CN108360147B - Method for preparing polyacrylonitrile pre-oxidized felt - Google Patents
Method for preparing polyacrylonitrile pre-oxidized felt Download PDFInfo
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- CN108360147B CN108360147B CN201810017014.2A CN201810017014A CN108360147B CN 108360147 B CN108360147 B CN 108360147B CN 201810017014 A CN201810017014 A CN 201810017014A CN 108360147 B CN108360147 B CN 108360147B
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/542—Adhesive fibres
- D04H1/548—Acrylonitrile series
Abstract
The invention discloses a method for preparing polyacrylonitrile pre-oxidized felt, which comprises the following steps: firstly, carrying out high-temperature heat treatment in air by using a heating furnace, along with water vapor and nitrogen; introducing nitrogen and spraying a cyclization auxiliary agent for cooling; filling a mixed gas of nitrogen, air and steam, and performing low-temperature heat treatment; introducing nitrogen and spraying a cyclization auxiliary agent for cooling; step five, improving the cyclization reaction rate through medium-temperature treatment; the invention relates to the technical field of polyacrylonitrile pre-oxidized felt. The method for preparing the polyacrylonitrile pre-oxidized felt solves the problems that the performance of the prepared polyacrylonitrile carbon fiber felt is poor, the prepared polyacrylonitrile carbon fiber felt cannot resist high temperature and cannot be quickly prepared due to the existing polyacrylonitrile pre-oxidized felt manufacturing method, and greatly improves the processing efficiency, so that the mass production of the carbon fiber heat-insulating material is greatly improved, and the obtained pre-oxidized felt product does not drop slag, has high fiber strength and good heat-insulating performance.
Description
Technical Field
The invention relates to the technical field of polyacrylonitrile pre-oxidized felts, in particular to a method for preparing a polyacrylonitrile pre-oxidized felt.
Background
The carbon fiber heat-insulating material has excellent performances of high strength, high modulus, low heat conductivity coefficient and the like, and the environmental protection requirement is improved; the traditional thermal power generation is gradually replaced by emerging photovoltaic power generation in the aspect of power generation; in the new material aspect, the traditional material is gradually replaced by the novel composite material. Both photovoltaic power generation and production of novel composite materials are carried out at ultrahigh temperature, and energy consumption is extremely high due to the ultrahigh temperature; the carbon fiber heat-insulating material has a good heat-insulating effect, the energy consumption can be greatly reduced through the heat-insulating effect of the carbon fiber heat-insulating material, and meanwhile, the carbon fiber heat-insulating material has high purity and does not introduce other impurity ash, so that the purity of the product is effectively ensured; the advantage greatly promotes the utilization rate of the carbon fiber thermal insulation material in the photovoltaic industry. At the present stage, the environment protection force is increased, and photovoltaic and new materials are rapidly developed; the demand of the carbon fiber heat-insulating material is greatly increased, and the phenomenon that the carbon fiber heat-insulating material is short in supply and demand and the like appears in the market; therefore, the rapid preparation of the carbon fiber heat-insulating material can not only fill the market demand, but also has great market potential; and is beneficial to the nation and the people. The polyacrylonitrile pre-oxidized felt can be processed at high temperature to obtain a polyacrylonitrile carbon fiber felt which is a main product of a carbon fiber heat-insulating material; the existing polyacrylonitrile pre-oxidation felt manufacturing method causes the defects that the prepared polyacrylonitrile carbon fiber felt is poor in performance and not high-temperature resistant, and the rapid preparation of the polyacrylonitrile pre-oxidation felt becomes a main reason for preventing the mass production of the carbon fiber heat-insulating material to a large extent.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for preparing a polyacrylonitrile pre-oxidized felt, which solves the problems that the performance of the prepared polyacrylonitrile carbon fiber felt is poor, the prepared polyacrylonitrile carbon fiber felt cannot resist high temperature and the polyacrylonitrile carbon fiber felt cannot be quickly prepared due to the existing polyacrylonitrile pre-oxidized felt manufacturing method.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme, and the method for preparing the polyacrylonitrile pre-oxidized felt comprises the following operation steps:
firstly, carrying out high-temperature heat treatment in air by using a heating furnace, along with water vapor and nitrogen;
introducing nitrogen and spraying a cyclization auxiliary agent for cooling;
filling a mixed gas of nitrogen, air and steam, and performing low-temperature heat treatment;
introducing nitrogen and spraying a cyclization auxiliary agent for cooling;
and step five, improving the cyclization reaction rate through medium-temperature treatment.
Preferably, the temperature of the high-temperature heat treatment in the air in the step one is 200-260 ℃; the treatment time is 60-300 min; air flow rate of 100-3Per, water vapor flow rate of 100-3H, nitrogen flow rate of 10-200m3H; air: water vapor: 1-10 parts of nitrogen: 0.1-1: 0.002-0.04.
Preferably, the nitrogen flow rate in the second step is 1-100m3Cooling for 10-10000s to below 80 ℃; the flow rate of the cyclization auxiliary agent is 1-50L/min; the auxiliary agent is acetic acid, urea solution or water.
Preferably, the low-temperature treatment temperature in the step three is 160-215 ℃; the treatment time is 60-300 min; the nitrogen flow is 10-200m3H, steamingThe steam flow is 100-500m3Per, air flow rate of 100-3H; the nitrogen flow is 10-200m3H, air: water vapor: 1-10 parts of nitrogen: 0.5-1: 0.01-0.2.
Preferably, the nitrogen flow rate in the fourth step is 1-100m3H; the flow rate of the cyclization auxiliary agent is 1-50L/min; the auxiliary agent is acetic acid, urea solution or water.
Preferably, the medium temperature treatment temperature in the step five is 180-235 ℃; the treatment time is 60-300 min; the circulating atmosphere medium in the furnace is nitrogen and water vapor, and the nitrogen flow is 20-200m3The flow rate of water vapor is 100-3H; nitrogen gas: water vapor is 0.02-0.2: 5-50.
Preferably, the running mode of the product adopts a mesh belt and rail traction mode.
Preferably, the method is applied to a raw material thickness of 3 to 20 mm.
Preferably, the circulating wind speed in the furnace is 0.5-10 m/s.
Preferably, the heating mode adopts a hot air circulation heating mode or an electric heating mode or a combination mode of the two modes.
(III) advantageous effects
The invention provides a method for preparing polyacrylonitrile pre-oxidized felt. The method has the following beneficial effects:
(1) according to the method for preparing the polyacrylonitrile pre-oxidized felt, the energy consumption is greatly reduced by adopting a continuous production mode, and the skirt edge of the pre-oxidized felt is prevented from being formed by a mesh belt or carrier roller drafting transmission mode, so that the product flatness is good, the product utilization rate is improved to the maximum degree, and the obtained pre-oxidized felt product does not drop slag, is high in fiber strength and has good heat insulation performance.
(2) The method for preparing the polyacrylonitrile pre-oxidized felt greatly improves the production efficiency of the polyacrylonitrile pre-oxidized felt, meets the market demand, has excellent product quality and good flatness, avoids a large amount of cutting waste, and is extremely suitable for large-scale continuous production.
(3) Compared with the traditional process for preparing the polyacrylonitrile pre-oxidized felt, the process time is 1/4-1/2 of the traditional process time, and the processing efficiency is greatly improved, so that the mass production of the carbon fiber heat-insulating material is greatly improved, the market demand can be filled, and the process is beneficial to the nation and the people.
Drawings
FIG. 1 is a process scheme of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme, and a method for quickly preparing polyacrylonitrile pre-oxidized felt, which comprises the following steps:
firstly, raw materials are rolled up and enter a pre-oxidation furnace in a mesh belt or carrier roller drafting mode.
Step two, high-temperature heat treatment: the raw material directly enters a high temperature furnace at the temperature of 200 ℃ and 260 ℃; opening an air inlet valve, introducing proper nitrogen and water vapor according to the air flow, and introducing the mixture according to the ratio of air: water vapor: 1-10 parts of nitrogen: 0.1-1: 0.002-0.04 percent of the raw material is introduced; adjusting the rotating speed of the circulating fan to ensure that the circulating wind speed is 0.5-10 m/s; the mesh belt or the drafting rate is adjusted to ensure that the reaction time in the furnace is 60-300 min.
Step three, a fast cooling section: after the high-temperature heat treatment is finished, entering a rapid cooling section; introducing nitrogen gas for 1-100m3And h, spraying an auxiliary agent simultaneously to realize rapid cooling to below 80 ℃.
Fourthly, low-temperature heat treatment: after the product is rapidly cooled, the product carries the auxiliary agent to enter a low-temperature heat treatment section; the heat treatment temperature is 160-215 ℃; the heat treatment time is 60-300 min; opening an air inlet valve to adjust air flow, and introducing proper amount of water vapor and nitrogen; the air is introduced in the ratio of: water vapor: 1-10 parts of nitrogen: 0.5-1: 0.01-0.2.
Step five, slow cooling section: low temperature heat treatment of the productThen, entering a slow cooling section; introducing 1-100m into the slow cooling section3The nitrogen gas per hour is used for cooling the product and simultaneously dissipating the heat accumulated inside the product.
Sixthly, medium-temperature heat treatment: the product is treated by the slow cooling section, the internal heat accumulation is removed, the reaction temperature is 180-235 ℃ in the medium temperature section, and the treatment time is 60-300 min; the furnace atmosphere is nitrogen and water vapor, and the introduction ratio of the nitrogen is as follows: water vapor is 0.02-0.2: 5-50; the temperature is increased to accelerate the process of internal cyclization of the product, and the product forms a naphthenic structure after the medium-temperature stage reaction is finished and has good heat-resistant gradient.
And seventhly, the heating modes in the second step, the fourth step and the sixth step are hot air circulation heating or furnace electric heating or a combination mode of the hot air circulation heating and the furnace electric heating.
During operation, set for raw and other materials and select its length for use polyacrylonitrile raw felt to be 35m, width be 1.8m, thickness 15mm, the transport mode is the guipure transport, first step: conveying the polyacrylonitrile original felt into a high-temperature air section through a mesh belt, treating the temperature gradient of 238-242 ℃, wherein the operation time is 300min, and the operation time is 3000m along with the atmosphere air3H, water vapor 200m3H, 20m of nitrogen3H; the second step is that: after the reaction is finished, the reaction product enters a slow cooling section and is filled with nitrogen gas for 100m3Spraying acetic acid solution for 30L/h, wherein the treatment time is 600 s; the third step: entering a low-temperature heat treatment section after the treatment, wherein the treatment temperature is 200-208 ℃; the treatment time is 300min, and the accompanying atmosphere is 800m3H, water vapor 400m3A/h, nitrogen gas 100m m3H; the fourth step: after the low-temperature heat treatment is finished, the mixture enters a slow cooling section again and is filled with nitrogen gas for 100m3Spraying acetic acid solution for 30L/h, wherein the treatment time is 600 s; the fifth step: after the treatment is finished, the medium temperature heat treatment section is carried out, and the treatment temperature is 226-232 ℃; the treatment time is 300min, and the accompanying atmosphere is nitrogen gas 200m3H, water vapor 800m3H; the polyacrylonitrile pre-oxidized felt obtained by the steps has the length of 31.2m, the width of 1.35-1.4m and the thickness of 10 mm; the obtained pre-oxidized felt is non-fusible, non-combustible, high in flatness, free of skirt phenomenon, high in fiber strength and excellent in heat preservation performance.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation. The use of the phrase "comprising one of the elements does not exclude the presence of other like elements in the process, method, article, or apparatus that comprises the element.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. The method for preparing the polyacrylonitrile pre-oxidized felt is characterized by comprising the following operation steps of:
step one, performing high-temperature heat treatment in air by using a heating furnace, wherein the temperature of the high-temperature heat treatment in the air is 230-260 ℃ along with water vapor and nitrogen; the treatment time is 60-300 min; air flow rate of 100-3Per, water vapor flow rate of 100-3H, nitrogen flow rate of 10-200m3H; air: water vapor: 1-10 parts of nitrogen: 0.1-1: 0.002-0.04;
step two, introducing nitrogen and spraying a cyclization auxiliary agent for cooling treatment, wherein the flow rate of the nitrogen is 1-100m3Cooling for 10-10000s to below 80 ℃; the flow rate of the cyclization auxiliary agent is 1-50L/min; the auxiliary agent is acetic acid, urea solution or water;
step three, filling mixed gas of nitrogen, air and water vapor, and carrying out low-temperature heat treatment at the low-temperature treatment temperature190 ℃ at 150 ℃; the treatment time is 60-300 min; the nitrogen flow is 10-200m3The flow rate of water vapor is 100-3Per, air flow rate of 100-3H; the nitrogen flow is 10-200m3H, air: water vapor: 1-10 parts of nitrogen: 0.5-1: 0.01-0.2;
introducing nitrogen and spraying a cyclization auxiliary agent for cooling;
and step five, improving the cyclization reaction rate through medium-temperature treatment.
2. The method for preparing polyacrylonitrile pre-oxidized felt according to claim 1, characterized in that: in the fourth step, the nitrogen flow is 1-100m3H; the flow rate of the cyclization auxiliary agent is 1-50L/min; the auxiliary agent is acetic acid, urea solution or water.
3. The method for preparing polyacrylonitrile pre-oxidized felt according to claim 1, characterized in that: in the fifth step, the medium temperature treatment temperature is 190-230 ℃; the treatment time is 60-300 min; the circulating atmosphere medium in the furnace is nitrogen and water vapor, and the nitrogen flow is 20-200m3The flow rate of water vapor is 100-3H; nitrogen gas: water vapor is 0.02-0.2: 5-50.
4. The method for preparing polyacrylonitrile pre-oxidized felt according to claim 1, characterized in that: the thickness of the raw material applicable to the method is 3-20 mm.
5. The method for preparing polyacrylonitrile pre-oxidized felt according to claim 2, characterized in that: the circulating wind speed in the furnace is 0.5-10 m/s.
6. The method for preparing polyacrylonitrile pre-oxidized felt according to claim 2, characterized in that: the heating mode adopts a hot air circulation heating mode or an electric heating mode or a combination mode of the two modes.
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| CN110685069A (en) * | 2019-10-28 | 2020-01-14 | 江苏米格新材料有限公司 | Method for continuously preparing pre-oxidized felt |
| CN113789607B (en) * | 2021-09-22 | 2023-07-07 | 辽宁兴汇碳材料科技有限公司 | Polyacrylonitrile-based fiber mat and preparation method and application thereof |
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| CN101260575B (en) * | 2008-04-17 | 2010-06-02 | 东华大学 | Pre-oxidation method for carbon fiber precursor polyacrylnitrile fiber |
| CN102465376A (en) * | 2010-11-09 | 2012-05-23 | 张孟福 | Preparation method of highly carbonized fiber woven filler |
| CN102181963B (en) * | 2011-03-30 | 2012-12-05 | 东华大学 | Curing treatment method of carbon fiber precursor polyacrylonitrile fiber |
| US20120322332A1 (en) * | 2011-06-17 | 2012-12-20 | Ut-Battelle, Llc | Advanced oxidation method for producing high-density oxidized polyacrylonitrile fibers |
| 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 |
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Denomination of invention: A method for preparing polyacrylonitrile pre oxygen felt Effective date of registration: 20210729 Granted publication date: 20200324 Pledgee: Suixi Jinmao financing Company limited by guarantee Pledgor: ANHUI HONGCHANG NEW MATERIAL Co.,Ltd. Registration number: Y2021980007032 |
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Address after: 235,000 South of China Resources Gas Station, east of Shanzha Road, west of Yingchun Road, Phase II, Suixi Economic Development Zone, Suixi County, Huaibei City, Anhui Province Patentee after: Anhui Hongchang New Materials Co.,Ltd. Address before: 235,000 South of China Resources Gas Station, east of Shanzha Road, west of Yingchun Road, Phase II, Suixi Economic Development Zone, Suixi County, Huaibei City, Anhui Province Patentee before: ANHUI HONGCHANG NEW MATERIAL Co.,Ltd. |
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