前苏联专利SU1590047A3 Method of producing mesophase pitch

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专利摘要:
A process for an efficient preparation of a mesophase pitch is disclosed. The process is suitable for the production of high performance carbon fibers, from a coal tar or a petroleum residual oil. More particularly, the present invention relates to a process for the preparation of a homogeneous mesophase pitch which comprises a continuous thermal treatment of a heavy oil or a pitch which does not contain quinoline insoluble fractions, in the presence or absence of an aromatic oil, subsequent distillation of the thermally treated product, recovery of a pitch with extremely low quinoline insoluble contents, hydrogenation of the pitch by continuous thermal treatment in the presence of a hydrogen-donating solvent, distillation and recovery of a hydrogenated pitch, and thermal treatment of the hydrogenated pitch. The mesophase pitch prepared by the process of the present invention is suitable for the production of high performance carbon fibers.
公开号:SU1590047A3
申请号:SU874202686
申请日:1987-05-25
公开日:1990-08-30
发明作者:Тсуситани Масатоси；Наито Сакае；Накаджима Риоиси
申请人:Кодзо Индзука И Марузен Петрокемикал Ко, Лтд (Фирма)；
IPC主号:

专利说明:

This invention relates to a method for producing mesophilic pitch used to produce high quality carbon fibers from coal tar, and can be used in the coal chemical industry.
High-quality carbon fibers have a negligible amount, high tensile strength and a high modulus of elasticity, and are currently used: they are used as composites; these are composite materials used in aircraft manufacturing, manufacturing-equipment inventory. industrial robots, etc.
The purpose of the invention is to obtain a spinning pitch for the production of carbon fibers.
Example 1. Coal tar is subjected to a single distillation at a temperature of 280 ° C and atmospheric pressure to obtain a heavy component in an amount of 80% by weight of coal tar. After dissolving it in a double amount of cc1-shool, the resulting insoluble fractions are removed by filtration and the filtrate after removal of xylene is used as a refined heavy component. In tab. 1 shows the properties of the heavy component and the refined heavy component.
1 ma.ch. refined heavy component and 1 ma.h. absorbing oil with a boiling range of 240-280 ° C is continuously pumped through pumps through a tubular reactor with an internal diameter of 6 mm and a length of 40 m, immersed in a molten salt bath, and the mixture is subjected to heat treatment at a temperature of 490-530 C and a pressure of 2 MPa for 228 s. The heat-treated products are immediately sent to a single distillation column and subjected to one-time distillation at 480 ° C and atmospheric pressure to obtain a pitch with a high softening point. The obtained quantities and properties of the pitches are given in Table. 2
1 ma.ch. pitches with a high softening temperature and 2 mach. hydrogenated anthracene oil, respectively, are mixed, the resulting solution is fed continuously to a second, tubular reactor with an internal diameter of 8 mm and a length of 60 m, immersed in a bath
molten salt, and heated at 440 ° C under a pressure of 5 MPa for 86 minutes After the reactor, the product is additionally heated in a preheater and sent to a transfer column, where it is subjected to a single distillation at temperature, temperature and atmospheric pressure to obtain hydrogenated pitches with a high softening point. The resulting quantities and properties of hydrogenated pitch are also given in Table. 2
Into 500 ml polymerization flasks, respectively, 100 g each of the hydrogenated high temperature softening pitches are placed and subjected to heat treatment with a molten salt bath for 105–150 min, and during this time gaseous nitrogen is bubbled through the peck 8 l / min.
The resulting mesophase beams are spun in a spinning device having a nozzle with an orifice diameter of 0.25 mm and a length of 0.75 mm at 348 C. The resulting pitch fibers are made infusible by heat treatment for 20 minutes in air and then carbonized at atmospheric nitrogen to get carbon fibers.
The conditions of heat treatments and spinning and the properties of mesophase pitches and carbon fibers are summarized in Table. 3.. Example 2. 1 ma.h. refined heavy component whose properties are presented in Table. 1. and 0.75 ma.ch. the absorbing oil is heat treated at a temperature of 510 C and a pressure of 2 MPa for 228 s in the same tubular kai reactor in example 1, and subjected to a single distillation under the conditions of example 1 to obtain a pitch with a high softening temperature, having an initial softening temperature , the content of the components that are not soluble in xylene is 55.8% by weight, and the components that are not soluble in the quinoline - 0.3% by weight. The pitch yield is 29.2% by weight of the refined heavy component.
1 ma.ch. pitch with a high softening temperature is mixed with 3 ma.h. hydrogenated anthracene oil. The mixture is continuously heated in a tubular reactor and separated by a single
51590047
by distillation under conditions identical to those of example 1. The hydrogenated pitch has an initial softening temperature of 185 C. The content is insoluble
; in the xylene, the fraction is 53.2% by mass, and the fraction not soluble in the quinoline is by mass%. Vycod of hydrogenated pitch is 23.0 wt.% Of the refined heavy component.
Hydrogenated pitch is subjected to heat treatment in a bath at a temperature of molten salt for about 140 minutes, as in Example 1. According to
ten
Example 4. 1 mac. pitch with a high softening temperature, obtained in Example 2, is mixed with 2 parts by weight. hydrogenated anthracene oil and subjected to heat treatment in the same tubular reactor, similarly to example 1, at a temperature and pressure of 5 MPa for 83 minutes. The heat-treated product is subjected to a single distillation under conditions identical to example 1 to obtain a hydrogenated pitch having an initial temperature softened mesophase pitch has jj or 171 ° C. The content is not dissolved
softening temperature, Mettler softening temperature of 316 C. The content of the fraction insoluble in xylene is 95.6% by mass, insoluble in the quinoline fraction -. 11.4 wt.%, And mesophases - 100 rel.%.
Carbon fibers obtained from mesophase pitch as in Example 1 have a strength of 269 kg / mm and a modulus of elasticity of 15.8 t / m
PRI m e. R., 3. 1 MA. CH. pitch with a high softening temperature obtained in the first stage in experiment 1, whose properties are listed in Table. 2, is mixed with 2 ma.h, hydrogenated quinoline, which contains 60% by weight of tetrahydroquinoline, and the mixture is subjected to heat treatment in the same tubular reactor and under conditions similar to example 1. Then, the heat-treated product is subjected to single distillation at hydrogenated pitch having an initial softening temperature of 173 ° C. The concentration of xylene insoluble fractions is 46.5 wt.% and the quinoline-insoluble fractions - 0.3 wt.%.
20
25
thirty
35
40
in xylene, the fractions comprise wt.%, and the quinoline-insoluble fractions - 0.4 wt.%.
Hydrogenated pitch is subjected to heat treatment. In a bath at a temperature of molten salt of 450 s and atmospheric pressure for .135 min. The resulting mesophase pitch has an initial softening temperature of 272 with a Mettler softening temperature. The content of insoluble in xylene fractions is 91.2 wt. .% quinoline-insoluble fractions - 18.7 wt.%, and mesophases - 90%.
The hydrocarbon fibers obtained from the mesophase pitch of Example 1 have a tensile strength of 264 kg / mm and a modulus of elasticity of 14.6 t / mm.
Example 5 (comparative). T zhelm component, whose properties are listed in Table. 1, without removing free carbons and xylene insoluble fractions and without using aromatic oils as a diluent in the first treatment step under conditions identical to those of Example 2. In this case, the first continuous tubular reactor clogs after 3 hours.
Example 5 (comparative). T zhelm component, whose properties are listed in Table. 1, without removing free carbons and xylene insoluble fractions and without using aromatic oils as a diluent in the first treatment step under conditions identical to those of Example 2. In this case, the first continuous tubular reactor clogs after 3 hours.
Example 6 (comparative). Refined heavy component whose properties are listed in Table. 1 in primer 1, is heat treated in an autoclave with.
Hydrogenated pitch is subjected to heat. jc treatment in a bath at a temperature of molten salt and at atmospheric pressure for 180 minutes.
The resulting mesophase pitch has on-.
initial softening temperature, 5Q cues 5 min. During this treatment, the softening temperature in accordance with the Met. Tler pressure is maintained at a level of 2 MPa. 314 C. The content of the xylene insoluble fractions is 93.9% by weight. quinoline-insoluble fractions - 14.9 wt.%, and mesophases - 100%.
Carbon fibers obtained from mesophase pitch as in Example 1 have a tensile strength of 263 kg / mm and a modulus of elasticity of 15.6 t / mm.
It takes about 2 hours to heat the refined heavy component. After cooling and spitting of the heat-treated product from the autoclave, it was established that the coke-like substance was deposited on the inner surface of the steamer of the autoclave. Light fractions are removed from the passage.
Example 4. 1 mac. pitch with a high softening temperature, obtained in example 2, is mixed with 2 ma.h. hydrogenated anthracene oil and subjected to heat treatment in the same tubular reactor, similarly to example 1, at a temperature and pressure of 5 MPa for 83 minutes The heat-treated product is subjected to a single distillation under conditions identical to Example 1 to obtain a hydrogenated pitch having an initial softening temperature of 171 ° C. The content is not dissolved.
20
five
0
five
0
in xylene, the fractions comprise wt.%, and the quinoline-insoluble fractions - 0.4 wt.%.
Hydrogenated pitch is subjected to heat treatment. In a bath at a temperature of molten salt for 450 seconds and atmospheric pressure for .135 minutes. The resulting mesophase pitch has an initial softening temperature of 272 with a Mettler softening temperature. The content of the xylene insoluble fractions is 91.2% by weight of the quinoline insoluble fractions - 18.7% by weight and the mesophases - 90%.
The hydrocarbon fibers obtained from the mesophase pitch of Example 1 have a tensile strength of 264 kg / mm and a modulus of elasticity of 14.6 t / mm.
Example 5 (comparative). T zhelm component, whose properties are listed in Table. 1, without removing free carbons and xylene insoluble fractions and without using aromatic oils as a diluent in the first treatment step under conditions identical to those of Example 2. In this case, the first continuous tubular reactor clogs after 3 hours.
Example 6 (comparative). Refined heavy component whose properties are listed in Table. 1 in primer 1, is heat treated in an autoclave with.
c
.
Q cue 5 min. During this treatment, the pressure is maintained at a level of 2 MPa.
5Q cues 5 min. During this treatment, the pressure is maintained at a level of 2 MPa.
It takes about 2 hours to heat the refined heavy component. After cooling and spitting of the heat-treated product from the autoclave, it was established that the coke-like substance was deposited on the inner surface of the steamer of the autoclave. Light fractions are removed from the heat-treated product by vacuum distillation to obtain a pitch with a high softening temperature, having an initial softening temperature of 160 ° C and a fraction of the quinoline soluble in the quinoline 2% by weight. By loading the pitch thus obtained without filtration into a liter autoclave together with a double quantity
20
25
ten
tetrahydroquinoline and when heated to 80 minutes with self-adjusting pressure, coke formation is observed on the inner surface of the autoclave wall. 15
The hydrogenated pitch obtained after removal of the solvent contains 3.5% by weight of quinoline-insoluble fractions. The pitch is subjected to heat treatment according to example 1 for.
: 100 min to obtain a mesophase. : pitch with the initial temperature dg-: theni 275 ° C. The content of the insoluble: quinoline fractions is 30.0% by weight. Attempts to do this
pitch in the conditions of example 1 does not 1trivod t to a positive effect due to
: frequent fiber breaks.
Example 7. Purified iron component prepared in Example 1 30
: without the use of absorption oil, is subjected to heat treatment first in the first tubular reactor at a pressure of 1 MPa, for 322 s at different temperatures (from 430 to jj 460 ° C). In each experiment, the heat-treated material was immediately sent to a single-distillation column, operating at the same temperature as the tubular reactor, and the distillation was once distilled at atmospheric pressure in the presence of a pre-heated nitrogen stream at a rate of 3 liters / min. fed to the bottom part of the distillation column. dB Thus, a high softening point peck is obtained from the bottom of the column. Temperatures used, properties of the resulting pitches with
effects in the second tubular reactor at a temperature of 420 C and a pressure of 5 MPa for 80 minutes. The material subjected to heat treatment is immediately sent to a single distillation column, where the temperature is maintained at 46 ° C and atmospheric pressure. The hydrogenated pitch is taken from the bottom part of the second single distillation column. The yield of hydrogenated pitch from the purified heavy component is 18.8% by weight; Peck has the following properties: the temperature of the beginning of softening, the content of xylene-soluble substances is 43.6 wt.%, And quinoline-insoluble substances - 0, .1 wt.%.
Hydrogenated pitch is subjected to heat treatment according to Example 1 in a salt bath at 450 ° C and atmospheric pressure for 165 minutes, resulting in the production of mesophase pitch having the following characteristics: content of mesophase 95 rel.%, Initial softening temperature gcheni mettler 323 ° C; the content of xylene-soluble substances is 91.6% by weight, and quinolin-insoluble substances is 21.7% by weight.
The mesophase pitch is extended and melted by melting according to Example 1. The resulting fibers are subjected to calibration at 1000 C. Thus, the resulting carbon fibers have a tensile strength of 233 kg / mm and a modulus of elasticity of 13.9 t / mm,
The yield of mesophase pitch from hydrogenated pitch is 79.8% by weight.
Example 8. 1 ma.h. the purified heavy component prepared according to example 1 is shifted from 0.78 May, h. absorb the oil and the mixture is subjected to heat treatment in the first tubular reactor at a temperature of 490 C and a pressure of 2.5 MPa for 114 s. The material after heat treatment is immediately sent to the column for single evaporation and
By a high softening point and by-distillation, at a temperature, the course of the resulting pitches is given in 80 ° C and atmospheric pressure. As a result, from the bottom part of the single distillation column, Peck with high temperature softening temperature is diverted to high softening temperature. The calculations prepared in experiment 6, the mixture of high-temperature pitch is crushed and dissolved in a double mix of purified heavy com- bl. four .
the amount of hydrogenated quinoline (containing 60 wt.% tetrahydroquinoline) f and then the mixture is subjected to thermal
ponenta is 25.2 wt.%. High-temperature pitch has the following properties: the onset temperature is g

effects in the second tubular reactor at a temperature of 420 C and a pressure of 5 MPa for 80 minutes. The material subjected to heat treatment is immediately sent to a single distillation column, where the temperature is maintained at 46 ° C and atmospheric pressure. The hydrogenated pitch is taken from the bottom part of the second single distillation column. The yield of hydrogenated pitch from the purified heavy component is 18.8% by weight; Peck has the following properties: the temperature of the beginning of softening, the content of xylene-soluble substances is 43.6 wt.%, And quinoline-insoluble substances - 0, .1 wt.%.
Hydrogenated pitch is subjected to heat treatment according to Example 1 in a salt bath at 450 ° C and atmospheric pressure for 165 minutes, resulting in the production of mesophase pitch having the following characteristics: content of mesophase 95 rel.%, Initial softening temperature gcheni mettler 323 ° C; the content of xylene-soluble substances is 91.6% by weight, and quinolin-insoluble substances is 21.7% by weight.
The mesophase pitch is extended and melted by melting according to Example 1. The resulting fibers are subjected to calibration at 1000 C. Thus, the resulting carbon fibers have a tensile strength of 233 kg / mm and a modulus of elasticity of 13.9 t / mm,
The yield of mesophase pitch from hydrogenated pitch is 79.8% by weight.
Example 8. 1 ma.h. the purified heavy component prepared according to example 1 is shifted from 0.78 May, h. The residual oil and the mixture are heat treated in the first tubular reactor with the result of discharging a high softening point from the bottom of a single distillation column. The high temperature softening pitch of the purified heavy component is 25.2% by weight. The high-temperature pitch has the following properties: the softening onset temperature is 152 ° C; the content of xylene-soluble substances is 51.5 wt.%, quinolin-insoluble substances - 0.1 wt.%.
High softening point pitch is dissolved in twice the amount of hydrogenated quinoline containing 60% by weight of tetrahydroquinoline, and the mixture is heat treated in a second tubular reactor at a temperature of 440 ° C and a pressure of 5 MPa for 85 minutes, after which the material is subjected to a single distillation at atmospheric pressure. As a result, hydrogenated pitch is made from the bottom of the column. Its yield from the purified heavy component is 18.4% by weight. The resulting pitch has the following properties: the softening onset temperature is 172 ° C; the content of xylene soluble components is 49.8 wt.%, the quinoline-insoluble components - 0.2 wt.%.
Hydrogenated pitch is subjected to heat treatment in a salt bath at 450 ° C and atmospheric pressure for .160 minutes in a stream of nitrogen. Pass at a rate of 8 l / min. As a result, mesophasic pitch is obtained with the following properties: softening onset temperature; softening temperature according to Mettler 321 ° C; the content of substances that are not soluble in xylene is 92.3% by weight; substances that are not soluble in quinoline are .17.2% by weight, and that of mesophases is 95 rel.%. The output of the mesophase pitch from the hydrogenated pitch 79.9 wt.
The transfer of the mesophase pitch and imparting to it infusibility is carried out according to Example-1. Then the fibers are carbonized at 1000 ° C. The resulting carbon fibers have a tensile strength of 244 kg / mm, a modulus of elasticity of 14.8 tons / mm.
Example 9. The hydrogenated pitch prepared according to Example 7 is subjected to heat treatment according to Example 1, using a similar polymerization flask with a volume of 500 ml. Herodess is carried out at atmospheric pressure, the temperature of the salt bath is 430 - 450 C in a stream of nitrogen, which is passed at a rate of 8 l / min. The processing time and properties of the mesophase pitch are given in Table. five
Example 10. 1 mac. pitch with high softening temperature, prepared according to example 2, solution
0
five
0
five
0
five
0
five
0
five
The mixture is hydrogenated anthracene oil twice and the mixture is subjected to heat treatment in a second tubular reactor at a temperature of 440 ° C and a pressure of 5 MPa for Z 72 minutes. After heat treatment, the material is immediately sent to a single distillation column. at temperature and atmospheric pressure. As a result, hydrogenated pitch is obtained from the bottom of the single-distillation column. The yield of hydrogenated pitch from the purified heavy component is 24.2% by weight. Peck has the following properties: initial softening temperature of 181 ° C; the content of xylene-soluble substances is 57.2 wt.%, quinolin-insoluble substances - 0.7 wt.%.
1.5 kg of hydrogenated pitch is loaded into a stainless steel reactor and subjected to heat treatment at atmospheric pressure and temperature for 240 minutes in a stream of nitrogen; skipped at a rate of 60 l / min, to obtain a mesophase pitch.
The yield of mesophase pitch from hydrogenated pitch is 77.5% by weight. The product has the following properties: initial softening temperature of 279 ° C; The softening point according to Mettler, the content of xylene-soluble substances is .90.6% by weight, quinolin-insoluble substances - 20.7% by weight, and mesophases - 95 rel.%.
The obtained pitch is subjected to spinning and gives it a low melting strength as in Example 1. As a result, fibers are obtained which are subjected to carbonization at 1000 C. Thus, the obtained fibers have a tensile strength of 253 kg / mm and a modulus of elasticity of 14.6 t / mm.
. Example 11. A high softening point pitch prepared in Example 1 is mixed and dissolved in twice the amount of hydrogenated quinoline (tetrahydroquinoline content is 60% by weight) and the mixture is used as a feedstock during heat treatment in the second tubular reactor. Heat treatment is carried out at different reaction conditions: at a temperature of 405-440 ° C, a pressure of 2-5 MPa, and a duration of 45-86 minutes.
The heat treated material to remove the solvent used is distilled under reduced pressure and the separated solvent is analyzed on gases with an oxygen graph, and the content of tetrahydroquinoline in it is determined. Gases are also collected that are contained in the second tubular bath at a temperature of 470 ° C and atmospheric pressure for 60 minutes. The result is a mesophase pitch with a content of mesophase 80 Rel,%. However, mesophase pitch has a high initial softening point () and a high content of quinoline-insoluble substances (47.1 wt.%).
tom reactor during the reaction, and analy- | (I compared the results achieved
They are measured on a gas chromatograph to determine hydrogen gas.
According to the content of tetrahydroquinoline in the fresh solvent and in the separated solvent, as well as by the amount of 15: hydrogen and the gas phase, the amount of hydrogen transferred during the thermal treatment in the second tube is determined;
In tab. 6 shows the magnitudes of the absorption of hydrogen in the second reactor reactor under different reaction conditions.
From the data table. 6, it follows that a higher absorption reaches 25 when the heat treatment is carried out in the second tubular reactor at higher temperatures, pressures and with a longer process time. The product obtained from the reactor, JQ, according to example 3, corresponds to the product obtained in experiment 24, the product after heat treatment, obtained in experiment 16, is distilled once under conditions similar to example 3, and a hydrogenated pitch is obtained with the following properties: onset temperature The softening content of xylene-soluble substances is 47.6% by weight, and the content of noline-insoluble substances is 0.2% by weight.
The yield of hydrogenated pitch from the purified heavy component is 22.7% by weight. Hydrogenated pitch is subjected to heat treatment in a 45-salt salt bath at temperature and atmospheric pressure for 240 minutes, bypassing a stream of nitrogen at a rate of 8 l / min. As a result, a mesophase puck is obtained, having the following properties: a softening onset temperature of 274 ° C; the softening point according to Mettler, the content of xylosensable substances is 85.2 wt.%, the quinoline-insoluble substances - 55 22.1 wt.%, and mesophases - 85 rel.%.
Next, the high softening point peck prepared according to Example 1 is heat treated on
35
in the case where pitch is obtained without hydrogenation, and in the case when the wire is hydrogenated, it is clear that the properties of the mesophase pitch obtained by hydration are significantly improved (data at low absorption of hydrogen equal to only 1.2 wt.% ).
Thus, according to the proposed method, a mesophynt is obtained from which carbon fibers are obtained, having a tensile strength of 233,269 kg / mm and a modulus of elasticity of 13.9 - 15.8 t / mm2.

权利要求:
Claims (1)
[1]
Invention Formula
The method of obtaining mesophase pitch by hydrogenating coal tar pitch at a temperature of 405 -, pressure 2-5 MPa for 45 - 86 minutes, subsequent heat treatment of the obtained hydrogenate at atmospheric pressure at 410 - for 105 - 330 minutes to obtain the desired product, which differs so that in order to obtain a spinning pitch for the production of carbon fibers, the original coal tar pitch obtained by distillation and not containing quinoline-insoluble compounds is subjected to continuous heating in a tubular reactor round 430–530 ° C, pressure 1.0– 2.5 MPa for 114–322 s without or in the presence of an absorption oil, having a boiling range of 240 280 ° C and not containing insoluble xylene compounds, taken in a weight ratio to the tar equal to 0.75-1: 1, the resulting product is subjected to a single distillation in a column at a temperature of 430–480 ° C and atmospheric pressure to obtain from the bottom of the pitch column having an initial softening temperature of 128-1174 ° C and containing 0–0, 9% by weight of quinolin-insoluble compounds and 35.1 - 67.2% by weight of x-solvent-soluble compounds
Compared the results achieved

in the case when a pitch is obtained without hydrogenation, and in the case when hydrogenation is carried out, it is clear that the properties of the mesophase pitch obtained by hydrogenation are significantly improved (even at low hydrogen absorption values of only 1.2% by weight) .
Thus, according to the proposed method, a mesofauna-pitch is obtained, from which carbon fibers having a tensile strength of 233-269 kg / mm and a modulus of elasticity of 13.9-15.8 tonnes / mm2 are obtained.
Invention Formula
The method of obtaining mesophase pitch by hydrogenating coal tar pitch at a temperature of 405 -, pressure 2-5 MPa for 45 - 86 min, followed by heat treatment of the obtained hydrogenate at atmospheric pressure at 410 - for 105 - 330 min to obtain the desired product, so that, in order to obtain a spinning pitch for the production of carbon fibers, the original coal tar pitch obtained by distillation and not containing quinoline-insoluble compounds is subjected to continuous heating in a tubular reactor 430–530 ° C, pressure 1.0–2.5 MPa for 114–322 s without or in the presence of an absorption oil having a boiling range of 240– 280 ° C and not containing xylene-insoluble compounds, taken in mass ratio to tar, equal to 0.75 - 1: 1, the resulting product is subjected to a single distillation in a column at a temperature of 430 - 480 C and atmospheric pressure to obtain from the bottom of a pitch column having an initial softening temperature of 128 - 174 C and containing O - 0.9% by weight of quinolin-insoluble compounds and 35.1 - 67.2% by weight of x-soluble compounds13
In addition, the pitch is mixed with a hydrogen donor — hydrogenated anthracene oil or hydrogenated quinoline containing 60% by weight of tetrahydroquinoline, taken in a mass ratio of 1: 2–3, with hydrogenation in a tubular reactor; the hydrogenated product is subjected to single distillation in a column at a temperature of 455- 465 C and atmospheric pressure to produce in the bottom of the pitch, having an initial softening temperature of 167- 187 C and containing 0.1 First stage
Heat treatment temperature, ° С 490 - Pitch yield to the refined heavy component, wt.% 27.1
The initial temperature is softer.
no, C
Xylene insoluble fraction, wt.% 4 €, 5
Insoluble in quinoline fraction, wt.%
59004714
1.2 wt% of quinoline-insoluble compounds and 43.6-58,.% Of xylene-soluble compounds that are sent for heat treatment to obtain during heat treatment of the target product having a Kettler 314 - softening temperature, containing 11.4 - 28 , 4 wt.% Quinoliner 0 soluble compounds, 85.2 95, 6 wt.% Xylene-soluble compounds, and 85-100 rel.% Mesophase, determined by polarization microscope.
Table 1
table 2
510520530
28,630,332,2
156163169
52,959,867.2
0.20.30.9
Second phase
Pitch yield to the refined heavy component, wt.%
Initial softening temperature, C
Xylene insoluble fractions, maCo%
Insoluble in quinoline fraction, wt.%
Meophase pitch
The holding time of the third heat treatment, min 150 150 120 105 Starting temperature softening, C -277 273 279 276
The softening temperature according to the method of Mettler, s316 317 322 319
Insoluble in xylene fraction, wt.% 95.5 95.2 92.3 94.3
Insoluble in quinoline fraction, wt.% 16.0 13.3 15.7 13.2
The content of the mesophase,% 90 909585
Carbon fiber
Razrysh strength, kg / mm 267 268258242
The modulus of elasticity, t / mm 15.3 15-1515,114.2
Indicators
Heat treatment temperature, С
Temperature . distillation, C; The output of the pitch to the purified heavy component, wt.%
Initial softening temperature, C
22.2 24.3 26.6 27.9
170
176
182
187
48.7 52.0 54.0 58.2
0.4
0.5
0.7 1.2
Table. four
Experience

440 440
450 450
460 460
29.3 26.3 24.4
143
157
174
17
Xylene insoluble substances, wt.%
Quinoline-insoluble substances, wt.%
Salt bath temperature, s Duration of treatment, min. Initial softening temperature, s
Mettler softening temperature, s
Xylene soluble substances, May.%
Quinoline-insoluble substances May. %
The content of mesophases, otn.%
Temperature, C405405 420430430 430430
Pressure, MPa5552355555
Time min 4586 864545 4558 8686
Hydrogen absorption by pitch
with high fever
softening, wt.% 1,21,7 2,31,31,7 1,92,1 2,63,0
159Q047
18 Continuation of table 4
35.1 41.3 48.5 57.1 00 O 0.1
440440450450 450
240270150165 180
282288275282 290
321326319323 328
92,593,789,691,693,4
20,625,218,021,7 28,4
951009095 100

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同族专利:

公开号 | 公开日

DE3770873D1|1991-07-25|

JPH0437873B2|1992-06-22|

CN87103787A|1987-12-23|

CN1015990B|1992-03-25|

EP0247565B1|1991-06-19|

EP0247565A1|1987-12-02|

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法律状态:

优先权:

申请号 | 申请日 | 专利标题

JP61119299A|JPH0437873B2|1986-05-26|1986-05-26|

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