CN116726845A - Preparation device and method of isotropic spinnable asphalt - Google Patents
Preparation device and method of isotropic spinnable asphalt Download PDFInfo
- Publication number
- CN116726845A CN116726845A CN202310724905.2A CN202310724905A CN116726845A CN 116726845 A CN116726845 A CN 116726845A CN 202310724905 A CN202310724905 A CN 202310724905A CN 116726845 A CN116726845 A CN 116726845A
- Authority
- CN
- China
- Prior art keywords
- pipe
- double
- screw reactor
- reaction kettle
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000010426 asphalt Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims description 21
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 137
- 239000000463 material Substances 0.000 claims abstract description 92
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000007789 gas Substances 0.000 claims abstract description 38
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 238000002347 injection Methods 0.000 claims abstract description 25
- 239000007924 injection Substances 0.000 claims abstract description 25
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 23
- 238000007599 discharging Methods 0.000 claims abstract description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 33
- 238000006068 polycondensation reaction Methods 0.000 claims description 18
- 238000001125 extrusion Methods 0.000 claims description 14
- 239000003208 petroleum Substances 0.000 claims description 4
- 239000003245 coal Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 229920000049 Carbon (fiber) Polymers 0.000 abstract description 9
- 239000004917 carbon fiber Substances 0.000 abstract description 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 9
- 238000007380 fibre production Methods 0.000 abstract description 2
- 239000011295 pitch Substances 0.000 description 15
- 230000001276 controlling effect Effects 0.000 description 10
- 238000010926 purge Methods 0.000 description 9
- 238000005485 electric heating Methods 0.000 description 6
- 238000009987 spinning Methods 0.000 description 6
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- 239000005977 Ethylene Substances 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000007664 blowing Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000011269 tar Substances 0.000 description 3
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- 239000011294 coal tar pitch Substances 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 239000012814 acoustic material Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000011300 coal pitch Substances 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011271 tar pitch Substances 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/20—Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/008—Feed or outlet control devices
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
- D01F9/15—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues from coal pitch
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
- D01F9/155—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues from petroleum pitch
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Working-Up Tar And Pitch (AREA)
Abstract
The invention discloses a preparation device and a preparation method of isotropic spinnable asphalt, relates to the technical field of asphalt-based carbon fiber production, and aims to effectively solve the problems of uneven heating and poor batch stability of materials in the preparation of isotropic spinnable asphalt. The main technical scheme of the invention is as follows: an apparatus for preparing an isotropic spinnable asphalt comprising: a reaction kettle and a double-screw reactor; the upper end of the reaction kettle is connected with a feed pipe and an exhaust pipe, an air ejector pipe is arranged in the reaction kettle, a plurality of air ejector holes are uniformly distributed on the pipe wall of the air ejector pipe, and the air ejector pipe is respectively connected with an air pipe and a nitrogen pipe; the front end of the double-screw reactor is provided with a feed inlet and a gas injection port, the middle section of the double-screw reactor is provided with a first gas outlet, and the tail end of the double-screw reactor is provided with a second gas outlet; one end of the conveying pipe is connected to the lower end of the reaction kettle, the other end of the conveying pipe is connected to the feeding hole, one end of the circulating pipe is connected to the upper end of the reaction kettle, and the other end of the circulating pipe is connected to the discharging pipe of the double-screw reactor.
Description
Technical Field
The invention relates to the technical field of asphalt-based carbon fiber production, in particular to a device and a method for preparing isotropic spinnable asphalt.
Background
The industrial production of general-purpose asphalt carbon fiber is low in price, has typical properties of carbon materials, such as light weight, electric conduction, heat resistance, wear resistance and good chemical stability, is suitable for furnace body heat insulation materials, fuel cell electrodes and cement reinforcements, and can also be used for automobile brake blocks, sealing materials, acoustic materials, gas masks and the like.
The universal asphalt carbon fiber is prepared from isotropic spinnable asphalt which has rich and low raw material sources and is a byproduct of petroleum and coal chemical industry. The spinnable asphalt has higher softening point and more concentrated molecular weight distribution, has good thixotropic viscosity-temperature characteristic in spinning Wen Oufei, has uniform plastic flow behavior, and can be stably and continuously spun.
Chinese patent CN103184062a discloses a "preparation method of high softening point spinning pitch", which comprises the steps of scraping, evaporating and removing part of light components from coal tar pitch without quinoline insoluble substances under proper conditions to obtain refined pitch, thermally polycondensing the obtained refined pitch in a reaction kettle, and removing light components by secondary scraping, evaporating and removing light components to obtain the spinning pitch with high softening point of 260-275 ℃.
Chinese patent CN102776014a discloses a method for preparing petroleum-based high softening point spinning pitch, which comprises removing light components from ethylene tar by wiped film evaporation, further performing thermal polycondensation, removing light components by wiped film evaporation, and obtaining high softening point 270-285 ℃.
Chinese patent 201210541249.4 discloses a method for preparing coal-series general-purpose pitch carbon fiber, which comprises oxidizing high-purity impregnant pitch in a continuous reaction kettle to obtain high-softening-point pitch, and preparing additive composition during preparation of high-softening-point pitch for improving carbon fiber quality.
Chinese patent CN200710163857.5 discloses a method for preparing general-purpose pitch carbon fiber, which comprises placing ethylene tar with 7-10% carbon residue and 0.01-0.04% ash into a reaction kettle, and preparing spinnable pitch by air oxidation.
Chinese patent CN105885907A discloses a preparation method of general-purpose asphalt carbon fiber spinning asphalt, which adopts a combination of liquid phase oxidant oxidation and thermal polycondensation to prepare the spinning asphalt, and compared with the prior air oxidation method or thermal polycondensation method, the liquid phase oxidant is adopted to make the reaction temperature milder and the time is greatly shortened.
Chinese patent CN202011055631.5 discloses a "preparation method of general-purpose pitch-based carbon fiber", which comprises heat treating coal tar or ethylene tar as raw material to melt the raw material, heating the melted raw material to reaction temperature in inert atmosphere, introducing chlorine gas, and performing chlorination reaction to prepare pitch precursor.
In the above scheme, when the temperature rises, dehydrogenation, crosslinking, polycondensation and other reactions occur to release H 2 、H 2 O、H 2 S, small molecular weight compounds and the like, and better spinnable asphalt is obtained, but no solution is given for local material overtemperature and uneven heating in the preparation process.
Disclosure of Invention
In view of the above, the invention provides a device and a method for preparing isotropic spinnable asphalt, which mainly aim to effectively solve the problems of uneven heating and poor batch stability of materials in the preparation of the isotropic spinnable asphalt.
In order to achieve the above purpose, the present invention mainly provides the following technical solutions:
in one aspect, the present invention provides an apparatus for preparing an isotropic spinnable asphalt, the apparatus comprising: a reaction kettle and a double-screw reactor;
the upper end of the reaction kettle is connected with a feed pipe and an exhaust pipe, an air jet pipe is arranged in the reaction kettle, a plurality of air jet holes are uniformly distributed on the pipe wall of the air jet pipe, and the air jet pipe is respectively connected with an air pipe and a nitrogen pipe;
the front end of the double-screw reactor is provided with a feed inlet and a gas injection port, the middle section of the double-screw reactor is provided with a first gas outlet, and the tail end of the double-screw reactor is provided with a second gas outlet;
the device comprises a reaction kettle, a discharge pipe, a circulating pipe, a reaction kettle, a double-screw reactor and a control valve, wherein the reaction kettle is characterized by further comprising a discharge pipe and a circulating pipe, one end of the discharge pipe is connected to the lower end of the reaction kettle, the other end of the discharge pipe is connected to the feed inlet, one end of the circulating pipe is connected to the upper end of the reaction kettle, and the other end of the circulating pipe is connected to the discharge pipe of the double-screw reactor.
In another aspect, the present invention provides a method of preparing an isotropic spinnable asphalt, the method comprising: the method comprises the following steps:
(1) Firstly, materials are added into a reaction kettle through a feed pipe, the materials are stirred, the temperature of the reaction kettle is increased, meanwhile, air is introduced into the reaction kettle through an air pipe, oxidation reaction is carried out on the materials, tail gas generated by the reaction is discharged from an exhaust pipe, after a double-screw reactor is started, the materials in the reaction kettle enter the double-screw reactor through a feed conveying pipe and flow back to the reaction kettle through a circulating pipe, meanwhile, an air injection port is opened, air is injected, and the pressure of a first exhaust port and the pressure of a second exhaust port are respectively adjusted to be micro negative pressure;
(2) After the oxidation reaction is finished, maintaining the reaction temperature of the materials, closing an air pipe valve and an air injection port, simultaneously opening a nitrogen pipe valve, introducing nitrogen into the reaction kettle, and discharging the mixture of volatile components and nitrogen in the materials through an exhaust pipe, a first exhaust port and a second exhaust port;
(3) Closing a nitrogen pipe valve, opening a gas injection port, closing a circulating pipe valve, continuously feeding materials in the reaction kettle into the double-screw reactor, and performing thermal polycondensation reaction in a medium flow passage of the double-screw reactor, or performing oxidation reaction in a medium flow passage of the double-screw reactor between the gas injection port and the first gas exhaust port, and performing thermal polycondensation reaction in a medium flow passage of the double-screw reactor between the first gas exhaust port and the second gas exhaust port;
(4) And discharging the finished product material generated after the material subjected to the thermal shrinkage polymerization reaction is devolatilized through the second exhaust port through a discharge pipe.
The aim and the technical problems of the invention can be further realized by adopting the following technical measures.
Optionally, in the step (1), the material is petroleum asphalt or coal asphalt.
Optionally, in the step (1), during the oxidation reaction, the reaction temperature is 300-320 ℃, and the residence time of the materials in the twin-screw reactor is 20-50min.
Optionally, in the step (2), the residence time of the material in the twin-screw reactor is 19-21min.
Optionally, in the step (3), the residence time of the material in the twin-screw reactor is 30-50min, and the vacuum degree of the first air outlet and the vacuum degree of the second air outlet are both 50-70Pa.
Optionally, in the step (3), the oxidation reaction temperature is 300-310 ℃, and the thermal polycondensation reaction temperature is 345-360 ℃.
Optionally, in the step (4), the extrusion pressure of the twin-screw reactor is greater than 4MPa, the vacuum degree of the second air outlet is 50-70Pa, and the target softening point of the finished product material is 223-307 ℃.
Optionally, the target softening point of the finished product is 273-276 ℃.
Optionally, in the step (1) and the step (2), the reaction temperature is less than or equal to the heating temperature of the reaction kettle is less than or equal to the reaction temperature +5 ℃, and the reaction temperature is less than or equal to the heating temperature of the double-screw reactor is less than or equal to the reaction temperature +3 ℃; in the step (3) and the step (4), the reaction temperature is less than or equal to the heating temperature of the double-screw reactor is less than or equal to the reaction temperature +3℃.
By means of the technical scheme, the invention has at least the following advantages:
the reaction kettle and the double-screw reactor form a linkage circulation reaction system, the double-screw reactor is linked with the reaction kettle during the reaction and devolatilization of materials in the reaction kettle, the materials are obtained from the bottom of the reaction kettle, the materials processed by the double-screw reactor (extrusion, extrusion pressure is more than or equal to 2 MPa) flow back to the reaction kettle, and meanwhile, the effect of circulating the materials is achieved.
The material performance is regulated and controlled by the twin-screw reactor, and finally the spinnable asphalt is extruded by the twin-screw reactor, the heating temperature is strictly controlled to be less than or equal to 5 ℃ in the whole preparation process, the material is heated uniformly and is not overtemperature, and the spinnable asphalt with isotropy, which has the target softening point of +/-3 ℃, good batch-to-batch stability and excellent spinnability, can be prepared.
Drawings
Fig. 1 is a schematic structural diagram of a device for preparing isotropic spinnable asphalt according to an embodiment of the present invention.
Reference numerals in the drawings of the specification include: the reaction kettle 1, the double-screw reactor 2, the feeding pipe 3, the exhaust pipe 4, the air injection pipe 5, the air pipe 6, the nitrogen pipe 7, the air injection port 8, the first exhaust port 9, the second exhaust port 10, the feeding pipe 11 and the circulating pipe 12.
Detailed Description
In order to further describe the technical means and effects adopted for achieving the preset aim of the invention, the following detailed description refers to the specific implementation, structure, characteristics and effects according to the application of the invention with reference to the accompanying drawings and preferred embodiments. In the following description, different "an embodiment" or "an embodiment" do not necessarily refer to the same embodiment. Furthermore, the particular features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.
The invention is described in further detail below with reference to the drawings and examples.
As shown in fig. 1, in one aspect, an embodiment of the present invention provides an apparatus for preparing isotropic spinnable asphalt, which includes: a reaction kettle 1 and a double-screw reactor 2;
the upper end of the reaction kettle 1 is connected with a feed pipe 3 and an exhaust pipe 4, an air jet pipe 5 is arranged in the reaction kettle 1, a plurality of air jet holes are uniformly distributed on the pipe wall of the air jet pipe 5, and the air jet pipe 5 is respectively connected with an air pipe 6 and a nitrogen pipe 7;
the front end of the double-screw reactor 2 is provided with a feed inlet and a gas injection port 8, the middle section of the double-screw reactor 2 is provided with a first gas outlet 9, and the tail end of the double-screw reactor 2 is provided with a second gas outlet 10;
the reactor further comprises a conveying pipe 11 and a circulating pipe 12, wherein one end of the conveying pipe 11 is connected to the lower end of the reaction kettle 1, the other end of the conveying pipe is connected to the feeding hole, one end of the circulating pipe 12 is connected to the upper end of the reaction kettle 1, and the other end of the circulating pipe is connected to a discharging pipe of the double-screw reactor 2.
Specifically, the reaction kettle 1 is an intermittent reaction kettle.
Specifically, the twin-screw reactor 2 is a twin-screw extruder with a reaction function, a devolatilization function and an extrusion function, and vacuum exhaust ports (the exhaust ports have a function of preventing materials from flowing backwards) are respectively arranged at the outlet section and the middle part of the twin-screw reactor 2 and are used for removing volatile matters; an air injection port 8 is additionally arranged between the front section of the inlet section and the middle air exhaust port; the extrusion pressure is more than or equal to 2MPa; the residence time of the flowable material in the twin-screw reactor 2 is controlled between 20 and 50 minutes.
Specifically, a stirrer is arranged in the reaction kettle 1, the air ejector tube 5 is annularly arranged at the lower end of the stirrer, and a heat conducting oil jacket is arranged on the side wall of the reaction kettle 1.
Specifically, the outer surface of the medium runner shell of the double-screw reactor 2 is provided with an electric heating wire.
Specifically, when the device is operated and the materials in the reaction kettle are purged by air or nitrogen, the tail gas in the reaction kettle can be discharged through the exhaust pipe.
On the other hand, the embodiment of the invention provides a preparation method of isotropic spinnable asphalt, which comprises the following steps:
example 1
(1) Adding low-temperature coal tar pitch with ash content less than 1ppm and softening point of 38 ℃ into a reaction kettle through a feed pipe, stirring asphalt materials, introducing heat conduction oil into a jacket to raise the temperature of the reaction kettle, introducing air into the reaction kettle through an air pipe, performing oxidation reaction on the materials, controlling the heating temperature of the reaction kettle (the heat conduction oil temperature of the jacket of the reaction kettle is less than or equal to 325 ℃, the reaction temperature of the materials is 320 ℃, the reaction pressure is micro positive pressure (gauge pressure is less than or equal to 100 Pa), and the reaction duration is 4 hours.
During the air blowing oxidation reaction of the materials in the reaction kettle, the tail gas generated by the reaction is discharged from the exhaust pipe, the materials in the reaction kettle enter the double-screw reactor through the conveying pipe, air is injected into the double-screw reactor through the air injection port of the double-screw reactor, the materials and the air perform oxidation reaction in the double-screw reactor, the heating temperature of the heating wire of the double-screw reactor is controlled to be less than or equal to 323 ℃, the reaction temperature of the materials is controlled to be 320 ℃, and the pressures of the first exhaust port and the second exhaust port are micro negative pressures (gauge pressure and more than or equal to-100 Pa); the materials treated by the double-screw reactor (extrusion, extrusion pressure 2 MPa) are returned to the reaction kettle through a circulating pipe, and the materials stay in the double-screw reactor for 50min.
(2) Then maintaining the reaction temperature at 320 ℃, and carrying out micro-positive pressure nitrogen purging for 0.5 hour to remove volatile components. During the nitrogen purging period of the materials in the reaction kettle, the gas injection port of the double-screw reactor is closed, the materials in the double-screw reactor are not subjected to oxidation reaction, the temperature is kept constant at 320 ℃, the devolatilization is continued (the pressure of the first gas outlet and the second gas outlet is micro negative pressure), the materials continue to circulate between the reaction kettle and the double-screw reactor, and the residence time of the materials in the double-screw reactor is 21min.
(3) Stopping nitrogen purging of the reaction kettle, closing a circulating pipe valve, continuously feeding materials in the reaction kettle into the double-screw reactor through a conveying pipe, keeping the flowing materials in the double-screw reactor for 30min, performing thermal polycondensation reaction and devolatilization, controlling the heating temperature of an electric heating wire of the double-screw reactor to be less than or equal to 363 ℃, controlling the thermal polycondensation reaction temperature to be 360 ℃, and controlling the devolatilization operation temperature to be 360 ℃ and controlling the vacuum degree of the first exhaust port and the second exhaust port to be 70Pa.
(4) And extruding the isotropy spinnable asphalt with a softening point of 279 ℃ from the materials treated by the double-screw reactor under the condition of an extrusion pressure of 4 MPa.
Example 2
(1) Adding medium-temperature coal pitch with ash content less than 1ppm and softening point of 86 ℃ into a reaction kettle through a feed pipe, stirring pitch materials, introducing heat-conducting oil into a jacket to raise the temperature of the reaction kettle, introducing air into the reaction kettle through an air pipe, performing oxidation reaction on the materials, controlling the heating temperature of the reaction kettle (the temperature of the heat-conducting oil of the jacket of the reaction kettle is less than or equal to 305 ℃, the reaction temperature is 300 ℃, the reaction pressure is micro-positive pressure (gauge pressure is less than or equal to 100 Pa), and the reaction duration is 6 hours.
During the air blowing oxidation reaction of the materials in the reaction kettle, the tail gas generated by the reaction is discharged from the exhaust pipe, the materials in the reaction kettle enter the double-screw reactor through the conveying pipe, air is injected into the double-screw reactor through the air injection port of the double-screw reactor, the materials and the air perform oxidation reaction in the double-screw reactor, the heating temperature of the heating wire of the double-screw reactor is controlled to be less than or equal to 303 ℃, the reaction temperature of the materials is controlled to be 300 ℃, and the pressures of the first exhaust port and the second exhaust port are micro negative pressures (gauge pressure and more than or equal to-100 Pa); the materials treated by the double-screw reactor (extrusion, extrusion pressure 2.5 MPa) are returned to the reaction kettle through a circulating pipe, and the materials stay in the double-screw reactor for 20min.
(2) Then maintaining the reaction temperature at 300 ℃, and carrying out micro-positive pressure nitrogen purging for 0.5 hour to remove volatile components. And during the nitrogen purging period of the materials in the reaction kettle, the gas injection port of the double-screw reactor is closed, the materials in the double-screw reactor are not subjected to oxidation reaction, the temperature is constant at 300 ℃, the devolatilization is continued (the pressure of the first gas outlet and the pressure of the second gas outlet are both micro negative pressures), the materials continue to circulate between the reaction kettle and the double-screw reactor, and the retention time of the materials in the double-screw reactor is 19min.
(3) Stopping nitrogen purging of the reaction kettle, closing a circulating pipe valve, continuously feeding materials in the reaction kettle into the double-screw reactor through a conveying pipe, and keeping the flowing materials in the double-screw reactor for 50min for oxidation reaction, thermal polycondensation reaction and devolatilization; (1) oxidation reaction: injecting air from an air injection port of the double-screw reactor, carrying out oxidation reaction on materials and air in a medium flow passage of the double-screw reactor between the air injection port and a first air exhaust port of the double-screw reactor, and controlling the heating temperature of an electric heating wire of the double-screw reactor to be less than or equal to 303 ℃ and the material reaction temperature to be 300 ℃; (2) thermal polycondensation reaction: carrying out thermal polycondensation reaction on the material subjected to the oxidation reaction in a medium flow channel of the double-screw reactor between the first exhaust port and the second exhaust port, and controlling the heating temperature of an electric heating wire of the double-screw reactor to be less than or equal to 353 ℃ and the material reaction temperature to be 350 ℃; (3) devolatilization: the temperature of the first exhaust port is 300 ℃, the temperature of the second exhaust port is 350 ℃, and the vacuum degree of the first exhaust port and the second exhaust port is 50Pa.
(4) And extruding the isotropy spinnable asphalt with a softening point of 270 ℃ under the condition of extruding pressure of 5 MPa.
Example 3
(1) Ethylene tar pitch with ash content less than 1ppm and thick oily liquid at normal temperature is added into a reaction kettle through a feed pipe, pitch materials are stirred, a jacket is filled with heat conducting oil to raise the temperature of the reaction kettle, meanwhile, air is filled into the reaction kettle through an air pipe, the materials undergo oxidation reaction, the heating temperature of the reaction kettle (the temperature of the heat conducting oil of the jacket of the reaction kettle) is controlled to be less than or equal to 313 ℃, the reaction temperature is 308 ℃, the reaction pressure is micro positive pressure (gauge pressure is less than or equal to 100 Pa), the reaction time is 5 hours,
during the air blowing oxidation reaction of materials in the reaction kettle, tail gas generated by the reaction is discharged from the exhaust pipe, the materials in the reaction kettle enter the double-screw reactor through the conveying pipe, air is injected into the double-screw reactor through the air injection port of the double-screw reactor, the materials and the air perform oxidation reaction in the double-screw reactor, the heating temperature of the heating wire of the double-screw reactor is controlled to be less than or equal to 311 ℃, the reaction temperature of the materials is controlled to be 308 ℃, the pressures of the first exhaust port and the second exhaust port are micro negative pressures (gauge pressure and more than or equal to-100 Pa), the materials treated by the double-screw reactor (extrusion pressure and extrusion pressure are 3 MPa) flow back to the reaction kettle through the circulating pipe, and the retention time of the materials in the double-screw reactor is 20min.
(2) Then maintaining the reaction temperature at 308 ℃, and carrying out micro-positive pressure nitrogen purging for 0.5 hour to remove volatile components. And closing a gas injection port of the double-screw reactor during the nitrogen purging period of the reaction kettle, wherein the double-screw reactor does not perform oxidation reaction, keeping the temperature at 308 ℃, continuously performing devolatilization (the pressure of the first gas outlet and the pressure of the second gas outlet are both micro negative pressures), continuously circulating the materials between the reaction kettle and the double-screw reactor, and keeping the materials in the double-screw reactor for 20min.
(3) Stopping nitrogen purging of the reaction kettle, closing a circulating pipe valve, continuously feeding materials in the reaction kettle into the double-screw reactor through a conveying pipe, and then keeping the flowing materials in the double-screw reactor for 45min for oxidation reaction, thermal polycondensation reaction and devolatilization; (1) oxidation reaction: injecting air from an air injection port of the double-screw reactor, carrying out oxidation reaction on materials and air in a medium flow passage of the double-screw reactor between the air injection port and a first air exhaust port of the double-screw reactor, and controlling the heating temperature of an electric heating wire of the double-screw reactor to be less than or equal to 303 ℃ and the material reaction temperature to be 300 ℃; (2) thermal polycondensation reaction: carrying out thermal polycondensation reaction on the material subjected to the oxidation reaction in a medium flow channel of the double-screw reactor between the first exhaust port and the second exhaust port, and controlling the heating temperature of an electric heating wire of the double-screw reactor to be less than or equal to 348 ℃ and the material reaction temperature to be 345 ℃; (3) devolatilization: the temperature of the first exhaust port is 300 ℃, the temperature of the second exhaust port is 345 ℃, and the vacuum degree of the first exhaust port and the second exhaust port is 60Pa.
(4) And extruding the isotropy spinnable asphalt with the softening point of 273 ℃ from the materials treated by the double-screw reactor under the condition of extrusion pressure of 4.5 MPa.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. An apparatus for preparing an isotropic spinnable asphalt, comprising:
the upper end of the reaction kettle is connected with a feed pipe and an exhaust pipe, an air ejector pipe is arranged in the reaction kettle, a plurality of air ejector holes are uniformly distributed in the pipe wall of the air ejector pipe, and the air ejector pipe is respectively connected with an air pipe and a nitrogen pipe;
the device comprises a double-screw reactor, wherein the front end of the double-screw reactor is provided with a feed inlet and a gas injection port, the middle section of the double-screw reactor is provided with a first gas outlet, and the tail end of the double-screw reactor is provided with a second gas outlet;
the device comprises a reaction kettle, a discharge pipe, a circulating pipe, a reaction kettle, a double-screw reactor and a control valve, wherein the reaction kettle is characterized by further comprising a discharge pipe and a circulating pipe, one end of the discharge pipe is connected to the lower end of the reaction kettle, the other end of the discharge pipe is connected to the feed inlet, one end of the circulating pipe is connected to the upper end of the reaction kettle, and the other end of the circulating pipe is connected to the discharge pipe of the double-screw reactor.
2. A method for preparing isotropic spinnable asphalt, comprising the steps of:
(1) Firstly, materials are added into a reaction kettle through a feed pipe, the materials are stirred, the temperature of the reaction kettle is increased, meanwhile, air is introduced into the reaction kettle through an air pipe, oxidation reaction is carried out on the materials, tail gas generated by the reaction is discharged from an exhaust pipe, after a double-screw reactor is started, the materials in the reaction kettle enter the double-screw reactor through a feed conveying pipe and flow back to the reaction kettle through a circulating pipe, meanwhile, an air injection port is opened, air is injected, and the pressure of a first exhaust port and the pressure of a second exhaust port are respectively adjusted to be micro negative pressure;
(2) After the oxidation reaction is finished, maintaining the reaction temperature of the materials, closing an air pipe valve and an air injection port, simultaneously opening a nitrogen pipe valve, introducing nitrogen into the reaction kettle, and discharging the mixture of volatile components and nitrogen in the materials through an exhaust pipe, a first exhaust port and a second exhaust port;
(3) Closing a nitrogen pipe valve, opening a gas injection port, closing a circulating pipe valve, continuously feeding materials in the reaction kettle into the double-screw reactor, and performing thermal polycondensation reaction in a medium flow passage of the double-screw reactor, or performing oxidation reaction in a medium flow passage of the double-screw reactor between the gas injection port and the first gas exhaust port, and performing thermal polycondensation reaction in a medium flow passage of the double-screw reactor between the first gas exhaust port and the second gas exhaust port;
(4) And discharging the finished product material generated after the material subjected to the thermal shrinkage polymerization reaction is devolatilized through the second exhaust port through a discharge pipe.
3. The method for preparing the isotropic spinnable asphalt according to claim 2,
in the step (1), the material is petroleum asphalt or coal asphalt.
4. The method for preparing the isotropic spinnable asphalt according to claim 2,
in the step (1), the reaction temperature is 300-320 ℃ and the residence time of the materials in the twin-screw reactor is 20-50min during the oxidation reaction.
5. The method for preparing the isotropic spinnable asphalt according to claim 2,
in the step (2), the residence time of the material in the twin-screw reactor is 19-21min.
6. The method for preparing the isotropic spinnable asphalt according to claim 2,
in the step (3), the residence time of the materials in the double-screw reactor is 30-50min, and the vacuum degree of the first exhaust port and the vacuum degree of the second exhaust port are both 50-70Pa.
7. The method for preparing the isotropic spinnable asphalt according to claim 2,
in the step (3), the oxidation reaction temperature is 300-310 ℃, and the thermal polycondensation reaction temperature is 345-360 ℃.
8. The method for preparing the isotropic spinnable asphalt according to claim 2,
in the step (4), the extrusion pressure of the double-screw reactor is more than 4MPa, the vacuum degree of the second exhaust port is 50-70Pa, and the target softening point of the finished product material is 223-307 ℃.
9. The method for preparing an isotropic spinnable asphalt according to claim 8,
the target softening point of the finished product material is 273-276 ℃.
10. The method for preparing the isotropic spinnable asphalt according to claim 2,
in the step (1) and the step (2), the reaction temperature is less than or equal to the heating temperature of the reaction kettle and less than or equal to the reaction temperature +5 ℃, and the reaction temperature is less than or equal to the heating temperature of the double-screw reactor and less than or equal to the reaction temperature +3 ℃; in the step (3) and the step (4), the reaction temperature is less than or equal to the heating temperature of the double-screw reactor is less than or equal to the reaction temperature +3℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310724905.2A CN116726845A (en) | 2023-06-19 | 2023-06-19 | Preparation device and method of isotropic spinnable asphalt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310724905.2A CN116726845A (en) | 2023-06-19 | 2023-06-19 | Preparation device and method of isotropic spinnable asphalt |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116726845A true CN116726845A (en) | 2023-09-12 |
Family
ID=87912988
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310724905.2A Pending CN116726845A (en) | 2023-06-19 | 2023-06-19 | Preparation device and method of isotropic spinnable asphalt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116726845A (en) |
-
2023
- 2023-06-19 CN CN202310724905.2A patent/CN116726845A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20220097274A1 (en) | Method and device for directly preparing foamed polylactic acid (pla) product from pla melt | |
| MX2007004220A (en) | Continuous extrusion process for producing grafted polymers. | |
| CN108407135B (en) | Polypropylene/exfoliated-graphite composite method and its application are prepared using water auxiliary molten mixing extrusion | |
| WO2023087756A1 (en) | Supercritical carbon dioxide assisted periodic devolatilization process and device | |
| CN113388148B (en) | Preparation method of supercritical carbon dioxide assisted heat-conducting composite material | |
| CN104723528A (en) | Process for producing polymer modified asphalt waterproof coil | |
| CN108485694A (en) | A method of carbonizatin method prepares high-quality mesophase pitch altogether | |
| CN116726845A (en) | Preparation device and method of isotropic spinnable asphalt | |
| WO2024051671A1 (en) | Polymerization-termination device and method for continuous production of organopolysiloxanes | |
| CN111286353A (en) | Production system and production method of coal pitch with high coking value and low quinoline insoluble | |
| CN115160771B (en) | Homogeneous isomerism micro-crosslinking regenerated nylon and preparation method thereof | |
| WO2021237655A1 (en) | Liquid additive assisted polymer extrusion and blending method and device and use thereof | |
| JP2021024904A (en) | Method for regenerating polymer compound | |
| CN114790592A (en) | Method for preparing high-performance asphalt-based carbon fiber through rapid pre-oxidation | |
| CN1540787A (en) | Method for preparing bipolar plate made from carbon/carbon composite of fuel cell of proton exchange membrane | |
| CN115449077B (en) | Method for dehydrating alkali metal sulfide and application of method in polymerization reaction | |
| CN115404092B (en) | Method and device for continuously preparing mesophase pitch | |
| CN114933784B (en) | TPEE extrusion grade material and preparation method thereof | |
| KR0146890B1 (en) | Apparatus and method for manufacture of anisotropic pitch | |
| CN116987524A (en) | Preparation method of environment-friendly asphalt with ultrahigh softening point, asphalt and application | |
| CN114907525B (en) | Preparation method of low-VOC maleic anhydride grafted olefin polymer | |
| CN106674714A (en) | Preparation method of ethylene-vinyl acetate copolymer (EVA)/asphalt composite carbon crystal plate | |
| CN117025248A (en) | Pyrolysis method for waste plastics | |
| CN211279689U (en) | Screw extruder is used in production of polyether ether ketone polymer | |
| CN113583233B (en) | Method for preparing poly (aryl ether ketone) by premixing and poly (aryl ether ketone) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |