WO2016019443A1

WO2016019443A1 - Method for producing spinnable mesophase petroleum pitch for the production of continuous carbon fibres

Info

Publication number: WO2016019443A1
Application number: PCT/BR2014/000264
Authority: WO
Inventors: Luiz Depine De Castro; Carlos Henrique Monteiro De Castro Dutra; AlexandreTaschetto DE CASTRO; Fabio FRANCESCHI PEREIRA; Maria Helena GONÇALVES PEREIRA; Wladimir FERRAZ DE SOUZA
Original assignee: Petróleo Brasileiro S.A. - Petrobras; Centro Tecnológico Do Exército - Exército Brasileiro
Priority date: 2014-08-05
Filing date: 2014-08-05
Publication date: 2016-02-11
Also published as: BR112015010499B1; AR106359A1; BR112015010499A2

Abstract

The invention relates to a method and devices for producing continuous carbon fibres with high-quality mechanical properties from heavy petroleum derivatives, such as decant oil, aromatic residues or any other mixture with a high aromatic hydrocarbon content. According to the method of the invention, a mesophase petroleum pitch with more than 70% mesophase content can be obtained in order to produce continuous carbon fibres from petroleum pitch with high-quality mechanical properties and at a low cost. These devices include bubblers designed to ensure satisfactory gas distribution within the material in a simple and effective manner.

Description

PROCESS FOR THE PRODUCTION OF RELIABLE MESOPHASIC OIL PICKLE FOR THE PRODUCTION OF

CONTINUOUS CARBON

FIELD OF INVENTION

[1] The invention relates to a special process and device for producing continuous carbon fibers with high mechanical properties from heavy petroleum derivatives such as decanted oil, aromatic residue or any other mixture containing high aromatic hydrocarbon content. According to the process of the invention it is possible to obtain mesophasic oil tar with mesophase content above 70% to produce continuous carbon fibers from petroleum tar with suitable mechanical characteristics and at low cost.

BACKGROUND OF THE INVENTION

[2] Oil tar from heavy oil is made by heating and removing the lighter molecules by distillation. A tar with low molecular weight molecules, called isotropic tar, is initially formed, characterized by the absence of spheres or mesophasic regions, which behave similar to a liquid crystal. This isotropic tar is easily reliable producing carbon fibers of low mechanical properties which are commercially available.

[3] Prolonged heating of the isotropic oil tar leads to the production of a tar with heavier molecules with large mesophasic regions, which is called an anesotropic / mesophasic tar. The higher the mesophase content produced in the tar, the higher the mechanical properties of the carbon fibers produced from the tar, and the lower the times and costs for its production in the following phases (stabilization and carbonization).

[4] Producing a mesophasic tar (around 70% mesophase) that can be spun continuously has been a challenge technological because by increasing the mesophase content of an oil tar by heating, what is observed is the formation of two distinct phases that prevent this type of wiring.

[5] In an attempt to resolve the issue, several cases have been proposed. However, due to the high production costs, they have become economically unviable for large scale application. By way of example, some patent documents may be cited:

[6] US4005183 discloses a process for producing carbon fiber from a tar partially transformed into a liquid crystal called a "mesophasic state". Subsequently the pitch was spun and the fiber stabilized in an oxygen atmosphere becoming infusible, and then charred in an inert atmosphere. The mesophasic pitch, obtained from aromatic base pits, was heated to a temperature between 350 ° C and 450 ° C, which was maintained over a period of time to form small mesophase spheres, which grew in size with heat treatment time, coalesce and formed anisotropic domains up to hundreds of microns in size, depending on the initial pitch used. At a temperature of 350 ° C it would take at least one week for the percentage of mesophase to reach 40%. Already at a temperature between 400 ° C and 450 ° C the conversion would be much faster and the same percentage of mesophase could be reached in a time between 1 and 40 hours, such temperatures being preferred for this reason. After the mesophase percentage was reached, these mesophasic pits could be made into fibers by conventional melt spinning, centrifugal spinning and blow spinning techniques. In order to obtain uniform fibers the pitch obtained by this technique had to be stirred immediately before spinning to make a mixture of the immiscible isotropic (non-mesophasic) and mesophasic phases that formed the pitch. The pitch to be spun should preferably have between 45 and 65% mesophase with a viscosity 30 to 60 poises (3 to 6 Pa.s) at a spinning temperature between 340 ° C and 380 ° C.

[7] From this technological framework, other documents proposing improvements in the properties of the mesophasic phase were presented. Document US4209500 which reports 100% tar production prepared by passing an inert gas through an isotropic tar at a flow rate of between 4 and 10 scfh per pound of tar (equivalent to 4.16 and 10.4) may be considered relevant. liters / min per kg tar) during the heat treatment of the tar at temperatures between 380 ° C and 430 ° C. Heating should be done under constant stirring to produce a homogeneous emulsion of the mesophase with the remaining non-mesophasic fraction, stirring and heating maintained until a completely anisotropic pitch was obtained. According to the author, at a temperature of 430 ° C, where conversion of tar into mesophase is relatively fast, a very high gas flow rate would be required, while at 380 ° C, where conversion of tar is much slower, a flow Much lower gas pressure would be required to achieve the same result. The 100% mesophasic pits produced had softening point lower than 350 ° C and viscosity less than 20 Pas and 60% pyridine insoluble at 380 ° C, while the conventional 100% mesophasic pits produced without stirring and without gas passage inert would be 100% pyridine insoluble. The higher solubility of the pits produced with the high flow rate of the inert gas was believed to be due to their lower molecular weight. This technology was not applied commercially due to the high flow of inert gas required in the process.

[8] Later documents emerged that taught the production of carbon fibers from mesophasic oil tar, pressure separation of mesophase, use of oxidizing gas, and solvent fractionation. Also the technology has not been commercially applied due to the high solvent volumes and production cost. [9] WO 2012/162766 teaches a process which allows the production of isotropic tar with high chemical characteristics and high yields. This isotropic tar when used as a production load of a mesophasic tar, allows to obtain a mesophasic tar with high levels of mesophase, that is, predominantly anisotropic.

[10] To date, therefore, the market has had as its option only tar-derived carbon fibers made from tar tar or synthetic tar. Tar tar has been reduced in supply and avoided, especially in more developed countries, due to occupational and environmental health due to its harmful properties to the human organism and aggressive to nature. Synthetic tar is extremely expensive, so its production is reserved for application in extremely noble areas.

[11] Thus the technique still lacks a process capable of producing continuous carbon fibers with high mechanical properties from heavy petroleum derivatives, which is the object of the invention presented herein.

SUMMARY OF THE INVENTION

[12] The present invention is a process for producing high mechanical strength continuous carbon fibers from oil tar containing high mesophase content (above 70%) which is obtained by controlled bubbling of a low flow inert gas of less than 4,00 L / min per kg tar within an isotropic tar also produced from heavy petroleum residue containing heteroatomic hydrocarbons. This tar produced when heated to about 80 ° C above its softening point produces only one liquid phase, allowing its continuous spinning and subsequent stabilization and carbonization.

[13] The invention also contemplates the bubblers used in the present process which were specifically developed for provide the low flow rate required for the production of reliable high mesophase chisels.

BRIEF DESCRIPTION OF THE FIGURES

[14] Figure 1 shows a first type of bubbler used in the process of the invention.

[15] Figure 2 shows a second type of nozzle-provided bubbler used in the process of the invention.

[16] Figure 3 shows details of the nozzles used in the second type of bubbler.

DETAILED DESCRIPTION OF THE INVENTION

[17] The reliable mesophasic tar production process described below applies to loads consisting of isotropic dies with a density between 1, 200 and 1, 300, and anisotropy of up to 10%.

[18] Broadly, the process is based on the use of low inert gas flow rates of less than 4.16 L / min per kg tar with the use of bubblers when producing mesophasic pits.

[19] The use of inert gas flow rates of less than 4.00 L / min per kg tar with bubblers promotes the removal of heteroatomic hydrocarbons, particularly polar, and especially sulfuric, from the reaction medium. to avoid undesirable chemical reactions during heating of the mesophasic tar. Such undesirable reactions resemble a kind of "vulcanization" in the oil tar, forming two phases, and increasing the elasticity of the tar, which ultimately prevents its continuous spinning. Reliable oil pits were produced with S contents below 0.95% and mesophase content above 70%.

[20] Thus, the present invention addresses the production of reliable mesophasic pitch, said process including the following steps:

- introduce a charge consisting of an isotropic oil tar into a reactor with at least one bubbler and agitator; subjecting the filler to a first heating step to a temperature of 250 ° C and stirring under an inert gas flow rate of 0,3 to 1,2L / min per kg tar;

subjecting the charge to a second heating step to a temperature of 350 ° C under agitation and raising the inert gas flow to the range between 0,40 and 4,00L / min per kg tar.

subject the charge to a third heating step to a temperature of 430 ° C under agitation and inert gas flow in the range 0.40 to 4.00L / min per kg tar and maintain this temperature for a period of time, ranging from 30 to 120 minutes, to promote the formation of a reliable mesophasic pitch;

[21] To ensure a good distribution of inert gas within the material, and the low gas flows required for the process of the present invention, two bubblers were developed.

[22] Thus, a first bubbler (100) developed for application in the process of the invention is shown in Figure 1. It basically comprises a small diameter pipe (101), bent to form a first vertical rod-shaped portion (102). ), which penetrates into the reactor to the height of its stirrer (not shown in the figure), and a second closed circular ring-shaped portion (103), forming an angle of 90 ° to the vertical rod (102) and provided with small holes (104) distributed in the upper surface of said ring for controlled release of inert gas to be introduced into the reactor. At the end of the vertical rod a nozzle (105) is installed for connection to the inert gas source.

[23] This first bubbler was tested in the lab, performing well, as will be shown later in the examples.

[24] In order to improve the gas / liquid ratio in the reaction medium a second bubbler (200), shown in Figure 2, was also developed for application in the process of the invention. Similar to the first bubbler, it basically comprises a small diameter pipe 201 bent to form a first vertical rod-shaped portion 202 which penetrates into the reactor to the height of its stirrer (not shown). in the figure), and a second closed circular ring-shaped portion (203) at an angle of 90 ° to the vertical rod (202) and provided with small holes (204) distributed in the upper surface of said ring for release. inert gas to be introduced into the reactor, and in each hole (204) a venturi ejector (205) is installed. This type of ejector creates a depression when high-speed gas passes through your throat which can be used to suck the material being processed into it. Thus, the ejector 205 is provided with a side bore 206 through which the pitch is sucked, optimizing the efficiency of the gas / liquid mixture. At the end of the rod a nozzle (207) is installed for connection to the inert gas source (not shown in Figure 2). An ejector is shown in detail in Figure 3.

The following examples correspond to laboratory scale experiments without limiting the scope of the reliable mesophasic pitch production process, described in detail hereinafter.

EXAMPLES

[25] The following comparative examples demonstrate that low and well-distributed inert gas flow rates are sufficient to produce mesophasic tar filaments of uniform characteristics.

The tables presented in the examples below have:

Where:

IT = insoluble in toluene

Inmp = N-methylpyrrolidinone insoluble

IQ = quinoline insoluble

CV = coking value

D = specific mass PA = softening point

Aniso = anisotropy

C - Percentage content of CARBON

H - Hydrogen percentage content

N - NITROGEN percentage content

S - Sulfur percentage content

EXAMPLE 1

[26] A first experiment was conducted in the laboratory to produce an 87% mesophase mesophasic pitch, as taught in US 4,209,500 as a reference. Using a 1.2 liter 700g tar reactor, a single tube dipped into the tar was used as a bubbler, whose inert gas (nitrogen) flow rate was 5L / min (equivalent to 6.87 scfh / pound). ) for a time period of 60 minutes.

[27] However, using a 3.8 liter tar reactor with 2500g tar capacity, the inert gas flow needed to be increased to 25L / min (equivalent to 9.61 scfh / pound) as suggested. In the reference, with the increase of the flow the production of reliable mesophasic pits Extrapolating these values to an industrial scale, it is verified that they are quite high values and that significantly cost the process.

[28] Attempting to employ lower flow rates caused phase separation within the reactor, producing a mesophasic pitch with elastic characteristics that could not be spun.

[29] The physicochemical parameters of the starting isotropic tar are shown in table 1 and the results of CHNS analysis of the same tar in table 2. Table 3 and table 4 show respectively the physicochemical and CHNS for the mesophasic tar produced. TABLE 1

TABLE 2

TABLE 3

TABLE 4

EXAMPLE 2

[30] The experiment described in example 1 was repeated using bubblers specially developed for the invention in order to better distribute and reduce inert gas flow to values lower than those suggested by US4209500 (in the range 4 to 4). 10 scfh / Pound of tar, or the equivalent of 4.16 to 10.4 liters / min per kg of tar). A treatment time of up to 90 minutes at a temperature range of 430 ° C was established as the basis for the test.

[31] The first type of bubbler developed was initially used. For the invention, which is shown in Figure 1. For application in the experiment, a bubbler with a 1/4 inch (0.63 cm) diameter tube with four 1mm holes in the circular ring, facing upwards, was made. . The bubbler was immersed in the tar to the height of the stirrer. The experiment was carried out in a 3.8 liter tar reactor with a capacity of 2500g tar at a temperature of 430 ° C for a time of 60 minutes with a flow rate of 5.77 scfh / pound (value still within the document value range). US 4209500 from reference). With the use of this type of bubbler reliable pits have been produced. The physicochemical parameters of the starting isotropic tar are presented in table 5 and the results of CHNS analysis of the same tar in table 6. Table 7 and table 8 show, respectively, the physicochemical and CHNS results for the mesophasic tar produced.

TABLE 5

TABLE 6

TABLE 7

Tar IT (%) INMP IQ (%) CV (%) PA D Mesophasic anise (%) (° C) (g / cm ³ ) (%)

66.7 53.1 50.9 90 321 1.296 89 TABLE 8

EXAMPLE 3

[32] In this experiment the second type of bubbler developed for the invention was used, which is shown in Figure 2. A bubbler with a 1/4 inch diameter tube with three holes in the circular ring facing upwards was made. , in which Venturi type ejectors were installed. The experiment was carried out at a temperature in the range of 350 ° C to a level of 430 ° C, remaining at this level for a time of 90 minutes, with a flow rate of 2.0 L / min per kg of tar (equivalent to 1.9 scfh / pound), which is half the value suggested in US 4209500. A mesophasic pitch with 93% mesophase has been obtained with characteristics that allow it to be continuously wired.

[33] The physicochemical parameters of the starting isotropic tar are shown in table 9 and the results of CHNS analysis of the same tar in table 10. Table 11 and table 12 show respectively the physicochemical and CHNS for the mesophasic tar produced.

TABLE 9

Tar IT (%) INMP IQ (%) CV (%) PA (° C) D Isotropic Aniso (%) (g / cm ³ ) (%)

20.7 7.7 3.5 45 86.2 1.218 5 TABLE 10

TABLE 12

[34] Despite this promising result, further experiments were carried out using a larger scale, so that it can be proved that with a lower flow of inert gas it is possible to produce a mesophasic pitch with characteristics that allow its continuous wiring.

EXAMPLE 4

[35] An isotropic tar with the physicochemical characteristics shown in table 13 and the values for CHNS in table 14 below was used as raw material:

TABLE 13

IT Inmp IQ VC n PA Aniso u

Tar (%) (%) (%) (%) (° C) (%) Isotropic 26.7 12.28 6.7 52 1, 277 105 48 TABLE 14

[36] In a 75 liter reactor, 64kg of the isotropic tar mentioned above was placed, and heating was started with the temperature of the reactor resistances set to 250 ° C to allow the tar to soften slowly. Then the temperature of the reactor resistances was then raised to 700 ° C and the lid was positioned to close the reactor. Stirring was started with the internal temperature at 250 ° C and nitrogen bubbling with a flow rate of 20 liters / min was started to prevent clogging of the bubbler. With the internal temperature at 350 ° C, the nitrogen bubbling flow rate increased to 40 liters / min using the first special type of bubbler (100) developed for the invention with seven holes.

[37] It should be noted that according to US4209500 patent used for comparison purposes, for this mass of material the minimum expected flow rate would be 262 liters / min.

[38] The temperature reached 430 ° C after 65 minutes of warming up. The material was at 430 ° C for one hour and thirty minutes, when the tar was discharged. At the end, 39 kg of a mesophasic tar (60.9%) were collected, without phase precipitation, whose result of the physicochemical analysis can be seen in table 15 and CHNS analysis in table 16.

TABLE 15

IT Inmp IQ VC PA Aniso

D

Tar (%) (%) (%) (%) (° C) (%) Mesophasic 69.9 65.0 63.4 86 1, 340 273 86 TABLE 16

[39] This tar spun continuously through a 12 hole array.

EXAMPLE 5

[40] An isotropic tar with the physicochemical characteristics shown in table 17 and the CHNS results shown in table 18 below was used as raw material. In order to better compare the results obtained with the experiments using the bubblers developed, and the tar with these same characteristics was used as raw material in the following examples.

TABLE 17

TABLE 18

[41] In a 3.8 liter reactor was placed 2.5kg of isotropic tar, which was fed into the reactor in solid form and then fused to allow the reactor to close. Nitrogen flow of 3 liters / min was maintained from the start of heating to the start of heating to prevent bubbler clogging. With 52 minutes of heating and a temperature of 250 ° C, stirring was switched on. THE Nitrogen bubbling, using the first type of special bubbler (100) developed for the invention, with four holes with a flow rate of 5 liters / min, began with 73 minutes of heating at 350 ° C. According to US4209500 used for comparison purposes, for this mass of material the expected minimum flow rate would be 10.25 liters / min.

[42] The landing reached 104 minutes of warm-up. The tar was 95 minutes at the 430 ° C level and was discharged. 1308.2g (52.3%) of reliable pitch and no phase precipitation were obtained. The result of physicochemical analysis is shown in table 19, while the result of CHNS analysis is shown in table 20 below:

TABLE 19

TABLE 20

[43] The carbon fiber produced after stabilization and carbonization at 1500 ° C had a tensile strength of 2.9GPa and Young's modulus of 400GPa.

EXAMPLE 6

[44] In a 3.8 liter reactor were placed 2.5kg of the same isotropic tar from the previous example, which was fed into the reactor in solid form and then fused to allow the reactor to close. Nitrogen flow of 3 liters / min was maintained from the start of heating to prevent bubbler clogging. With 51 minutes heating and temperature of 250 ° C, stirring was switched on. Nitrogen bubbling was performed using the second special type of bubbler (200) developed for the invention, provided with ejectors, with a flow rate of 5 liters / min, rather than the minimum 10.25 liters / min provided in the reference document. comparison, and started with 71 minutes of heating at 350 ° C. Arrival at the landing occurred with 104 minutes of warm-up. The tar was 85 minutes at the 430 ° C level and was discharged. 1274.00 g (51.0%) of reliable pitch and no phase precipitation were obtained. The result of the physicochemical analysis is shown in table21 and the CHNS analysis result in table 22:

TABLE 21

TABLE 22

[45] The carbon fiber produced after stabilization and carbonization at 1500 ° C had a tensile strength of 3GPa and a Young modulus of 420GPa.

EXAMPLE 7

[46] In a 3.8 liter reactor were placed 2.5kg of the same isotropic tar from the previous example, which was fed into the reactor in solid form and then fused to allow the reactor to close. Nitrogen flow of 3 liters / min was maintained from the start of heating to prevent bubbler clogging. With 50 minutes of heating and temperature of 250 ° C, stirring was switched on. THE Nitrogen bubbling using the ejectors at a flow rate of 4 liters / min (instead of the minimum 10.25 liters / min provided for in the reference) began with 71 minutes of heating at 350 ° C. Arrival at the landing occurred with 100 minutes of warm-up. The tar was 95 minutes at the 430 ° C level and was discharged. 1342.9g (53.7%) of reliable tar without phase precipitation were obtained whose physicochemical analysis presented the result shown in table 23 and the result of CHNS analysis shown in table 24:

TABLE 23

TABLE 24

[47] Carbon fiber produced after stabilization and carbonization at 500 ° C showed tensile strength of 2.7GPa and Young modulus of 380GPa.

EXAMPLE 8

[48] In a 3.8 liter reactor were placed 2.5kg of the same isotropic tar from the previous example, which was fed into the reactor in solid form and then fused to allow the reactor to close. Nitrogen flow of 3 liters / min was maintained from the start of heating to prevent bubbler clogging. With 50 minutes of heating and temperature of 250 ° C, stirring was switched on. Nitrogen bubbling using the nozzles at a flow rate of 4 liters / min (instead of the minimum 10.25 liters / min provided in the reference), began with 71 minutes of heating at 350 ° C. Arrival at the landing occurred with 104 minutes of warm-up. The tar was 95 minutes at the 430 ° C level and was discharged. 1336.0g (53.4%) of reliable tar without phase precipitation were obtained, whose physicochemical analysis presented the result shown in table 25 while the result of CHNS analysis is shown in table 26:

TABLE 25

TABLE 26

EXAMPLE 9

[49] In a 3.8 liter reactor were placed 2.5kg of the same isotropic tar from the previous example, which was fed into the reactor in solid form solid and then fused to allow the reactor to close. Nitrogen flow of 3 liters / min was maintained from the start of heating to prevent bubbler clogging. With 53 minutes of heating and a temperature of 250 ° C, stirring was switched on. Nitrogen bubbling using the four-hole stem with a flow rate of 4 liters / min began with 73 minutes of heating at 350 ° C. Arrival at the landing took place with 105 minutes of warm-up. The tar was 95 minutes at the 430 ° C level and was discharged. 1395.3g (55.8%) of tar were obtained whose physicochemical analysis presented the result shown in table 27 while the CHNS analysis presented the result shown in table 28: TABLE 27

TABLE 28

[50] Examples 8 and 9, in which the 95-minute threshold time and the reduced nitrogen flow to 4 liters / min were maintained, can be compared to note the difference between the use of the bubbler stem types: four holes and rod with the ejectors.

[51] Comparing only these last two experiments, it is observed that the pitch produced using the ejectors presented the highest value for softening point (PA) and anisotropy, maintaining the same processing conditions. This indicates that the use of ejectors accelerates the release of undesirable compounds responsible for phase "vulcanization" and precipitation, allowing either the reduction of heat treatment time or the production of a tar with higher properties at the same time as heat treatment.

[52] It is therefore demonstrated that the production of a mesophasic tar (around 80% mesophase) capable of being continuously spun becomes feasible with the use of the inventive bubblers, which promote efficient gas distribution within of material.

[53] The invention has been described according to a preferred embodiment. However, it should be made clear that adjustments can be made by those skilled in the art without departing from their inventive concept, which is limited only by their claim framework.

Claims

1. PROCESS FOR PRODUCING RELIABLE MESOPHASIC OIL PICKLE FOR THE PRODUCTION OF CONTINUOUS CARBON FIBERS characterized by comprising the following steps:

introducing a charge consisting of an isotropic oil tar into a reactor with at least one bubbler and agitator;

subjecting the filler to a first heating step to a temperature of 250 ° C and stirring under an inert gas flow rate of 0.3 to 1.2 L / min per kg tar;

subject the charge to a second heating step to a temperature of 350 ° C under agitation and raise the inert gas flow rate to between 0.40 and 4.00L / min per kg tar. subject the charge to a third heating step to a temperature of 430 ° C under agitation and inert gas flow rate between 0,40 and 4,00L / min per kg tar and maintain this temperature for a period of time varying 30 to 120 minutes to promote the formation of a reliable mesophasic pitch;

2. PROCESS FOR PRODUCING RELIABLE MESOPHASIC OIL PICKLE FOR THE PRODUCTION OF CONTINUOUS CARBON FIBERS characterized by the isotropic pitch having a density between 1, 200 and 1, 300, and anisotropy of up to 10%,

Process for the production of reliable mesophasic oil tank for the production of continuous carbon fibers according to claim 1, characterized in that the bubbler comprises a small diameter pipe (101), bent to form a first portion. rod-shaped shape (102) which penetrates into the reactor to the height of its agitator, and a second closed circular ring-shaped portion (103), forming an angle of 90 ° to the vertical rod (102) and provided with small holes (104) distributed in the upper surface of said ring for controlled release of the stirrer. inert gas to be introduced into the reactor; A nozzle (105) is installed at the end of the vertical rod for connection to the inert gas source.

Process for the production of reliable mesophasic oil tank for the production of continuous carbon fibers according to claim 1, characterized in that the bubbler comprises a small diameter pipe (201) bent to form a first portion. vertical rod-shaped rod (202) which penetrates into the reactor up to the height of its stirrer, and a second closed circular ring-shaped portion (203) forming an angle of 90 ° to the vertical rod (202) and provided with small holes (204) distributed on the upper surface of said ring for controlled release of the inert gas to be introduced into the reactor, and in each hole (204) a venturi type ejector (205) is installed; ejector 205 is provided with a side bore 206 through which tar is sucked; At the end of the vertical rod a nozzle (207) is installed for connection to the inert gas source.

Process for the production of reliable mesophasic oil core for the production of continuous carbon fibers according to claim 1, characterized in that the mesophasic oil tar produced has a mesophase content above 70%, suitable for continuous spinning.

Process for the production of reliable mesophasic oil tank for the production of continuous carbon fibers according to claim 1, characterized in that it produces carbon filaments with tensile strength in the order of 3 GPa and Young's high modulus above 400. GPa

Process for the production of reliable mesophasic oil core for the production of continuous carbon fibers according to claim 1, characterized in that the mesophasic oil tar produced has an S content below 0.95%, suitable for continuous spinning. .