° C to about 850 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock. 92 ·

41. The method of any preceding or following embodiment / feature / aspect, further comprising heating the graphite-providing feedstock to a first temperature of from about 300 ° C to about 850 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock, and then heating the fluid / feed mixture to a second temperature that is higher than the first temperature, each of said heating steps prior to feeding to the graphite reactor. A method according to any preceding or following embodiment / feature / aspect, further comprising heating the graphite-providing feedstock to a first temperature of about 400 ° C to about 600 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock, and then heating the fluid / feed mixture to a second temperature that is greater than the first temperature of at least 50 ° C, each of said heating steps prior to being introduced into the graphite reactor. 43. The method of any preceding or following embodiment / feature / aspect, further comprising heating the graphite-providing feedstock to a first temperature of about 400 ° C to about 600 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock, and then heating the fluid / feed mixture to a second temperature that is greater than the first temperature of at least 100 ° C, each of said heating steps prior to being introduced into the graphite reactor. A method according to any preceding or following embodiment / feature / aspect, further comprising heating the graphite-providing feedstock to a first temperature prior to mixing with the filler fluid to form a mixture of fluid and feedstock, and then heating the fluid / feedstock mixture to a second temperature, which is higher than the first temperature, and up to about 950 ° C, each of said heating steps being carried out prior to introduction into the graphite reactor. A method according to any preceding or following embodiment / feature / aspect, wherein the penetration is adjusted by a filler fluid affecting the constricted flow rate or critical velocity, or both, in one or more fluid / feedstock feed streams. A method for producing graphite, comprising the steps of: feeding a stream of heated gas to a graphite reactor, feeding at least one treated graphite feedstock to at least one feedstock feed point into a graphite reactor, feeding at least one filler fluid to at least one feedstock sites for the graphite reactor, wherein the at least one filler feed point is positioned such that at least one filler fluid increases the momentum of the at least one graphite-yielding feedstock when the graphite feedstock encounters the heated gas stream;

Mixing at least one graphite-providing feedstock and at least one filler fluid with a heated gas stream to generate a reaction stream in which the graphite is formed in the graphite reactor, and recovering the graphite in the reaction stream. A method according to any preceding or following embodiment / feature / aspect, wherein the filler fluid is inert to the graphite-providing feedstock being treated. 48. The method of any preceding or following embodiment / feature / aspect, wherein the filler fluid is distributed to the graphite-providing feedstock. A method according to any preceding or following embodiment / feature / aspect, wherein the feedstock feedstock supplying the graphite feed and the filler fluid feed is in the form of one or more streams, one or more streams, each stream having a central hollow tip with an annulus for delivery filler fluids. 50. A method according to any preceding or following embodiment / feature / aspect, wherein the feedstock feedstock providing feedstock and filler fluid is fed in the form of a pair of one or more adjacent streams, wherein one stream in each pair feeds the feedstock providing graphite and the second stream in each pair feeds the filler fluid. 51. The method of any preceding or following embodiment / feature / aspect, wherein the filler fluid is fed at a pressure sufficient to penetrate the graphite-providing feedstock. 52. A method according to any preceding or following embodiment / feature / aspect, further comprising heating the treated feedstock providing the solid to a temperature greater than about 300 ° C before being fed to the at least one feed site. 53. A method according to any preceding or following embodiment / feature / aspect, further comprising heating the treated feedstock providing a solid to a temperature of about 360 ° C to about 850 ° C before being fed to at least one feed site. 54. A method of controlling at least one graphite particle comprising: separately feeding, a) at least one filler fluid b) at least one graphite feedstock processed into a solid reactor, wherein the feed of a) and b) is carried out in the form of one or more and controlling the amount of filler fluid present to control at least one particle property. 96 • · · · · ·

55. The method of any preceding or following embodiment / feature / aspect, wherein the at least one particle property is a hue. 56. The method of any preceding or following embodiment / feature / aspect, further comprising heating the filler fluid to a first temperature prior to mixing with the feedstock to form a fluid / feedstock mixture. 57. A method according to any preceding or following embodiment / feature / aspect, further comprising heating the graphite-providing feedstock to a first temperature prior to mixing with the filler fluid and heating the filler fluid to a second temperature prior to mixing with the graphite-providing feedstock and then mixing to form a mixture of fluid and feedstock, and then heating the fluid / feedstock mixture to a third temperature that is higher than the first temperature and up to a temperature of about 950 ° C, each of the heating steps being carried out prior to feeding the reactor to the solid. 58. The method of any preceding or following embodiment / feature / aspect, wherein the at least one particle property is a surface area. 59. The method of any preceding or following embodiment / feature / aspect, wherein the graphite-providing feedstock is comminuted prior to mixing with the filler fluid. 60. The method of any preceding or following embodiment / feature / aspect, further comprising heating the graphite-providing feedstock to a temperature greater than about 300 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock, wherein the graphite-yielding feedstock is processed it is comminuted prior to mixing with the filler fluid. 61. The method of any preceding or following embodiment / feature / aspect, wherein the filler fluid is present in the fluid / feedstock mixture in an amount of from about 0.1% by weight to about 50% by weight based on the weight of graphite-providing feedstock.

The present invention may include any combination of these various features or embodiments set forth above and / or below as set forth in the sentences and / or paragraphs.

Any combination of the features described herein is considered to be part of the present invention, with no limitation being considered with respect to combinable features.

Applicants specifically encompass the entire contents of all references cited herein.

In addition, when the amount, concentration, or other value or parameter, either range, preferred range, or list of the preferred values and the preferred values set forth below is referred to, this is to be understood as specific. Describing any ranges formed from any pair of any upper range or preferred value, and any lower range or preferred value, regardless of whether the ranges are separately described.

If a numerical range is given herein, unless otherwise indicated, this range is intended to include all endpoints and all integers or fractions within that range.

The scope of the invention should not be limited to the specific particular values given when defining the range.

[00104]

Other embodiments of the present invention will be apparent to those skilled in the art upon consideration of the present disclosure and practice of the present invention described herein. The present description and examples are to be construed as merely exemplary within the true scope and spirit of the invention as set forth in the following claims, as well as equivalents thereof.

Claims

99 / V / Le / f-jfy 99 • · ·· * ···· • PATENT REQUIREMENTS 1. Method of producing graphite, comprising the steps of: supplying a stream of heated gas to a graphite reactor, mixing at least one filler fluid with at least one processed feedstock providing a solid to form a mixture of fluid and feedstock such that at least one filler fluid increases the momentum of at least one graphite feedstock being processed in the direction which is axial or substantially axial to at least one point of feed of the feedstock to the graphite reactor, feed of the fluid and feedstock mixture to at least one feed point feed point into the graphite reactor, mix at least a mixture of fluid and feedstock through at least one feed point to a reactor for producing graphite with a heated gas stream; for generating a reaction stream in which a graphite is formed in the graphite reactor and recovering the graphite in the reaction stream. 100

1 according to that

Process according to Claim 1, characterized in that the filler fluid is chemically inert to the graphite-providing feedstock.

3. The process of claim 1 wherein the filler fluid is uniformly distributed to the graphite-providing feedstock.

Method according to claim 1, characterized in that the supply of the fluid and the feedstock mixture is carried out in the form of one or more streams, wherein one or more streams of the fluid / feedstock mixture contain sufficient filler fluid to drive the processed feedstock providing graphite to the inner portion gas flow. claim 1 that the filler fluid

5. The process of claim 1 wherein the at least one inert gas is.

The method of claim 1, wherein the filler fluid is steam, water, air, carbon dioxide, natural gas, carbon monoxide, hydrogen, residual graphite, nitrogen, or any combination thereof.

7. The process of claim 1 wherein the filler fluid is nitrogen. • ♦ 101

8. The process of claim 1 wherein the filler fluid is fed to the feedstock provided to provide a solid at a pressure sufficient to penetrate the graphite feedstock to form a mixture of fluid and feedstock.

9. The method of claim 1 wherein the filler fluid is fed to the graphite feedstock at a pressure of from about one pound per inch to about 350 pounds per inch to form a mixture of fluid and feedstock.

10. The process of claim 1 wherein the graphite-yielding feedstock is comminuted prior to mixing with the filler fluid.

11. The method of claim 1 wherein the amount of filler fluid that is mixed with the graphite-providing feedstock is adjustable during continuous graphite production.

12. A method according to claim 1, wherein the feeding of the fluid and feedstock mixture is carried out in the form of one or more streams, wherein the flow of the fluid / feedstock stream into the heated gas stream is adjusted by varying the content of the filler fluid in the fluid mixture. and the processed raw material during continuous graphite production. 102 ·· »·

13. The method of claim 1 wherein the filler fluid is at least partially distributed to the graphite-providing feedstock.

14. The method of claim 1 wherein the filler fluid is present in the fluid / feedstock mixture in an amount of from about 0.1% to about 400% by weight based on the weight of the graphite-providing feedstock.

15. The method of claim 1, further comprising heating the graphite-providing feedstock prior to mixing with the filler fluid to form a mixture of fluid and feedstock.

16. The method of claim 1 further comprising heating the graphite-providing feedstock to a temperature above about 300 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock.

17. The method of claim 1, further comprising heating the graphite-providing feedstock to a temperature of about 360 ° C to about 850 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock. 103 • · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · ·

18. The method of any of claims 1 further comprising heating the graphite-providing feedstock to a first temperature of from about 300 ° C to about 850 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock, and then heating the mixture the liquid and the feedstock to a second temperature that is higher than the first temperature, each of said heating steps being carried out prior to being introduced into the graphite reactor.

19. The method of claim 1, further comprising heating the graphite-providing feedstock to a first temperature of from about 400 ° C to about 600 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock, and then heating the fluid mixture. and treating the feedstock to a second temperature that is greater than the first temperature of at least 50 ° C, wherein each of said heating steps takes place before being fed to the graphite reactor.

20. The method of claim 1 further comprising heating the graphite-providing feedstock to a first temperature of from about 400 ° C to about 600 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock, and then heating the fluid mixture. and treating the feedstock to a second temperature that is greater than the first temperature of at least 100 ° C, wherein each of said heating steps takes place before being fed to the graphite reactor. 104 • · ·· ····· • · · · · · · · · · · · · · · · · · · · · · · · ·

21. The method of claim 1, further comprising heating the graphite-providing feedstock to a first temperature prior to mixing with the filler fluid to form a fluid / feedstock mixture, and then heating the fluid / feedstock mixture to a second temperature that is higher than the first temperature, and up to about 950 ° C, wherein each of the heating steps takes place before being fed to the graphite reactor.

Method according to claim 4, characterized in that the setting of the filler fluid is carried out to regulate the constricted flow rate or critical velocity or both at one or more streams of the fluid and feedstock mixture, thereby changing the penetration of the mixture and the feedstock into gas flow.

A method of controlling at least one property of graphite particles, comprising the steps of: mixing at least one filler fluid with at least one graphite-treated feedstock to form a mixture of fluid and feedstock and supplying said fluid and feedstock mixture to a graphite reactor, the fluid and the feedstock are conducted in the form of one or more streams and the amount of filler fluid present in the fluid / feedstock mixture is controlled to control at least one particle property. The claim 23 that at least once

24. A method according to any one of the preceding claims wherein the particulate property is a hue.

The method of claim 23, wherein the filler fluid is chemically inert to the graphite-providing feedstock.

26. The method of claim 23, wherein the filler fluid is uniformly distributed to the graphite-providing feedstock.

Method according to claim 23, characterized in that the feed of the fluid and feedstock mixture is carried out in the form of one or more streams, wherein one or more streams of fluid and feedstock mixture contain sufficient filler fluid to drive the feedstock providing graphite to the inner portion gas flow. claim 23 that the filler fluid

28. The process of claim 1 wherein the at least one inert gas is.

The method of claim 23, wherein the filler fluid is steam, water, air, carbon dioxide, natural gas, carbon monoxide, hydrogen, residual graphite, nitrogen, or any combination thereof.

The method of claim 23, wherein the nitrogen-containing filler fluid. 106 • · · · · · · · · · · · · · · · · · · · · · · · · · · · ·

31. The method of claim 23, wherein the filler fluid is fed to the feedstock provided to provide a solid at a pressure sufficient to penetrate into the feedstock to provide a graphite to form a mixture of fluid and feedstock.

32. The method of claim 23, wherein the filler fluid is fed to the graphite feedstock at a pressure of about 1 pound per inch to about 350 pounds per inch to form a mixture of fluid and feedstock.

33. The method of claim 23 wherein the amount of filler fluid that is mixed with the graphite-providing feedstock is adjustable during said graphite production process.

34. The method of claim 23 wherein the amount of filler fluid that is mixed with the graphite-providing feedstock is adjustable during continuous graphite production.

Method according to claim 23, characterized in that the supply of the mixture of the fluid and the feedstock is carried out in the form of one or more streams, the passage of the flow of the mixture of liquid and the feedstock into the stream of heated gas being adjusted by changing the content of the filler fluid in liquid and processed material during continuous graphite production. 107

36. The method of claim 23 wherein the filler fluid is present in the fluid / feedstock mixture in an amount of from about 0.1% to about 400% by weight based on the weight of the graphite-providing feedstock.

37. The method of claim 23, wherein the filler fluid is present in the mixture of fluid and feedstock in an amount of from about 0.1% to about 50% by weight based on the weight of the graphite-providing feedstock.

38. The method of claim 23, further comprising heating the graphite-providing feedstock prior to mixing with the filler fluid to form a mixture of fluid and feedstock.

39. The method of claim 23, further comprising heating the graphite-providing feedstock to a temperature above about 300 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock.

40. The method of claim 23, further comprising heating the graphite-providing feedstock to a temperature of about 360 ° C to about 850 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock. • 108 • · 108 • · · ··· · · · # · · · ···· · · «

41. The method of claim 23 further comprising heating the graphite-providing feedstock to a first temperature of from about 300 [deg.] C. to about 850 [deg.] C. prior to mixing with the filler fluid to form a mixture of fluid and feedstock, and then heating the fluid mixture. and treating the feedstock to a second temperature that is higher than the first temperature, each of said heating steps being carried out before being fed to the graphite reactor.

42. The method of claim 23, further comprising heating the graphite-providing feedstock to a first temperature of from about 400 ° C to about 600 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock, and then heating the fluid mixture. and treating the feedstock to a second temperature that is greater than the first temperature of at least 50 ° C, wherein each of said heating steps takes place before being fed to the graphite reactor.

43. The method of claim 23, further comprising heating the graphite-providing feedstock to a first temperature of from about 400 ° C to about 600 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock, and then heating the fluid mixture. and treating the feedstock to a second temperature that is greater than the first temperature of at least 100 ° C, wherein each of said heating steps takes place before being fed to the graphite reactor. 109 • · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · ·

44. The method of claim 23, further comprising heating the graphite-providing feedstock to a first temperature prior to mixing with the filler fluid to form a fluid / feedstock mixture, and then heating the fluid / feedstock mixture to a second temperature that is higher than the first temperature, and up to about 950 ° C, wherein each of the heating steps takes place before being fed to the graphite reactor.

45. The method of claim 27, wherein the current penetration is adjusted by the filler fluid, affecting the constricted flow rate or critical velocity, or both, in one or more fluid and feedstock streams.

A method for producing graphite, comprising the steps of: feeding a stream of heated gas to a graphite reactor, feeding at least one treated graphite feedstock to at least one feedstock feed point into a graphite reactor, feeding at least one filler fluid to at least one feedstock sites for the graphite reactor, wherein the at least one filler feed point is positioned such that at least one filler fluid increases the momentum of the at least one graphite feedstock processed when the graphite feedstock impinges on the heated gas stream 110 mixing at least one feedstock provided solids and at least one filler fluid with a heated gas stream for generating a reaction stream in which the graphite is formed in the graphite reactor and recovering the graphite in the reaction stream.

47. The method of claim 46 wherein the filler fluid is inert to the feedstock being treated.

48. The method of claim 46, wherein the filler fluid is distributed to the graphite-providing feedstock.

49. The method of claim 46, wherein feeding the feedstock to be supplied with a solid and feeding the filler fluid is in the form of one or more streams, wherein one or more streams, each stream having a central hollow tip with a cover ring for supplying filler fluid.

A method according to claim 46, characterized in that the feed of the feedstock providing the solid and the filler fluid is carried out in the form of a pair of one or more adjacent streams, wherein one stream in each pair feeds the feedstock providing the graphite and the second stream in feeding the liquid to each pair.

51. The method of claim 46, wherein the filler fluid is fed at a pressure sufficient to penetrate the graphite-providing feedstock. • 111 • · · · · · · · · · · · · · · · · · · ·

52. A method of heating processed to greater than about 300 feed points. according to claim 46, further comprising feedstock providing graphite to a temperature of ° C prior to being fed to at least one

53. The method of claim 46, further comprising heating the graphite-providing feedstock to a temperature of about 360 ° C to about 850 ° C prior to feeding it to at least one feed point.

54. A method of controlling at least one property of graphite particles comprising: separately feeding, a) at least one filler fluid b) at least one graphite feedstock processed into a solid-state reactor, the feed of a) and b) being carried out in the form of one or multiple streams, and controlling the amount of filler fluid present to control at least one particle property.

55. The method of claim 1, wherein the particle property is a hue. of at least 54, once 112

56. The method of the claim further comprising heating the filler fluid to a first temperature prior to mixing with the feedstock to form a mixture of fluid and feedstock. According to that, 1

57. The method further comprising heating the graphite-providing feedstock to a first temperature prior to mixing with the filler fluid and heating the filler fluid to a second temperature prior to mixing with the graphite-providing feedstock, and then mixing to form a fluid / feedstock mixture, and then heating a mixture of fluid and feedstock to a third temperature that is higher than the first temperature, and up to a temperature of about 950 ° C, wherein each of the heating steps is carried out before being fed to the reactor in solid state.

58. The method of claim 23 wherein the at least one particle property is a surface area.

59. The method of claim 46, wherein the graphite-providing feedstock is comminuted prior to mixing with the filler fluid.

60. The method of claim 1 further comprising heating the graphite-providing feedstock to a temperature greater than about 300 ° C prior to mixing with the filler fluid to form a mixture of fluid and feedstock, wherein the graphite-yielding feedstock is comminuted prior to by mixing it with the filler fluid. 113 • · · ·

61. The method of claim 1, wherein the filler fluid is present in the fluid / feedstock mixture in an amount of from about 0.1% to about 50% by weight based on the weight of the graphite-providing feedstock.