CN108360147A - A method of preparing the pre- oxygen felt of polyacrylonitrile - Google Patents
A method of preparing the pre- oxygen felt of polyacrylonitrile Download PDFInfo
- Publication number
- CN108360147A CN108360147A CN201810017014.2A CN201810017014A CN108360147A CN 108360147 A CN108360147 A CN 108360147A CN 201810017014 A CN201810017014 A CN 201810017014A CN 108360147 A CN108360147 A CN 108360147A
- Authority
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- China
- Prior art keywords
- nitrogen
- polyacrylonitrile
- temperature
- felt
- oxygen felt
- 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.)
- Granted
Links
- 229920002239 polyacrylonitrile Polymers 0.000 title claims abstract description 37
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000001301 oxygen Substances 0.000 title claims abstract description 36
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 36
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 87
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 239000003570 air Substances 0.000 claims abstract description 23
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 239000008246 gaseous mixture Substances 0.000 claims abstract description 3
- 238000007363 ring formation reaction Methods 0.000 claims abstract description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Natural products CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 230000001351 cycling effect Effects 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 238000011017 operating method Methods 0.000 claims description 2
- 229920000049 Carbon (fiber) Polymers 0.000 abstract description 14
- 239000004917 carbon fiber Substances 0.000 abstract description 14
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 14
- 239000011810 insulating material Substances 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000000835 fiber Substances 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 238000010583 slow cooling Methods 0.000 description 6
- 239000011157 advanced composite material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention discloses a kind of methods preparing the pre- oxygen felt of polyacrylonitrile, include the following steps：Step 1 is heat-treated using heating furnace high-temperature in air, with water vapour and nitrogen；Step 2 is passed through nitrogen, sprinkling cyclisation auxiliary agent carries out cooling processing；Step 3 is filled with the gaseous mixture of nitrogen, air and water vapour, Low Temperature Heat Treatment；Step 4 is passed through nitrogen, sprinkling cyclisation auxiliary agent carries out cooling processing；Step 5, heat-treated under medium temperature improve cyclization rate；The present invention relates to the pre- oxygen felt technical fields of polyacrylonitrile.This prepares the method for the pre- oxygen felt of polyacrylonitrile, it solves the pre- oxygen felt manufacturing method of existing polyacrylonitrile and results in prepared polyacrylonitrile carbon fiber felt poor performance, there are the defects of non-refractory, and the problem of cannot quickly preparing, substantially increase processing efficiency, to make the volume production of carbon fiber thermal insulating material increase substantially, and the pre- oxygen felt product of gained is not scaling-off, fibre strength is high, heat-insulating property is good.
Description
Technical field
The present invention relates to the pre- oxygen felt technical field of polyacrylonitrile, specially a kind of method preparing the pre- oxygen felt of polyacrylonitrile.
Background technology
Carbon fiber thermal insulating material has the excellent properties such as high intensity, high-modulus and low thermal conductivity, with environmental requirement
It improves；Traditional thermal power generation is gradually substituted by emerging photovoltaic generation in terms of power generation；In terms of new material traditional material by
Gradually substituted by advanced composite material (ACM).The either production of photovoltaic generation or advanced composite material (ACM) at a temperature of superelevation, by
Cause energy consumption very big in the temperature of superelevation；Carbon fiber thermal insulating material has good heat insulation effect, passes through carbon fiber thermal insulating material
Heat insulation effect energy consumption can be greatly lowered, while carbon fiber thermal insulating material purity height does not introduce other impurities ash content, effectively
The purity that ensure that product；This advantage has greatly facilitated utilization rate of the photovoltaic industry to carbon fiber thermal insulating material.Existing rank
Duan Guojia increases environmentally friendly dynamics, and photovoltaic and new material are fast-developing；Carbon fiber thermal insulating material demand increases considerably, and market goes out
Existing carbon fiber thermal insulating material phenomena such as supply falls short of demand；So the need in market can not only be filled up by quickly preparing carbon fiber thermal insulating material
It asks, there is great market potential；And it benefits the nation and the people.The pre- oxygen felt of polyacrylonitrile can obtain polyacrylonitrile carbon by high-temperature process
Fibrofelt is carbon fiber thermal insulating material major product；The existing pre- oxygen felt manufacturing method of polyacrylonitrile results in prepared gather
, there is the defect in non-refractory in acrylic carbon fibre felt poor performance, and quickly prepare the pre- oxygen felt of polyacrylonitrile as hindering
Carbon fiber thermal insulating material significantly volume production the main reason for.
Invention content
(1) the technical issues of solving
In view of the deficiencies of the prior art, it the present invention provides a kind of method preparing the pre- oxygen felt of polyacrylonitrile, solves existing
Some pre- oxygen felt manufacturing methods of polyacrylonitrile result in prepared polyacrylonitrile carbon fiber felt poor performance, exist in non-refractory
Defect, and the problem of cannot quickly prepare.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs, it is a kind of to prepare the pre- oxygen felt of polyacrylonitrile
Method, including following operating procedure：
Step 1 is heat-treated using heating furnace high-temperature in air, with water vapour and nitrogen；
Step 2 is passed through nitrogen, sprinkling cyclisation auxiliary agent carries out cooling processing；
Step 3 is filled with the gaseous mixture of nitrogen, air and water vapour, Low Temperature Heat Treatment；
Step 4 is passed through nitrogen, sprinkling cyclisation auxiliary agent carries out cooling processing；
Step 5, heat-treated under medium temperature improve cyclization rate.
Preferably, the temperature of the heat treatment of air high temperature described in step 1 is 200-260 DEG C；Processing time is 60-
300min；Air mass flow is 100-5000m3/ h, steam rates 100-500m3/ h, nitrogen flow 10-200m3/h；Air：
Water vapour：Nitrogen=1-10：0.1-1：0.002-0.04.
Preferably, nitrogen flow described in step 2 is 1-100m3Temperature fall time 10-10000s ,/h is cooled to 80 DEG C
Below；Cyclisation auxiliary agent flow is 1-50L/min；Auxiliary agent is acetic acid, urea liquid or water.
Preferably, low-temperature treatment temperature described in step 3 is 160-215 DEG C；Processing time is 60-300min；Nitrogen stream
Amount is 10-200m3/ h, steam rates 100-500m3/ h, air mass flow 100-1000m3/h；Nitrogen flow is 10-
200m3/ h, air：Water vapour：Nitrogen=1-10：0.5-1：0.01-0.2.
Preferably, nitrogen flow described in step 4 is 1-100m3/h；Cyclisation auxiliary agent flow is 1-50L/min；Auxiliary agent is
Acetic acid, urea liquid or water.
Preferably, heat-treated under medium temperature temperature described in step 5 is 180-235 DEG C；Processing time is 60-300min；It is followed in stove
Ring atmosphere medium is nitrogen and water vapour, nitrogen flow 20-200m3/ h, steam rates 100-1000m3/h；Nitrogen：Water
Steam=0.02-0.2：5-50.
Preferably, the product method of operation is by the way of guipure, track drawing.
Preferably, the applicable material stock thickness of the method is 3-20mm.
Preferably, cycle wind speed is 0.5-10m/s in the stove.
Preferably, the mode of heating is by the way of Cycling hot-blast heating or electrical heating or both combination.
(3) advantageous effect
The present invention provides a kind of methods preparing the pre- oxygen felt of polyacrylonitrile.Has following advantageous effect：
(1), the method for preparing the pre- oxygen felt of polyacrylonitrile, is substantially reduced using quantity-produced mode in terms of energy consumption,
The formation that pre- oxygen felt shirt rim is avoided by way of guipure or carrying roller drawing-off transmission maximizes to keep product flatness good
Improve product utilization rate, and the pre- oxygen felt product of gained is not scaling-off, fibre strength is high, heat-insulating property is good.
(2), the method for preparing the pre- oxygen felt of polyacrylonitrile, greatly improves the production efficiency of the pre- oxygen felt of polyacrylonitrile,
The demand in market is met, while product quality is excellent, flatness well avoids a large amount of cut and wastes, and is extremely applicable to big
The continuous production of scale.
(3), the method for preparing the pre- oxygen felt of polyacrylonitrile, compared with tradition prepares the technique of the pre- oxygen felt of polyacrylonitrile, this
Process time is the 1/4-1/2 of traditional handicraft time, substantially increases processing efficiency, to make the volume production of carbon fiber thermal insulating material
It increases substantially, the demand in market can be filled up, and benefit the nation and the people.
Description of the drawings
Fig. 1 is present invention process route map.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
The present invention provides a kind of technical solution, a method of the pre- oxygen felt of polyacrylonitrile quickly being prepared, is included the following steps：
The first step rolls on raw material, enters pre-oxidation furnace by way of guipure or carrying roller drawing-off.
Second step, high-temperature heat treatment：Raw material are directly entered 200-260 DEG C of high temperature furnace；It opens air and enters the wind valve, foundation
Air mass flow is passed through nitrogen appropriate, water vapour, is passed through ratio according to air：Water vapour：Nitrogen=1-10：0.1-1：0.002-
0.04 is passed through；Adjustment circulating fan rotating speed ensures that it is 0.5-10m/s to recycle wind speed；It adjusts guipure or drafting rate ensures in stove instead
It is 60-300min between seasonable.
Third walks, rapid cooling section：After the completion of high-temperature heat treatment, into rapid cooling section；It is passed through nitrogen 1-100m3/ h, sprays simultaneously
Auxiliary agent realizes fast cooling to 80 DEG C or less.
4th step, Low Temperature Heat Treatment：Product carries auxiliary agent and enters Low Temperature Heat Treatment section after fast cooling；Heat treatment temperature
Degree is 160-215 DEG C；Heat treatment time is 60-300min；It opens intake valve adjustment air mass flow, be passed through appropriate water vapour, nitrogen
Gas；It is air to be passed through ratio：Water vapour：Nitrogen=1-10：0.5-1：0.01-0.2.
5th step, slow cooling section：After the completion of product Low Temperature Heat Treatment, into slow cooling section；1-100m is passed through in slow cooling section3/ h's
Nitrogen cools down to product and handles while dispersing interiors of products accumulated heat.
6th step, medium temperature heat treatment：Product internal accumulated heat behind slow cooling section has been removed, into middle-temperature section reaction temperature
It is 180-235 DEG C, processing time 60-300min；Furnace atmosphere be nitrogen and water vapour its to be passed through ratio be nitrogen：Water vapour=
0.02-0.2：5-50；The raising of temperature accelerates the process of interiors of products cyclisation, product formation ring after the completion of medium temperature elementary reaction
Alkyl structure has good Heat-Resistant Gradient.
7th step, in second step of the present invention, the 4th step and the 6th step mode of heating be in Cycling hot-blast heating or stove electricity plus
The mode that heat or both combines.
When work, the length of 35m of raw material selection polyacrylonitrile original felt, width 1.8m, thickness 15mm are set, is conveyed
Mode is mesh-belt conveying, the first step：Polyacrylonitrile original felt enters high temperature air section, treatment temperature 238- by mesh-belt conveying
242 DEG C of temperature gradient, run time 300min, with ambient air 3000m3/ h, water vapour 200m3/ h, nitrogen 20m3/
h；Second step：After the completion of reaction nitrogen 100m is passed through into slow cooling section3/ h, sprinkling acetum 30L/h, processing time is
600s；Third walks：Enter Low Temperature Heat Treatment section after being processed into, treatment temperature is 200-208 DEG C；Processing time is 300min, companion
It is air 800m with atmosphere3/ h, water vapour 400m3/ h, nitrogen 100m m3/h；4th step：After the completion of Low Temperature Heat Treatment again into
Enter slow cooling section and is passed through nitrogen 100m3/ h, sprinkling acetum 30L/h, processing time 600s；5th step：Processing is completed laggard
Enter medium temperature heat treatment section, treatment temperature is 226-232 DEG C；Processing time is 300min, is nitrogen 200m with atmosphere3/ h, water
Steam 800m3/h；Through the above steps processing obtain the length of 31.2m of the pre- oxygen felt of polyacrylonitrile, width 1.35-1.4m,
Thickness is 10mm；The pre- oxygen felt of gained is not molten, non-ignitable, Pingdu is high, without shirt rim phenomenon, fibre strength is high simultaneously, excellent thermal insulation performance.
It should be noted that herein, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also include other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions.By sentence " including one ... the element limited, it is not excluded that
There is also other identical elements in the process, method, article or apparatus that includes the element ".
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (10)
1. a kind of method preparing the pre- oxygen felt of polyacrylonitrile, which is characterized in that including following operating procedure：
Step 1 is heat-treated using heating furnace high-temperature in air, with water vapour and nitrogen；
Step 2 is passed through nitrogen, sprinkling cyclisation auxiliary agent carries out cooling processing；
Step 3 is filled with the gaseous mixture of nitrogen, air and water vapour, Low Temperature Heat Treatment；
Step 4 is passed through nitrogen, sprinkling cyclisation auxiliary agent carries out cooling processing；
Step 5, heat-treated under medium temperature improve cyclization rate.
2. a kind of method preparing the pre- oxygen felt of polyacrylonitrile according to claim 1, it is characterised in that：Described in step 1
The temperature of air high temperature heat treatment is 200-260 DEG C；Processing time is 60-300min；Air mass flow is 100-5000m3/h、
Steam rates 100-500m3/ h, nitrogen flow 10-200m3/h；Air：Water vapour：Nitrogen=1-10：0.1-1：0.002-
0.04。
3. a kind of method preparing the pre- oxygen felt of polyacrylonitrile according to claim 1, it is characterised in that：Described in step 2
Nitrogen flow is 1-100m3Temperature fall time 10-10000s ,/h is cooled to 80 DEG C or less；Cyclisation auxiliary agent flow is 1-50L/
min；Auxiliary agent is acetic acid, urea liquid or water.
4. a kind of method preparing the pre- oxygen felt of polyacrylonitrile according to claim 1, it is characterised in that：Described in step 3
Low-temperature treatment temperature is 160-215 DEG C；Processing time is 60-300min；Nitrogen flow is 10-200m3/ h, steam rates are
100-500m3/ h, air mass flow 100-1000m3/h；Nitrogen flow is 10-200m3/ h, air：Water vapour：Nitrogen=1-
10：0.5-1：0.01-0.2.
5. a kind of method preparing the pre- oxygen felt of polyacrylonitrile according to claim 1, it is characterised in that：Described in step 4
Nitrogen flow is 1-100m3/h；Cyclisation auxiliary agent flow is 1-50L/min；Auxiliary agent is acetic acid, urea liquid or water.
6. a kind of method preparing the pre- oxygen felt of polyacrylonitrile according to claim 1, it is characterised in that：Described in step 5
Heat-treated under medium temperature temperature is 180-235 DEG C；Processing time is 60-300min；Circulating atmosphere medium is nitrogen and water vapour, nitrogen in stove
Throughput is 20-200m3/ h, steam rates 100-1000m3/h；Nitrogen：Water vapour=0.02-0.2：5-50.
7. a kind of method preparing the pre- oxygen felt of polyacrylonitrile according to claim 1, it is characterised in that：The product operation
Mode is by the way of guipure, track drawing.
8. a kind of method preparing the pre- oxygen felt of polyacrylonitrile according to claim 1, it is characterised in that：The method is applicable in
Material stock thickness be 3-20mm.
9. a kind of method preparing the pre- oxygen felt of polyacrylonitrile according to claim 2,4 or 6, it is characterised in that：The stove
Interior cycle wind speed is 0.5-10m/s.
10. a kind of method preparing the pre- oxygen felt of polyacrylonitrile according to claim 2,4 or 6, it is characterised in that：It is described to add
Hot mode is by the way of Cycling hot-blast heating or electrical heating or both combination.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810017014.2A CN108360147B (en) | 2018-01-09 | 2018-01-09 | Method for preparing polyacrylonitrile pre-oxidized felt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810017014.2A CN108360147B (en) | 2018-01-09 | 2018-01-09 | Method for preparing polyacrylonitrile pre-oxidized felt |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108360147A true CN108360147A (en) | 2018-08-03 |
| CN108360147B CN108360147B (en) | 2020-03-24 |
Family
ID=63011140
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810017014.2A Active CN108360147B (en) | 2018-01-09 | 2018-01-09 | Method for preparing polyacrylonitrile pre-oxidized felt |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN113789607A (en) * | 2021-09-22 | 2021-12-14 | 辽宁兴汇碳材料科技有限公司 | Polyacrylonitrile-based fibrofelt and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113789607A (en) * | 2021-09-22 | 2021-12-14 | 辽宁兴汇碳材料科技有限公司 | Polyacrylonitrile-based fibrofelt and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108360147B (en) | 2020-03-24 |
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