CN103184589A - Preparation method of PAN (polyacrylonitrile)-based carbon fiber for modifying protofilament through ammonification - Google Patents
Preparation method of PAN (polyacrylonitrile)-based carbon fiber for modifying protofilament through ammonification Download PDFInfo
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Abstract
The invention discloses a preparation method of PAN (polyacrylonitrile)-based carbon fiber for modifying protofilament through ammonification, wherein the ammonified PAN protofilament is subjected to pre-oxidation with total draft degree of -2% through 4 temperature zones. The final product of PAN-based carbon fiber is obtained through low-temperature carbonization and high-temperature carbonization. A low-temperature carbonization furnace is divided into 6 temperature zones in total, the total time of low-temperature carbonization is 90-150 seconds, and the draft degree of low-temperature carbonization is 7 per mill. A high-temperature carbonization furnace is divided into 4 temperature zones, the total time of high-temperature carbonization is 60-100 seconds, and the draft degree of high-temperature carbonization is -4 per mill. According to the invention, in the fixed temperature condition and technological conditions, different pre-oxidation times are realized by changing the operation speed of the whole production line. The average strength of the produced carbon fiber reaches 4,538MPa.
Description
Technical field
The present invention relates to polyacrylonitrile (PAN) base carbon fibre charing field, specifically is a kind ofly to accelerate pre-oxidation and improve the preparation method of PAN base carbon fibre performance by ammonification.
Background technology
Carbon fiber and composite thereof are important dual-use new materials, also are responsive strategic materials.In recent years, the market demand of China's carbon fiber progressively enlarges, and the PAN base carbon fibre is as most important applications the most a kind of carbon fiber and its development and application is subjected to common concern in the industry.The preparation of PAN base carbon fibre is divided into and mainly is divided into two processes, the preparation of precursor and pre-oxidation, carbonization process.Wherein the preparation of precursor is most important process, and the performance of precursor determines final properties of carbon; High-quality PAN precursor is the primary essential condition of making high-performance carbon fibre, and improving PAN based precursor performance can be by realizations such as polymerization, spinning, coagulation bath condition, washing conditions, and the polymerization ammonification is a kind of important method wherein.Preoxidation process is the heat-resisting trapezium structure that the linear molecule chain warp pre-oxidation of PAN based precursor under certain temperature, degree of draft and preoxidation time condition is converted into pre-oxidized fibers, forms pre-oxidized fibers.Preoxidation process is the most consuming time and to the tangible process of final carbon fiber performance impact in the carbon fiber preparation process, carbonization process is divided into low-temperature carbonization and two processes of high temperature carbonization, and pre-oxidized fibers is converted into the random graphits structure carbon fiber through low-temperature carbonization and high temperature carbonization process successively.Save cost in pre-oxidation, carbonization process, shorten pre-oxidation, carbonization time, enhancing productivity is the key that high-performance carbon fibre is produced in present industrialization.
In recent years, the experts and scholars of many carbon fiber aspects have studied the influence of ammonification to the structural evolution of PAN precursor and microstructure, and in the spinning process variation of process conditions to PAN precursor Effect on Performance.Feed a certain amount of ammonia in document and patent report the have been arranged spinning solution after the polymerization and can improve precursor and final properties of carbon, and can accelerate the pre-oxidation process, but report is not at the charing method of ammonification PAN precursor.And these researchs bias toward the research of knowwhy, and research is that ammonification is to the research of single-point influence factor in the carbon fiber preparation process, do not form pre-oxidation, the charing method of the ammonification PAN precursor of system, integral body, and because the complexity of carbon fiber preparation process, the directive function that its theory study is produced industrialization is limited.The present invention is target both from industrialization production to enhance productivity and to improve the carbon fiber mechanical property, by shortening preoxidation time and improving pre-oxidation speed and produce high performance carbon fiber.
Summary of the invention
For improving PAN base carbon fibre production efficiency of products and mechanical property thereof, the present invention proposes the preparation method of the PAN base carbon fibre of the ammoniation modified precursor of a kind of process.
Detailed process of the present invention is:
Step 1, the pre-oxidation of ammonification PAN precursor: carry out pre-oxidation by 4 humidity provinces; 4 humidity provinces, the 1st humidity province to the by low temperature to high temperature formation temperature gradient, ammonification PAN precursor by low temperature to hot operation.The speed of service of ammonification PAN precursor in preoxidation process is 3～5m/min, and the preoxidation time in each humidity province is respectively 10.0～16.5min.Ammonification PAN precursor is-2% through the total draft rate after the pre-oxidation.
Step 2, charing: charing is divided into low-temperature carbonization and two steps of high temperature cabonization, wherein:
The first step, low-temperature carbonization.To the pre-oxidized fibers low-temperature carbonization process that obtains be: 6 humidity provinces are set in the described low-temperature carbonization stove altogether, and pre-oxidized fibers is operation continuously under the traction of drawing roller, passes through each humidity province successively.The total time of low-temperature carbonization is 90～150s, and the low-temperature carbonization degree of draft is 7 ‰.Obtain the low-temperature carbonization fiber.
Second step, high temperature cabonization.The low-temperature carbonization fiber that obtains is carried out high temperature carbonization.4 humidity provinces are set in the described high temperature carbonization stove altogether, and the low-temperature carbonization fiber is operation continuously under the traction of drawing roller, carries out high temperature carbonization through each humidity province successively and handles.The total time of high temperature carbonization is 60～100s, and the high temperature carbonization degree of draft is-4%.Obtain final products PAN base carbon fibre.
4 humidity provinces have 3 temperature sections respectively in the described ammonification PAN precursor pre-oxidation, and wherein: 3 temperature sections of the 1st warm area are respectively 195 ℃, 200 ℃ and 205 ℃; 3 temperature sections of the 2nd humidity province are respectively 210 ℃, 215 ℃ and 220 ℃; 3 temperature sections of the 3rd humidity province are respectively 235 ℃, 245 ℃ and 255 ℃; 3 temperature sections of the 4th humidity province are respectively 265 ℃, 270 ℃ and 270 ℃.
The temperature of the pre-oxidized fibers that obtains being carried out 6 humidity provinces of low-temperature carbonization is respectively 400 ℃, 400 ℃, 520 ℃, 625 ℃, 750 ℃ and 750 ℃.
The temperature of the pre-oxidized fibers that obtains being carried out 4 humidity provinces of high temperature carbonization is respectively 800 ℃, 1000 ℃, 1200 ℃ and 1400 ℃.
Described low-temperature carbonization and high temperature carbonization all are to carry out in the nitrogen medium of oxygen content≤1ppm.
For the checking properties of product, carbon fiber has been carried out Mechanics Performance Testing.Testing equipment is 3365 serial universal testing machines, gauge length 200mm, and speed is 0.5cm/min, and comes calculating mean value with the Mechanics Performance Testing numerical value of ten carbon fiber samples.Test gained carbon fiber strength value by analysis and bring up to 4538MPa by 3608MPa.
Under the condition that the temperature conditions process conditions are fixed, by changing the whole production line speed of service, realize different preoxidation times in the process of the present invention.To be the structure of the most consuming time and pre-oxidized fibers and performance play a decisive role to the structural behaviour of final carbon fiber PAN precursor pre-oxidation process.The PAN precursor changes into ring-type or heat-resisting stable ladder polymer by linear macromolecule through reactions such as dehydrocyclization, crosslinked, oxidations.And the ammonification precursor can play the effect that stops polymerization owing to feed ammonia in the process of polymerization, generates the 3-aminopropionitrile, has strengthened the hydrophily of resin, in the process of pre-oxidation, is easier to be combined with oxygen, has accelerated processes such as dehydrocyclization, crosslinked, oxidation.Therefore can accelerate the pre-oxidation reaction, shorten the reaction time, enhance productivity.The present invention is both from actual production, be target to enhance productivity and to improve the carbon fiber mechanical property, by shortening preoxidation time and improving pre-oxidation speed and produce high performance carbon fiber, carbon fiber strength mean value reaches 4538MPa, is equivalent to toray T400 level level.
The performance indications table of table 1 ammonification PAN precursor
Table 2 product of the present invention and toray T300 properties of product are relatively
The specific embodiment
Embodiment one
Present embodiment is a kind of by changing the method that the tow speed of service changes preoxidation time raising polyacrylonitrile-based carbon fibre performance and production efficiency.
The detailed process of present embodiment may further comprise the steps:
Step 1, the pre-oxidation of ammonification PAN precursor: the pre-oxidation medium is compressed air, and pre-oxidation furnace adopts pre-oxidation furnace of the prior art.Described pre-oxidation furnace has 4 humidity provinces, and each humidity province has 3 temperature sections respectively.Wherein, 3 of the 1st humidity province temperature sections are respectively 195 ℃, 200 ℃ and 205 ℃; 3 temperature sections of the 2nd humidity province are respectively 210 ℃, 215 ℃ and 220 ℃; 3 temperature sections of the 3rd humidity province are respectively 235 ℃, 245 ℃ and 255 ℃; 3 temperature sections of the 4th humidity province are respectively 265 ℃, 270 ℃ and 270 ℃.Each temperature section is all controlled by thermocouple.4 humidity provinces, the 1st humidity province to the by low temperature to high temperature formation temperature gradient, the traction of ammonification PAN precursor by drawing roller by low temperature to hot operation.The speed of service of ammonification PAN precursor in preoxidation process is 3m/min, and the preoxidation time in each humidity province is respectively 16.5min.Ammonification PAN precursor is-2% through the total draft rate after the pre-oxidation, and the degree of draft in each humidity province respectively is 9 ‰, 0 ‰ ,-10 ‰ and-19 ‰.The PAN precursor forms the pre-oxidized fibers of heat-resisting trapezium structure through pre-oxidation.
Step 2, charing: charing is divided into low-temperature carbonization and two steps of high temperature cabonization, wherein:
The first step, low-temperature carbonization.Adopt existing low-temperature carbonization stove.The low-temperature carbonization process is: the pre-oxidized fibers that obtains enters low temperature carbonization furnace by drawing roller and carries out low-temperature carbonization.6 humidity provinces are set in the described low-temperature carbonization stove altogether, and each temperature of distinguishing temperature is respectively 400 ℃, 400 ℃, 520 ℃, 625 ℃, 750 ℃ and 750 ℃ from low to high, and pre-oxidized fibers is operation continuously under the traction of drawing roller, passes through each humidity province successively.The temperature of each humidity province is controlled by thermocouple respectively.In the nitrogen medium of oxygen content≤1ppm, carry out low-temperature carbonization.The total time of low-temperature carbonization is 150s, and the low-temperature carbonization degree of draft is 7 ‰.Obtain the low-temperature carbonization fiber.
Second step, high temperature cabonization.Adopt existing high temperature carbonization stove that the low-temperature carbonization fiber that obtains is carried out high temperature carbonization.The high temperature cabonization process is: 4 humidity provinces are set in the described high temperature carbonization stove altogether, each temperature of distinguishing temperature is respectively 800 ℃, 1000 ℃, 1200 ℃, 1400 ℃ from low to high, the low-temperature carbonization fiber is operation continuously under the traction of drawing roller, carries out high temperature carbonization through each humidity province successively and handles.The temperature of each humidity province is controlled by thermocouple respectively.In the nitrogen medium of oxygen content≤1ppm, carry out high temperature carbonization.The total time of high temperature carbonization is 100s, and the high temperature carbonization degree of draft is-4%.Obtain final products PAN base carbon fibre.
Present embodiment by changing the whole production line speed of service, has changed pre-oxidation, the carbonization time of ammonification PAN precursor under the fixing condition of temperature and drawing-off.Through the test of mechanical strength analyzer, present embodiment gained carbon fiber product tensile strength mean value is that 3608MPa(is as shown in table 3).
Table 3 embodiment one preparation PAN base carbon fibre performance table
Embodiment two
Present embodiment is a kind of by changing the method that the tow speed of service changes preoxidation time raising polyacrylonitrile-based carbon fibre performance and production efficiency.
The detailed process of present embodiment may further comprise the steps:
Step 1, the pre-oxidation of ammonification PAN precursor: the pre-oxidation medium is compressed air, and pre-oxidation furnace adopts pre-oxidation furnace of the prior art.Described pre-oxidation furnace has 4 humidity provinces, and each humidity province has 3 temperature sections respectively.Wherein, 3 of the 1st humidity province temperature sections are respectively 195 ℃, 200 ℃ and 205 ℃; 3 temperature sections of the 2nd humidity province are respectively 210 ℃, 215 ℃ and 220 ℃; 3 temperature sections of the 3rd humidity province are respectively 235 ℃, 245 ℃ and 255 ℃; 3 temperature sections of the 4th humidity province are respectively 265 ℃, 270 ℃ and 270 ℃.Each temperature section is all controlled by thermocouple.4 humidity provinces, the 1st humidity province to the by low temperature to high temperature formation temperature gradient, the traction of ammonification PAN precursor by drawing roller by low temperature to hot operation.The speed of service of ammonification PAN precursor in preoxidation process is 4m/min, and the preoxidation time in each humidity province is respectively 12.25min.Ammonification PAN precursor is-2% through the total draft rate after the pre-oxidation, and the degree of draft in each humidity province respectively is 9 ‰, 0 ‰ ,-10 ‰ and-19 ‰.The PAN precursor forms the pre-oxidized fibers of heat-resisting trapezium structure through pre-oxidation.
Step 2, charing: charing is divided into low-temperature carbonization and two steps of high temperature cabonization, wherein:
The first step, low-temperature carbonization.Adopt existing low-temperature carbonization stove.The low-temperature carbonization process is: the pre-oxidized fibers that obtains enters low temperature carbonization furnace by drawing roller and carries out low-temperature carbonization.6 humidity provinces are set in the described low-temperature carbonization stove altogether, and each temperature of distinguishing temperature is respectively 400 ℃, 400 ℃, 520 ℃, 625 ℃, 750 ℃ and 750 ℃ from low to high, and pre-oxidized fibers is operation continuously under the traction of drawing roller, passes through each humidity province successively.The temperature of each humidity province is controlled by thermocouple respectively.In the nitrogen medium of oxygen content≤1ppm, carry out low-temperature carbonization.The total time of low-temperature carbonization is 112.5s, and the low-temperature carbonization degree of draft is 7 ‰.Obtain the low-temperature carbonization fiber.
Second step, high temperature cabonization.Adopt existing high temperature carbonization stove that the low-temperature carbonization fiber that obtains is carried out high temperature carbonization.The high temperature cabonization process is: 4 humidity provinces are set in the described high temperature carbonization stove altogether, each temperature of distinguishing temperature is respectively 800 ℃, 1000 ℃, 1200 ℃, 1400 ℃ from low to high, the low-temperature carbonization fiber is operation continuously under the traction of drawing roller, carries out high temperature carbonization through each humidity province successively and handles.The temperature of each humidity province is controlled by thermocouple respectively.In the nitrogen medium of oxygen content≤1ppm, carry out high temperature carbonization.The total time of high temperature carbonization is 75s, and the high temperature carbonization degree of draft is-4%.Obtain final products PAN base carbon fibre.
Present embodiment by accelerating the speed of service of pre-oxidation, charing, shortens the preoxidation time of knowing clearly under the fixing condition of temperature and degree of draft.Through the test of mechanical strength analyzer, present embodiment gained carbon fiber product tensile strength mean value is that 4068MPa(is as shown in table 4).
Table 4 embodiment two preparation PAN base carbon fibre performance tables
Embodiment three
Present embodiment is a kind of by changing the method that the tow speed of service changes preoxidation time raising polyacrylonitrile-based carbon fibre performance and production efficiency.
The detailed process of present embodiment may further comprise the steps:
Step 1, the pre-oxidation of ammonification PAN precursor: the pre-oxidation medium is compressed air, and pre-oxidation furnace adopts pre-oxidation furnace of the prior art.Described pre-oxidation furnace has 4 humidity provinces, and each humidity province has 3 temperature sections respectively.Wherein, 3 of the 1st humidity province temperature sections are respectively 195 ℃, 200 ℃ and 205 ℃; 3 temperature sections of the 2nd humidity province are respectively 210 ℃, 215 ℃ and 220 ℃; 3 temperature sections of the 3rd humidity province are respectively 235 ℃, 245 ℃ and 255 ℃; 3 temperature sections of the 4th humidity province are respectively 265 ℃, 270 ℃ and 270 ℃.Each temperature section is all controlled by thermocouple.4 humidity provinces, the 1st humidity province to the by low temperature to high temperature formation temperature gradient, the traction of ammonification PAN precursor by drawing roller by low temperature to hot operation.The speed of service of ammonification PAN precursor in preoxidation process is 5m/min, and the preoxidation time in each humidity province is respectively 10min.Ammonification PAN precursor is-2% through the total draft rate after the pre-oxidation, and the degree of draft in each humidity province respectively is 9 ‰, 0 ‰ ,-10 ‰ and-19 ‰.The PAN precursor forms the pre-oxidized fibers of heat-resisting trapezium structure through pre-oxidation.
Step 2, charing: charing is divided into low-temperature carbonization and two steps of high temperature cabonization, wherein:
The first step, low-temperature carbonization.Adopt existing low-temperature carbonization stove.The low-temperature carbonization process is: the pre-oxidized fibers that obtains enters low temperature carbonization furnace by drawing roller and carries out low-temperature carbonization.6 humidity provinces are set in the described low-temperature carbonization stove altogether, and each temperature of distinguishing temperature is respectively 400 ℃, 400 ℃, 520 ℃, 625 ℃, 750 ℃ and 750 ℃ from low to high, and pre-oxidized fibers is operation continuously under the traction of drawing roller, passes through each humidity province successively.The temperature of each humidity province is controlled by thermocouple respectively.In the nitrogen medium of oxygen content≤1ppm, carry out low-temperature carbonization.The total time of low-temperature carbonization is 90s, and the low-temperature carbonization degree of draft is 7 ‰.Obtain the low-temperature carbonization fiber.
Second step, high temperature cabonization.Adopt existing high temperature carbonization stove that the low-temperature carbonization fiber that obtains is carried out high temperature carbonization.The high temperature cabonization process is: 4 humidity provinces are set in the described high temperature carbonization stove altogether, each temperature of distinguishing temperature is respectively 800 ℃, 1000 ℃, 1200 ℃, 1400 ℃ from low to high, the low-temperature carbonization fiber is operation continuously under the traction of drawing roller, carries out high temperature carbonization through each humidity province successively and handles.The temperature of each humidity province is controlled by thermocouple respectively.In the nitrogen medium of oxygen content≤1ppm, carry out high temperature carbonization.The total time of high temperature carbonization is 60s, and the high temperature carbonization degree of draft is-4%.Obtain final products PAN base carbon fibre.
Present embodiment by accelerating the speed of service of pre-oxidation, charing, shortens the preoxidation time of knowing clearly under the fixing condition of temperature and degree of draft.Through the test of mechanical strength analyzer, present embodiment gained carbon fiber product tensile strength mean value is that 4538MPa(is as shown in table 5).
Table 5 embodiment three preparation PAN base carbon fibre performance tables
Claims (5)
1. the preparation method of the PAN base carbon fibre of an ammoniation modified precursor is characterized in that, detailed process comprises and is:
Step 1, the pre-oxidation of ammonification PAN precursor: carry out pre-oxidation by 4 humidity provinces; 4 humidity provinces, the 1st humidity province to the by low temperature to high temperature formation temperature gradient, ammonification PAN precursor by low temperature to hot operation; The speed of service of ammonification PAN precursor in preoxidation process is 3～5m/min, and the preoxidation time in each humidity province is respectively 10.0～16.5min; Ammonification PAN precursor is-2% through the total draft rate after the pre-oxidation;
Step 2, charing: charing is divided into low-temperature carbonization and two steps of high temperature cabonization, wherein:
The first step, low-temperature carbonization; To the pre-oxidized fibers low-temperature carbonization process that obtains be: 6 humidity provinces are set in the described low-temperature carbonization stove altogether, and pre-oxidized fibers is operation continuously under the traction of drawing roller, passes through each humidity province successively; The total time of low-temperature carbonization is 90～150s, and the low-temperature carbonization degree of draft is 7 ‰; Obtain the low-temperature carbonization fiber;
Second step, high temperature cabonization; The low-temperature carbonization fiber that obtains is carried out high temperature carbonization; 4 humidity provinces are set in the described high temperature carbonization stove altogether, and the low-temperature carbonization fiber is operation continuously under the traction of drawing roller, carries out high temperature carbonization through each humidity province successively and handles; The total time of high temperature carbonization is 60～100s, and the high temperature carbonization degree of draft is-4%; Obtain final products PAN base carbon fibre.
2. a kind of preparation method of PAN base carbon fibre of ammoniation modified precursor according to claim 1, it is characterized in that, 4 humidity provinces have 3 temperature sections respectively in the ammonification PAN precursor pre-oxidation, and wherein: 3 temperature sections of the 1st warm area are respectively 195 ℃, 200 ℃ and 205 ℃; 3 temperature sections of the 2nd humidity province are respectively 210 ℃, 215 ℃ and 220 ℃; 3 temperature sections of the 3rd humidity province are respectively 235 ℃, 245 ℃ and 255 ℃; 3 temperature sections of the 4th humidity province are respectively 265 ℃, 270 ℃ and 270 ℃.
3. a kind of preparation method of PAN base carbon fibre of ammoniation modified precursor according to claim 1, it is characterized in that the temperature of the pre-oxidized fibers that obtains being carried out 6 humidity provinces of low-temperature carbonization is respectively 400 ℃, 400 ℃, 520 ℃, 625 ℃, 750 ℃ and 750 ℃.
4. a kind of preparation method of PAN base carbon fibre of ammoniation modified precursor according to claim 1 is characterized in that the temperature of the pre-oxidized fibers that obtains being carried out 4 humidity provinces of high temperature carbonization is respectively 800 ℃, 1000 ℃, 1200 ℃ and 1400 ℃.
5. a kind of preparation method of PAN base carbon fibre of ammoniation modified precursor according to claim 1 is characterized in that described low-temperature carbonization and high temperature carbonization all are to carry out in the nitrogen medium of oxygen content≤1ppm.
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