CN105401262A - Middle-modulus carbon fiber preparation method based on rapid spinning and high denier precursor - Google Patents

Middle-modulus carbon fiber preparation method based on rapid spinning and high denier precursor Download PDF

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Publication number
CN105401262A
CN105401262A CN201510960119.8A CN201510960119A CN105401262A CN 105401262 A CN105401262 A CN 105401262A CN 201510960119 A CN201510960119 A CN 201510960119A CN 105401262 A CN105401262 A CN 105401262A
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low
carbon fiber
temperature carbonization
temperature
oxidation
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连峰
郭鹏宗
张家好
杨平
欧阳新峰
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China Composites Group Corporation Ltd
Zhongfu Shenying Carbon Fiber Co Ltd
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China Composites Group Corporation Ltd
Zhongfu Shenying Carbon Fiber Co Ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/21Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/22Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Inorganic Fibers (AREA)

Abstract

The invention discloses a middle-modulus carbon fiber preparation method based on rapid spinning and high denier precursor, and belongs to the field of high-performance carbon fiber preparation method. The middle-modulus carbon fiber preparation method comprises following steps: PAN precursor is delivered into a pre-oxidation furnace for pre-oxidation so as to obtain a pre-oxidized fiber body with a density ranging from 1.33 to 1.36g/cm<3>; the pre-oxidized fiber body is delivered into a low temperature carbonization furnace for low temperature carbonization so as to obtain a low temperature carbonized fiber body; the low temperature carbonized fiber body is delivered into a high temperature carbonization furnace for high temperature carbonization, and the carbon fiber with tensile strength ranging from 4500 to 5100MPa, tensile modulus ranging from 270 to 310GPa, and filament diameter ranging from 6 to 10<mu>m is obtained via carbonization. The middle-modulus carbon fiber preparation method is capable of realizing synchronous increasing of carbon fiber tensile modulus and strength, and solving key problems that the tensile strength of middle-modulus carbon fiber is reduced, and cost is high.

Description

A kind of based on modules carbon fibre preparation method in quick spinning and high fiber number precursor
Technical field
The present invention relates to the preparation method field of high-performance carbon fibre, be specifically related to a kind of based on modules carbon fibre preparation method in quick spinning and high fiber number precursor.
Background technology
Modulus is one of of paramount importance performance indications of carbon fiber, carry out composite Materials Design overriding concern parameter, as reinforcing material, the modulus of composite is mainly provided by carbon fiber, directly determine DIMENSIONAL STABILITY and the non-deformability of composite material structural member, affect the many factors of carbon fiber stretch modulus, the wherein precursor degree of orientation and carburizing temperature having the greatest impact to modulus, the precursor of high-orientation and regularity is easy to the carbon fiber obtaining high-modulus on the one hand, and more high-carbon tensile fiber modulus is higher for carbon fiber temperature on the other hand.But carbon fiber tensile strength raises first to raise with carburizing temperature and reduces afterwards, flex point is had to exist, therefore obtain high strength and modulus simultaneously and there is higher technical difficulty, the thin dawn of precursor, that fiber obtains more uniform institutional framework in coagulation forming and preoxidation process, and then obtain the carbon fiber product of high strength, but thin dawnization significantly can reduce the production efficiency of carbon fiber, production cost raises, be unfavorable for promoting the commercial market of Price Sensitive, in Vehicles Collected from Market, modules carbon fibre filament diameter is commonly less than 5 μm, the line density of 12K product is at below 500g/km, production cost is high, this is also that domestic middle modules carbon fibre has demand but the few main cause of consumption.
Summary of the invention
The object of the invention is to the defect for prior art and deficiency, there is provided a kind of reasonable in design based on modules carbon fibre preparation method in quick spinning and high fiber number precursor, realize the Synchronous lifting of carbon fiber stretch modulus and intensity, solve middle modules carbon fibre TENSILE STRENGTH decline and cost occupy high key issue.
For achieving the above object, the technical solution used in the present invention is: its preparation method is as follows:
Step 1: by high molecular, high solids content and full-bodied polymerization stoste, after de-list, deaeration and ammoniated treatment, high-pressure filteration removing microgel and impurity;
Step 2: after stoste step 1 obtained is sprayed by spinning head, give its 2-5 positive drawing-off doubly, thread realizes molecular chain orientation and thin dawn under the effect of uniaxially drafting force, then in low temperature, low dense coagulating bath, carries out double diffusion and is separated, and forms as-spun fibre;
Step 3: as-spun fibre step 2 obtained carries out washing, water leads, after densification, then implement steam drafting, obtain carbon fibre precursor;
Step 4: the PAN precursor that specification step 3 obtained is 12K/24K, fiber number is 0.9 ~ 2.0dtex is put into pre-oxidation furnace and carried out pre-oxidation, Pre oxidation is at 230 ~ 270 DEG C, degree of draft is-15 ~ 0%, preoxidation time is 40 ~ 60min, obtains the pre-oxidized fibers body that density is 1.33 ~ 1.36g/cm3;
Step 5: be that the pre-oxidized fibers body of 1.33 ~ 1.36g/cm3 is put into low temperature carbonization furnace and carried out low-temperature carbonization by step 4 Midst density, the temperature of low-temperature carbonization is 400 ~ 800 DEG C, and degree of draft is 0 ~ 5%, and the low-temperature carbonization time is 40 ~ 120s, low-temperature carbonization corpus fibrosum, doubling grade is 1 grade;
Step 6: the low-temperature carbonization corpus fibrosum in step 5 is put into high temperature carbonization furnace and carries out high temperature cabonization process, the temperature of high temperature cabonization is 1500 ~ 1800 DEG C, degree of draft is-2 ~-6%, the high temperature cabonization time is 30 ~ 80s, after carbonization, the final TENSILE STRENGTH that obtains is at 4500 ~ 5100MPa, stretch modulus is at 270 ~ 310GPa, and filament diameter is the carbon fiber of 6-10 μm.
Beneficial effect of the present invention is:
1. the filament surfaces prepared of dry-jet wet-spinning is smooth, defect is few, internal organizational structure is fine and close, hole is few, the few surface defects of corresponding carbon fiber, more easily obtain the carbon fiber of high strength, carbon fiber tensile strength is lost few under higher carburizing temperature, is suitable for preparing high strength, middle modulus carbon fiber.This precursor adopts dry-jet wet-spinning technique preparation, high molecular, high solids content and full-bodied polymerization stoste, after de-list, deaeration and ammoniated treatment, high-pressure filteration removing microgel and impurity, have employed higher precursor fiber number, fiber number value controls at 0.9-2.0dtex, can prepare the specifications not of the same race such as 12K/24K;
2, adopt the mode of Wind Volume, large wind speed, vertical blowing, reach the uniformity of pre-oxidation, achieve high pre-oxidation initial temperature and rapid preoxidation simultaneously.Pre-oxidation hot blast speed is at more than 2m/s, initial Pre oxidation more than 230 DEG C, preoxidation time controls at 40 ~ 60min, solve dry-jet wet-spinning filament surfaces smooth, without groove, cross section is regular rounded, specific area is little, tow bulk density is high, in preoxidation process, oxygen is not easily to tow diffusion inside, the heat of pre-oxidation simultaneously not easily sheds, and tow internal oxidation degree is low and accumulation of heat is many, easily produces fault of construction in low-temperature carbonization section, cause lousiness even fracture of wire, have a strong impact on the problem of carbon fiber performance;
3, preoxidation process adopts certain drawing-off, suppress chemical shrinkage and physical constriction, dry-jet wet-spinning precursor due to drafting multiple large, fiber internal stress is high, contraction in preoxidation process is large, in order to prevent, tow tension is excessive causes molecular chain rupture, and general employing bears drawing-off, according to the difference in pre-oxidation stage, adopt different negative drawing-off amounts, by tow tension monitoring adjustment tow drawing-off amount, this pre-oxidation degree of draft is-15 ~ 0%, 12K carbon fibre tow tension force is 10-20N;
4, this high temperature cabonization temperature is at 1500 DEG C-1800 DEG C, the high temperature cabonization time is at 30-80S, high temperature cabonization degree of draft is between-2 ~-6%, by controlling carbon fiber surface defect and crystalline size, realize carbon fiber tensile strength to move with after high temperature cabonization temperature flex point, namely in 1600-1800 DEG C carbon fiber tensile strength without significantly sacrificing, high temperature cabonization temperature is the key factor realizing modulus in carbon fiber, the fiber number of this precursor is higher, compared with the high-strength middle modules carbon fibre precursor at thin dawn, molecular weight is low, strand regularity is little, the degree of orientation is low;
5, modules carbon fibre in being prepared by secondary high-temperature carbonization on high-strength dry-jet wet-spinning carbon fiber basis, the method can break pre-oxidation and the unmatched problem of carbonization speed, low cost is realized by rapid preoxidation in the pre-oxidation stage, can proper extension carbonization time in the high temperature cabonization stage, thus reduction carburizing temperature, reduce loss of strength, first carry out except glue process to carbon fiber before carrying out secondary high-temperature carbonization;
6, middle modulus carbon fiber raises due to stretch modulus, and toughness reduces, and in composite processing forming process, easily occurs that monofilament fractures, wearing and tearing etc., produces lousiness, affects shaping continuity on the one hand; Composite materials property is caused to decline on the other hand, carbon fiber strength utilization rate is low, for the composite processing processing performance of modules carbon fibre in evaluation, worked out carbon fiber spilt filament detection method, carbon fibre tow under certain tension state, by several deflector roll with certain angle, deflector roll is through surface treatment, reduce the damage to silk, then collect the lousiness of tow performance after deflector roll, and weigh.When identical tow tension and roll body angle, the lousiness of generation is few, and the abrasion resistance properties of carbon fiber is good;
7, NOL ring is the typical method evaluating laminated structure part in carbon fiber winding, winding process is adopted to prepare NOL sample, then TENSILE STRENGTH and the stretch modulus of NOL is tested, according to NOL TENSILE STRENGTH and fiber volume fraction and carbon fiber multifilament TENSILE STRENGTH, calculate the rate of utilization of strength of carbon fiber in NOL ring, ganoid carbon fiber damages few in forming process, rate of utilization of strength is relatively high, these related products have smooth surface, and in NOL, carbon fiber strength utilization rate reaches more than 85%.
Detailed description of the invention
Detailed description of the invention one:
The technical scheme that this detailed description of the invention adopts is: its preparation method is as follows:
Be 1.05dtex by precursor fiber number, specification is that the PAN precursor of 12K is put into pre-oxidation furnace and carried out pre-oxidation, Pre oxidation is at 260 DEG C, preoxidation time is 45min, pre-oxidation degree of draft is-10%, after the ejection of stoste thread, gives its 2-5 positive drawing-off doubly, thread realizes molecular chain orientation and thin dawn under the effect of uniaxially drafting force, and obtaining pre-oxidized fibers volume density is 1.342g/cm3, be that the pre-oxidized fibers body of 1.342g/cm3 is put into low temperature carbonization furnace and carried out double diffusion in low temperature, low dense coagulating bath and be separated by density, the temperature of low-temperature carbonization is 780 DEG C, degree of draft is 2%, and the low-temperature carbonization time is 60s, and the low-temperature carbonization corpus fibrosum doubling grade obtained is 1 grade, the low-temperature carbonization corpus fibrosum of 1 grade of doubling is washed, water lead with densification after, put into high temperature carbonization furnace and carry out high temperature cabonization, the temperature of high temperature cabonization is 1750 DEG C, degree of draft is-5%, the high temperature cabonization time is 70s, fiber carries out high power steam drafting, steam drafting adopts two-stage drafting system, the first order is preliminary draft section, effect is preheating tow, whole tow is made to be in homogeneous drawing-off state, and improve the drawability of tow, for the high drafting of the second level, steam drafting multiple is more than 4 times, with the lifting of the further raising and carbon fiber mechanical property that realize fiber-wall-element model degree, the carbon fiber tensile strength obtained is at 5100Mpa, stretch modulus is at 293Gpa.Spinning of this detailed description of the invention is fast between 300-450m/min, and the pre-oxidation caused for reducing dissolvent residual is melted also, and control tow solvent residual amount within 60ppm, solvent recovering rate reaches 99.5-100%.
The beneficial effect of this detailed description of the invention: the Synchronous lifting realizing carbon fiber stretch modulus and intensity, solves the decline of middle modules carbon fibre TENSILE STRENGTH and cost occupies high key issue.
Detailed description of the invention two:
The technical scheme that this detailed description of the invention adopts is: its preparation method is as follows:
Be 1.16dtex by precursor fiber number, specification is that the PAN precursor of 12K is put into pre-oxidation furnace and carried out pre-oxidation, and Pre oxidation is at 270 DEG C, and preoxidation time is 40min, and pre-oxidation degree of draft is-8%, and pre-oxidized fibers volume density is 1.345g/cm3; Be that the pre-oxidized fibers body of 1.345g/cm3 is put into low temperature carbonization furnace and carried out low-temperature carbonization by density, the temperature of low-temperature carbonization is 780 DEG C, and degree of draft is 3%, and the low-temperature carbonization time is 60s, and the low-temperature carbonization corpus fibrosum doubling grade obtained is 1.5 grades; The low-temperature carbonization corpus fibrosum of 1.5 grades of doublings is put into high temperature carbonization furnace and carries out high temperature cabonization, the temperature of high temperature cabonization is 1800 DEG C, and degree of draft is-4.5%, and the high temperature cabonization time is 70s, and the carbon fiber tensile strength obtained is at 4900Mpa, and stretch modulus is at 302Gpa.
Detailed description of the invention three:
The technical scheme that this detailed description of the invention adopts is: its preparation method is as follows: be 1.18dtex by precursor fiber number, specification is that the PAN precursor of 12K is put into pre-oxidation furnace and carried out pre-oxidation, Pre oxidation is at 265 DEG C, preoxidation time is 45min, pre-oxidation degree of draft is-8%, and pre-oxidized fibers volume density is 1.338g/cm3; Be that the pre-oxidized fibers body of 1.338g/cm3 is put into low temperature carbonization furnace and carried out low-temperature carbonization by density, the temperature of low-temperature carbonization is 760 DEG C, and degree of draft is 5%, and the low-temperature carbonization time is 60s, and the low-temperature carbonization corpus fibrosum doubling grade obtained is 2 grades; The low-temperature carbonization corpus fibrosum of 2 grades of doublings is put into high temperature carbonization furnace and carries out high temperature cabonization, the temperature of high temperature cabonization is 1750 DEG C, and degree of draft is-4.5%, and the high temperature cabonization time is 70s, and the carbon fiber tensile strength obtained is at 4700Mpa, and stretch modulus is at 288Gpa.
Detailed description of the invention four:
The technical scheme that this detailed description of the invention adopts is: its preparation method is as follows: be 1.12dtex by precursor fiber number, specification is that the PAN precursor of 12K is put into pre-oxidation furnace and carried out pre-oxidation, Pre oxidation is at 270 DEG C, preoxidation time is 45min, pre-oxidation degree of draft is-10%, and pre-oxidized fibers volume density is 1.349g/cm3; Be that the pre-oxidized fibers body of 1.349g/cm3 is put into low temperature carbonization furnace and carried out low-temperature carbonization by density, the temperature of low-temperature carbonization is 780 DEG C, and degree of draft is 3%, and the low-temperature carbonization time is 60s, and the low-temperature carbonization corpus fibrosum doubling grade obtained is 1.5 grades; The low-temperature carbonization corpus fibrosum of 1.5 grades of doublings is put into high temperature carbonization furnace and carries out high temperature cabonization, the temperature of high temperature cabonization is 1650 DEG C, and degree of draft is-4%, and the high temperature cabonization time is 70s, and the carbon fiber tensile strength obtained is at 4900Mpa, and stretch modulus is at 277Gpa.
Detailed description of the invention five:
A kind of based on modules carbon fibre preparation method in quick spinning and high fiber number precursor, be 1.20dtex by precursor fiber number, specification is that the PAN precursor of 12K is put into pre-oxidation furnace and carried out pre-oxidation, Pre oxidation is at 266 DEG C, preoxidation time is 45min, pre-oxidation degree of draft is-10%, and pre-oxidized fibers volume density is 1.341g/cm3; Be that the pre-oxidized fibers body of 1.341g/cm3 is put into low temperature carbonization furnace and carried out low-temperature carbonization by density, the temperature of low-temperature carbonization is 780 DEG C, and degree of draft is 5%, and the low-temperature carbonization time is 60s, and the low-temperature carbonization corpus fibrosum doubling grade obtained is 2.0 grades; The low-temperature carbonization corpus fibrosum of 2.0 grades of doublings is put into high temperature carbonization furnace and carries out high temperature cabonization, the temperature of high temperature cabonization is 1600 DEG C, and degree of draft is-4%, and the high temperature cabonization time is 70s, and the carbon fiber tensile strength obtained is at 4700Mpa, and stretch modulus is at 274Gpa.
Detailed description of the invention six:
The technical scheme that this detailed description of the invention adopts is: its preparation method is as follows: be 1.03dtex by precursor fiber number, specification is that the PAN precursor of 12K is put into pre-oxidation furnace and carried out pre-oxidation, Pre oxidation is at 269 DEG C, preoxidation time is 45min, pre-oxidation degree of draft is-10%, and pre-oxidized fibers volume density is 1.351g/cm3; Be that the pre-oxidized fibers body of 1.351g/cm3 is put into low temperature carbonization furnace and carried out low-temperature carbonization by density, the temperature of low-temperature carbonization is 780 DEG C, and degree of draft is 2%, and the low-temperature carbonization time is 60s, and the low-temperature carbonization corpus fibrosum doubling grade obtained is 1.0 grades; The low-temperature carbonization corpus fibrosum of 1.0 grades of doublings is put into high temperature carbonization furnace and carries out high temperature cabonization, the temperature of high temperature cabonization is 1700 DEG C, and degree of draft is-5%, and the high temperature cabonization time is 70s, and the carbon fiber tensile strength obtained is at 5000Mpa, and stretch modulus is at 292Gpa.
Detailed description of the invention seven:
The technical scheme that this detailed description of the invention adopts is: its preparation method is as follows: be 1.24dtex by precursor fiber number, specification is that the PAN precursor of 12K is put into pre-oxidation furnace and carried out pre-oxidation, Pre oxidation is at 260 DEG C, preoxidation time is 45min, pre-oxidation degree of draft is-10%, and pre-oxidized fibers volume density is 1.341g/cm3; Be that the pre-oxidized fibers body of 1.341g/cm3 is put into low temperature carbonization furnace and carried out low-temperature carbonization by density, the temperature of low-temperature carbonization is 780 DEG C, and degree of draft is 5%, and the low-temperature carbonization time is 60s, and the low-temperature carbonization corpus fibrosum doubling grade obtained is 1.5 grades; The low-temperature carbonization corpus fibrosum of 1.5 grades of doublings is put into high temperature carbonization furnace and carries out high temperature cabonization, the temperature of high temperature cabonization is 1750 DEG C, and degree of draft is-3%, and the high temperature cabonization time is 70s, and the carbon fiber tensile strength obtained is at 4600Mpa, and stretch modulus is at 294Gpa.
Detailed description of the invention eight:
The technical scheme that this detailed description of the invention adopts is: its preparation method is as follows: be 1.10dtex by precursor fiber number, specification is that the PAN precursor of 24K is put into pre-oxidation furnace and carried out pre-oxidation, Pre oxidation is at 270 DEG C, preoxidation time is 45min, pre-oxidation degree of draft is-8%, and pre-oxidized fibers volume density is 1.354g/cm3; Be that the pre-oxidized fibers body of 1.354g/cm3 is put into low temperature carbonization furnace and carried out low-temperature carbonization by density, the temperature of low-temperature carbonization is 780 DEG C, and degree of draft is 1%, and the low-temperature carbonization time is 60s, and the low-temperature carbonization corpus fibrosum doubling grade obtained is 1.0 grades; The low-temperature carbonization corpus fibrosum of 1.0 grades of doublings is put into high temperature carbonization furnace and carries out high temperature cabonization, the temperature of high temperature cabonization is 1700 DEG C, and degree of draft is-4%, and the high temperature cabonization time is 70s, and the carbon fiber tensile strength obtained is at 4800Mpa, and stretch modulus is at 272Gpa.The above, only in order to technical scheme of the present invention to be described and unrestricted, other amendment that those of ordinary skill in the art make technical scheme of the present invention or equivalently to replace, only otherwise depart from the spirit and scope of technical solution of the present invention, all should be encompassed in the middle of right of the present invention.
Detailed description of the invention nine:
The technical scheme that this detailed description of the invention adopts is: its preparation method is as follows: be 1.03dtex by precursor fiber number, specification is that the PAN precursor of 12K is put into pre-oxidation furnace and carried out pre-oxidation, Pre oxidation is at 269 DEG C, preoxidation time is 45min, pre-oxidation degree of draft is-10%, and pre-oxidized fibers volume density is 1.351g/cm3; Be that the pre-oxidized fibers body of 1.351g/cm3 is put into low temperature carbonization furnace and carried out low-temperature carbonization by density, the temperature of low-temperature carbonization is 780 DEG C, and degree of draft is 2%, and the low-temperature carbonization time is 60s, and the low-temperature carbonization corpus fibrosum doubling grade obtained is 1.0 grades; The low-temperature carbonization corpus fibrosum of 1.0 grades of doublings is put into high temperature carbonization furnace and carries out high temperature cabonization, the temperature of high temperature cabonization is 1200 DEG C, and degree of draft is-5%, and the high temperature cabonization time is 60s, and the carbon fiber tensile strength obtained is at 5200Mpa, and stretch modulus is at 232Gpa; The standard modulus carbon fiber of acquisition is carried out secondary high-temperature carbonization, and the temperature of high temperature cabonization is 1700 DEG C, and degree of draft is-1%, and the high temperature cabonization time is 70s, and the carbon fiber tensile strength obtained is at 5000Mpa, and stretch modulus is at 292Gpa.

Claims (3)

1., based on a modules carbon fibre preparation method in quick spinning and high fiber number precursor, it is characterized in that: its preparation method is as follows:
Step 1): by high molecular, high solids content and full-bodied polymerization stoste, after de-list, deaeration and ammoniated treatment, high-pressure filteration removing microgel and impurity;
Step 2): by step 1) after the stoste that obtains sprays by spinning head, give its 2-5 positive drawing-off doubly, thread realizes molecular chain orientation and thin dawn under the effect of uniaxially drafting force, then in low temperature, low dense coagulating bath, carries out double diffusion and is separated, and forms as-spun fibre;
Step 3): by step 2) as-spun fibre that obtains carries out washing, water leads, after densification, then implement steam drafting, obtain carbon fibre precursor;
Step 4): by step 3) specification that obtains is 12K/24K, fiber number is 0.9 ~ 2.0dtex PAN precursor puts into pre-oxidation furnace and carries out pre-oxidation, Pre oxidation is at 230 ~ 270 DEG C, degree of draft is-15 ~ 0%, preoxidation time is 40 ~ 60min, obtains the pre-oxidized fibers body that density is 1.33 ~ 1.36g/cm3;
Step 5): by step 4) Midst density is that the pre-oxidized fibers body of 1.33 ~ 1.36g/cm3 is put into low temperature carbonization furnace and carried out low-temperature carbonization, the temperature of low-temperature carbonization is 400 ~ 800 DEG C, degree of draft is 0 ~ 5%, the low-temperature carbonization time is 40 ~ 120s, obtain low-temperature carbonization corpus fibrosum, doubling grade is 1 grade;
Step 6): by step 5) in low-temperature carbonization corpus fibrosum put into high temperature carbonization furnace and carry out high temperature cabonization process, degree of draft is-2 ~-6%, the high temperature cabonization time is 30 ~ 80s, after carbonization, the final TENSILE STRENGTH that obtains is at 4500 ~ 5100MPa, stretch modulus is at 270 ~ 310GPa, and filament diameter is the carbon fiber of 6-10 μm.
2. according to claim 1 a kind of based on modules carbon fibre preparation method in quick spinning and high fiber number precursor, it is characterized in that: described step 3) steam drafting be divided into two-stage, the first order is preliminary draft section, and the second level is drafting multiple homogeneous drawing-off more than 4 times.
3. according to claim 1 a kind of based on modules carbon fibre preparation method in quick spinning and high fiber number precursor, it is characterized in that: the high temperature cabonization process described rapid 6) is divided into two-stage, first 1100-1300 DEG C of high temperature cabonization process is adopted, through sizing agent, high intensity standard modulus carbon fiber is obtained after winding, then this carbon fiber is carried out secondary high-temperature carbonization treatment through 1500-1800 DEG C, modulus carbon fiber during surface treatment again, starching, winding obtain.
CN201510960119.8A 2015-12-21 2015-12-21 Middle-modulus carbon fiber preparation method based on rapid spinning and high denier precursor Pending CN105401262A (en)

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CN107287699A (en) * 2017-07-07 2017-10-24 中复神鹰碳纤维有限责任公司 A kind of polyacrylonitrile base carbon fiber precursors rapid preoxidation technique
CN111118671A (en) * 2019-12-26 2020-05-08 长春工业大学 Preparation method of 25k large-tow carbon fiber
CN111118669A (en) * 2019-12-30 2020-05-08 中复神鹰碳纤维有限责任公司 Preparation method of wear-resistant carbon fiber for high-tension winding
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CN102154740A (en) * 2011-05-13 2011-08-17 北京化工大学 Method for preparing high-strength carbon fiber
CN102766989A (en) * 2012-07-25 2012-11-07 北京化工大学 Middle-modulus high-strength polyacrylonitrile-based carbon fiber, and preparation method thereof
JP5849127B2 (en) * 2014-06-13 2016-01-27 東邦テナックス株式会社 Polyacrylonitrile-based carbon fiber strand and method for producing the same
CN104651979A (en) * 2015-03-17 2015-05-27 威海拓展纤维有限公司 Preparation method of high-strength medium-model carbon fiber
CN104818546A (en) * 2015-05-18 2015-08-05 威海拓展纤维有限公司 Preparation method of high-strength high-modulus graphite fiber

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CN106835365A (en) * 2017-01-20 2017-06-13 哈尔滨天顺化工科技开发有限公司 A kind of method that carbon fiber is prepared by polyacrylonitrile fibril carbonization
CN106835365B (en) * 2017-01-20 2019-03-15 哈尔滨天顺化工科技开发有限公司 A method of carbon fiber is prepared by polyacrylonitrile fibril carbonization
CN107287699A (en) * 2017-07-07 2017-10-24 中复神鹰碳纤维有限责任公司 A kind of polyacrylonitrile base carbon fiber precursors rapid preoxidation technique
CN107287699B (en) * 2017-07-07 2020-08-21 中复神鹰碳纤维有限责任公司 Rapid preoxidation process for polyacrylonitrile-based carbon fiber precursor
CN111118671A (en) * 2019-12-26 2020-05-08 长春工业大学 Preparation method of 25k large-tow carbon fiber
CN111118669A (en) * 2019-12-30 2020-05-08 中复神鹰碳纤维有限责任公司 Preparation method of wear-resistant carbon fiber for high-tension winding
CN112064354A (en) * 2020-08-14 2020-12-11 中复神鹰碳纤维有限责任公司 Preparation method of carbon fiber for IV-type high-pressure hydrogen storage cylinder
CN112323182A (en) * 2020-09-10 2021-02-05 中复神鹰碳纤维有限责任公司 Preparation method of carbon fiber for carbon-carbon composite material needled net tire
CN113737319A (en) * 2021-10-14 2021-12-03 荣成碳纤维科技有限公司 Method and device for recycling polymerization liquid in carbon fiber production
CN114941187A (en) * 2022-06-28 2022-08-26 中复神鹰碳纤维股份有限公司 Preparation method of high-performance low-cost carbon fiber
CN114941187B (en) * 2022-06-28 2023-04-11 中复神鹰碳纤维股份有限公司 Preparation method of high-performance low-cost carbon fiber
WO2024001261A1 (en) * 2022-06-28 2024-01-04 中复神鹰碳纤维股份有限公司 Preparation method for high-performance, low-cost carbon fiber

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Application publication date: 20160316