CN107268215A - A kind of carbon fibre precursor wash mill and washing methods - Google Patents
A kind of carbon fibre precursor wash mill and washing methods Download PDFInfo
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- CN107268215A CN107268215A CN201710479377.3A CN201710479377A CN107268215A CN 107268215 A CN107268215 A CN 107268215A CN 201710479377 A CN201710479377 A CN 201710479377A CN 107268215 A CN107268215 A CN 107268215A
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- tow
- water
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- rinsing
- carbon fibre
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- 238000005406 washing Methods 0.000 title claims abstract description 71
- 239000000835 fiber Substances 0.000 title claims abstract description 64
- 239000002243 precursor Substances 0.000 title claims abstract description 45
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 100
- 238000005554 pickling Methods 0.000 claims abstract description 20
- 239000007921 spray Substances 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000005507 spraying Methods 0.000 claims abstract description 10
- 238000010612 desalination reaction Methods 0.000 claims description 10
- 150000004965 peroxy acids Chemical class 0.000 claims description 5
- 229910001415 sodium ion Inorganic materials 0.000 abstract description 21
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 abstract description 16
- 229920000049 Carbon (fiber) Polymers 0.000 description 18
- 239000004917 carbon fiber Substances 0.000 description 18
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 18
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 description 15
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 10
- 229920002239 polyacrylonitrile Polymers 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 7
- 238000006116 polymerization reaction Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 6
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 239000012530 fluid Substances 0.000 description 6
- 239000003999 initiator Substances 0.000 description 6
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 6
- 239000000178 monomer Substances 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 238000002166 wet spinning Methods 0.000 description 5
- 238000010790 dilution Methods 0.000 description 4
- 239000012895 dilution Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 101100298222 Caenorhabditis elegans pot-1 gene Proteins 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B21/00—Successive treatments of textile materials by liquids, gases or vapours
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B1/00—Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating
- D06B1/02—Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating by spraying or projecting
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B23/00—Component parts, details, or accessories of apparatus or machines, specially adapted for the treating of textile materials, not restricted to a particular kind of apparatus, provided for in groups D06B1/00 - D06B21/00
- D06B23/02—Rollers
- D06B23/023—Guiding rollers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B23/00—Component parts, details, or accessories of apparatus or machines, specially adapted for the treating of textile materials, not restricted to a particular kind of apparatus, provided for in groups D06B1/00 - D06B21/00
- D06B23/04—Carriers or supports for textile materials to be treated
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B23/00—Component parts, details, or accessories of apparatus or machines, specially adapted for the treating of textile materials, not restricted to a particular kind of apparatus, provided for in groups D06B1/00 - D06B21/00
- D06B23/20—Arrangements of apparatus for treating processing-liquids, -gases or -vapours, e.g. purification, filtration or distillation
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B23/00—Component parts, details, or accessories of apparatus or machines, specially adapted for the treating of textile materials, not restricted to a particular kind of apparatus, provided for in groups D06B1/00 - D06B21/00
- D06B23/20—Arrangements of apparatus for treating processing-liquids, -gases or -vapours, e.g. purification, filtration or distillation
- D06B23/22—Arrangements of apparatus for treating processing-liquids, -gases or -vapours, e.g. purification, filtration or distillation for heating
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
- D06B3/04—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of yarns, threads or filaments
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Treatment Of Fiber Materials (AREA)
Abstract
The invention discloses a kind of carbon fibre precursor wash mill and washing methods.Device includes：Rinsing machine seal wire roller group, circulating water chennel, feeding spraying pump, spray nozzle, rinsing tank；Rinsing machine seal wire roller group is arranged in above circulating water chennel, staggered above and below godet, and there is squeeze roller group outlet, and the tow by pickling processes is by rinsing machine seal wire roller group and squeeze roller group, into rinsing tank；Spray nozzle is provided with above rinsing machine seal wire roller group；Spray nozzle is connected with feeding spraying pump.Method includes：1) after desalted water heating, it is delivered to rinsing tank；2) desalted water enters rinsing machine circulating water chennel by overflow in rinsing tank；3) tow enters rinsing machine after pickling processes, and shower water is emitted into atomized water from spray nozzle, and tow is washed；4) rinsed after tow is scrubbed into potcher, tow direction of advance is opposite in the flow direction of potcher with desalted water.The present invention can reduce the sodium ion in tow, improve the quality of carbon fibre precursor.
Description
Technical field
The present invention relates to carbon fiber production field, further say, be to be related to a kind of carbon fibre precursor wash mill and wash
Wash method.
Background technology
Carbon fiber is as a kind of new and high technology material, with high intensity, high-modulus, low-density, high temperature resistant, high conductance and heat
The advantages of leading, is widely used in the fields such as aviation, automobile, style.Polyacrylonitrile base carbon fiber precursors are the weights for preparing carbon fiber
Raw material is wanted, the quality of precursor plays decisive role to carbon fiber quality.
It is generally to use sodium sulfocyanate for solvent that sodium rhodanate one-step method, which prepares carbon fiber, acrylonitrile, second comonomer propylene
Sour methyl esters, Third monomer itaconic acid are raw material, and azodiisobutyronitrile is that initiator carries out binary polymerization reaction, by de- single, de-
Polyacrylonitrile polymer fluid is obtained after bubble.It polymerize stoste after metering, entering coagulating bath by spinning head forms as-spun fibre, just
Raw fiber carries out the pre-heat treatment and drawing-off by pre- heating bath, subsequently into washing, carries out pickling after washing, then by oiling,
The process such as dry obtains carbon fibre precursor.
It is solvent as a result of sodium sulfocyanate, in spinning process, has a certain amount of sodium ion and be wrapped in carbon fiber
In as-spun fibre, fiber adheres to pickling residue and sodium ion after descaling bath processing on fibre bundle, influence carbon fiber
Performance.The too high electricity that can influence carbon fiber of sodium ions content, hot property, in preoxidation process, ternary polymerization acrylonitrile precursor
In contain carboxylic acid group, can make cyclisation heat release relax, and sodium ion to carboxylic acid rise neutralization, make cyclisation heat release tend to concentration.
Under high temperature, metal impurities are gradually escaped, the lower hole of residual, are caused carbon fiber surface defect, are influenceed the intensity of carbon fiber.
The main method of carbon fibre precursor washing, which has, embathes and embathes plus two kinds of spray, in existing technology, through overpickling
The carbon fibre tow of processing, impregnates by the elongated sink equipped with desalted water, plays a part of washing tow.Such washing
Mode mainly has two defects, is on the one hand that washing slot length is too short, only 6 meters long, the residence time is short in a water bath for tow, because of silk
Remain sodium ion in beam to be directly proportional to washing time, so tow can not be washed fully.On the other hand do not had in elongated sink
Weir subregion is set, washing water easily forms dead band when flowing on sink both sides, it is impossible to keeps certain concentration difference, reduces water
The effect washed.
The content of the invention
Employ during sodium sulfocyanate prepares carbon fibre precursor for solvent, having a certain amount of sodium ion, to be wrapped in carbon fine
Tie up in as-spun fibre, fiber adheres to pickling residue and sodium ion after descaling bath processing on fibre bundle, influence carbon is fine
Tie up performance.To solve produced problem in the prior art, the invention provides a kind of carbon fibre precursor wash mill and washing side
Method.The sodium ions content in secondary washing, reduction precursor is carried out, carbon fibre precursor quality is improved.
An object of the present invention is to provide a kind of carbon fibre precursor wash mill.
Including：
Rinsing machine seal wire roller group, circulating water chennel, feeding spraying pump, spray nozzle, rinsing tank；
Rinsing machine seal wire roller group is arranged in above circulating water chennel, staggered above and below godet, and there is squeeze roller group outlet, is passed through
The tow of overpickling processing is by rinsing machine seal wire roller group and squeeze roller group, into rinsing tank；
Spray nozzle is provided with above rinsing machine seal wire roller group；Spray nozzle is connected with feeding spraying pump.
Wherein, preferably：
The circulating water chennel bottom is provided with snakelike heating coil.
The circulating water chennel is divided into three sections of tanks, every section of alone cycle water, successively overflow；
The circulating water chennel is provided with downflow weir and overfall.
The potcher is provided with downflow weir and overfall.
The wash mill is provided with water fender, and water fender is arranged between adjacent two godets up and down staggeredly, with
Tow is parallel in adjacent two seal wire roller group traffic directions up and down, and tow passes through between shower and water fender.Water fender with
Tow spacing distance can adjust.
Desalination water pot, desalted water delivery pump, plate type heat exchanger connect rinsing tank and circulating water chennel respectively after being sequentially connected.
The second object of the present invention is to provide a kind of carbon fibre precursor washing methods.
Including：
1) after desalted water heating, rinsing machine and rinsing tank are delivered to respectively；
2) desalted water enters rinsing machine circulating water chennel by overflow in rinsing tank, and rinsing machine adds desalted water in circulation
Tank successively overflow, direction is opposite with tow direction of advance；
3) tow enters rinsing machine after pickling processes, and shower water is emitted into atomized water from spray nozzle, and tow is washed；
4) rinsed after tow is scrubbed into potcher, tow direction of advance is with desalted water in the flowing side of potcher
To opposite.
Wherein, preferably：
Desalination coolant-temperature gage is 45-55 DEG C；
It is 50-60 DEG C to spray coolant-temperature gage.
As-spun fibre tow residence time in described device is 60-144 seconds；
As-spun fibre tow is 1-5 seconds in the rinsing tank residence time.
The present invention can specifically use following technical scheme：
Desalted water in desalination water pot is conveyed by desalination water pump, be delivered to after being heated by plate type heat exchanger rinsing tank and
Rinsing machine circulating water chennel.In rinsing tank rinsing machine circulating water chennel, rinsing machine circulating water chennel wash-in are entered after desalted water overflow
Water is washed from rear to preceding successively overflow, the flow direction of washings is opposite with tow direction of advance.As-spun fibre tow is through overpickling
After processing, pickling residue and sodium ion absorption are had in fibrous inside, tow enters after rinsing machine, washing in circulating water chennel
Wash water and shower is delivered to by feeding spraying pump, washings have spray nozzle ejection, and vaporific water curtain, tow are formed between water fender
Passed through in vaporific water curtain, displacement tow internal moisture reaches the purpose of washing, and the water after washing is back to along water fender to follow
Ring tank is circulated, and in order to ensure the effect of washing, rinsing machine circulating water chennel keeps a certain amount of desalted water to add, by washing
The washings of machine overfall outflow are delivered to sewage disposal and handled.
Fibre bundle is entered in potcher after rinsing machine washing, and tow is rinsed in desalination water-bath, silk
Beam lead is opposite with desalted water flow direction.
The effect of invention：
Employ during sodium sulfocyanate prepares carbon fibre precursor for solvent, having a certain amount of sodium ion, to be wrapped in carbon fine
Tie up in as-spun fibre, fiber adheres to pickling residue and sodium ion, pickling processes after descaling bath processing on fibre bundle
Afterwards without secondary washing, fibre bundle is directly in the carbon fibre precursor that oils, is dried to obtain, analysis detection carbon fibre precursor
Sodium ions content be 340ppm.
Water washing device is provided after pickling processes, secondary washing, washing temperature >=55 are carried out to PAN base carbon fiber protofilaments
DEG C, tow was in water washing device residence time ＞ 60 seconds, and fibre bundle obtains carbon fiber by the process such as oil, dry after washing
Sodium ions content in precursor, analysis detection carbon fibre precursor is reduced to below 150ppm.
It is staggered in apparatus of the present invention above and below the seal wire roller group of rinsing machine, adds effective row of the tow in rinsing machine
Journey, washing length is up to 60 meters, and provided with three sections of tanks, every section of alone cycle, successively overflow, with tow traffic direction on the contrary,
Certain concentration difference is kept, the efficiency of washing is improved, reduces sodium ion in tow, improve the quality of precursor.So this
Invention device and method can effectively wash PAN based precursors, the sodium ion of fibre bundle be reduced, so as to improve carbon fibre precursor
Quality.
Brief description of the drawings
The carbon fibre precursor wash mill schematic diagram of Fig. 1 present invention；
Description of reference numerals：
1 desalination water pot；2 desalted water delivery pumps；3 plate type heat exchangers；4 pickling traction roller groups；5 feeding spraying pumps；6 recirculated waters
Groove；7 snakelike heating coils；8 spray nozzles；9 rinsing machine seal wire roller groups；10 rinsing tanks；11 rinsing traction roller groups；12 water fenders；
13 steam；14 condensate liquids.
Embodiment
With reference to embodiment, the present invention is further illustrated.
Embodiment 1
As shown in figure 1, a kind of device for washing carbon fibre precursor.
Described device is arranged in spinning technique after pickling processes.
Described device includes：
Rinsing machine seal wire roller group 9, circulating water chennel 6, snakelike heating coil 7, feeding spraying pump 5, spray nozzle 8, rinsing tank 10,
Water fender 12；
Snakelike heating coil 7 is laid on the bottom of circulating water chennel 6, heats the washings of rinsing machine circulating water chennel.
Rinsing machine seal wire roller group 9 is arranged on the top of circulating water chennel 6, the tow come out by pickling traction roller group 4, through washing
Machine seal wire roller group 9 is drawn through rinsing machine, into potcher 10, then is drawn by rinsing traction roller group 11 to next procedure.
Washings in circulating water chennel 6, shower is delivered to by feeding spraying pump 5, and will wash Water spray by spray nozzle 8 exists
On tow, the water after washing falls back to circulating water chennel, is circulated.
The rinsing tank 10 is provided with overfall；
The rinsing machine circulating water chennel 6 is provided with overfall.
Desalination water pot 1, desalted water delivery pump 2, plate type heat exchanger 3 are sequentially connected；Washings are conveyed by desalination water pump 2.
The wash mill is provided with water fender 12, water fender 12 be arranged on adjacent two godets up and down staggeredly it
Between, parallel in adjacent two seal wire roller group traffic directions up and down with tow, tow passes through between shower and water fender.Dash
Plate can adjust with tow spacing distance.
It is generally to use sodium sulfocyanate for solvent to use sodium rhodanate one-step method to prepare carbon fiber, acrylonitrile, second comonomer
Methyl acrylate, Third monomer itaconic acid are raw material, and azodiisobutyronitrile is that initiator carries out binary polymerization reaction, by de-
Polyacrylonitrile polymer fluid is obtained after single, deaeration.By wet spinning, formed at as-spun fibre tow, the washing of tow process, pickling
After reason, secondary washing carrying out washing treatment is carried out using Fig. 1 device.Acidwash solution concentration 1%, 75 DEG C of temperature, tow is through peracid
Dilution, secondary washing, shower water temperature 50 C, tow residence time 80 seconds in rinsing machine are carried out into wash mill.Wash
Enter desalted water temperature 50 C in potcher, potcher, tow and potcher desalted water counter flow washing, 2 seconds residence times after washing.
Tow after rinsing obtains carbon fibre precursor by the process such as oil, dry, by analysis detection carbon fibre precursor tow sodium from
Sub- content is 142ppm.
Embodiment 2
It is generally to use sodium sulfocyanate for solvent to use sodium rhodanate one-step method to prepare carbon fiber, acrylonitrile, second comonomer
Methyl acrylate, Third monomer itaconic acid are raw material, and azodiisobutyronitrile is that initiator carries out binary polymerization reaction, by de-
Polyacrylonitrile polymer fluid is obtained after single, deaeration.By wet spinning, formed at as-spun fibre tow, the washing of tow process, pickling
After reason, secondary washing carrying out washing treatment is carried out using Fig. 1 device.Acidwash solution concentration 1%, 75 DEG C of temperature, tow is through peracid
Dilution, into the secondary washing of rinsing machine, 55 DEG C of secondary washing coolant-temperature gage, tow residence time 60 seconds in rinsing machine.Washing
Enter desalted water temperature 50 C in potcher, potcher, tow and potcher desalted water counter flow washing, 4 seconds residence times afterwards.Drift
Tow after washing obtains carbon fibre precursor by the process such as oil, dry, by analysis detection carbon fibre precursor tow sodium ion
Content is 126ppm.
Embodiment 3
It is generally to use sodium sulfocyanate for solvent to use sodium rhodanate one-step method to prepare carbon fiber, acrylonitrile, second comonomer
Methyl acrylate, Third monomer itaconic acid are raw material, and azodiisobutyronitrile is that initiator carries out binary polymerization reaction, by de-
Polyacrylonitrile polymer fluid is obtained after single, deaeration.By wet spinning, formed at as-spun fibre tow, the washing of tow process, pickling
After reason, secondary washing carrying out washing treatment is carried out using Fig. 1 device.Acidwash solution concentration 1%, 75 DEG C of temperature, tow is through peracid
Dilution, into the secondary washing of rinsing machine, second wash water temperature 60 C, tow residence time 120 seconds in rinsing machine.Washing
Enter desalted water temperature 50 C in potcher, potcher, tow and potcher desalted water counter flow washing, 4 seconds residence times afterwards.Drift
Tow after washing obtains carbon fibre precursor by the process such as oil, dry, by analysis detection carbon fibre precursor tow sodium ion
Content is 80ppm.
Embodiment 4
It is generally to use sodium sulfocyanate for solvent to use sodium rhodanate one-step method to prepare carbon fiber, acrylonitrile, second comonomer
Methyl acrylate, Third monomer itaconic acid are raw material, and azodiisobutyronitrile is that initiator carries out binary polymerization reaction, by de-
Polyacrylonitrile polymer fluid is obtained after single, deaeration.By wet spinning, formed at as-spun fibre tow, the washing of tow process, pickling
After reason, secondary washing carrying out washing treatment is carried out using Fig. 1 device.Acidwash solution concentration 1%, temperature 50 C, tow is through peracid
Dilution, into the secondary washing of rinsing machine, 55 DEG C of secondary washing coolant-temperature gage, tow residence time 70 seconds in rinsing machine.Washing
Enter desalted water temperature 50 C in potcher, potcher, tow and potcher desalted water counter flow washing, 3 seconds residence times afterwards.Drift
Tow after washing obtains carbon fibre precursor by the process such as oil, dry, by analysis detection carbon fibre precursor tow sodium ion
Content is 136ppm.
Comparative example 1
It is generally to use sodium sulfocyanate for solvent to use sodium rhodanate one-step method to prepare carbon fiber, acrylonitrile, second comonomer
Methyl acrylate, Third monomer itaconic acid are raw material, and azodiisobutyronitrile is that initiator carries out binary polymerization reaction, by de-
Polyacrylonitrile polymer fluid is obtained after single, deaeration.By wet spinning, formed at as-spun fibre tow, the washing of tow process, pickling
After reason, handled by potcher, then by oiling, being dried to obtain carbon fibre precursor, carbon fibre precursor silk is detected by analysis
Sodium ions content is 340ppm in beam.
Can be seen that the present apparatus and method by the data of embodiment and comparative example can effectively wash pickling and treat
Carbon fibre precursor, substantially reduce the sodium ion in tow, hence it is evident that improve carbon fibre precursor quality.
Claims (10)
1. a kind of carbon fibre precursor wash mill, it is characterised in that described device includes：
Rinsing machine seal wire roller group, circulating water chennel, feeding spraying pump, spray nozzle, rinsing tank；
Rinsing machine seal wire roller group is arranged in above circulating water chennel, staggered above and below godet, and there is squeeze roller group outlet, through peracid
The tow of processing is washed by rinsing machine seal wire roller group and squeeze roller group, into rinsing tank；
Spray nozzle is provided with above rinsing machine seal wire roller group；Spray nozzle is connected with feeding spraying pump.
2. carbon fibre precursor wash mill as claimed in claim 1, it is characterised in that：
The circulating water chennel bottom is provided with snakelike heating coil.
3. carbon fibre precursor wash mill as claimed in claim 2, it is characterised in that：
The circulating water chennel is divided into three sections of tanks, every section of alone cycle water, successively overflow；
The circulating water chennel is provided with downflow weir and overfall.
4. carbon fibre precursor wash mill as claimed in claim 1, it is characterised in that：
The potcher is provided with downflow weir and overfall.
5. the carbon fibre precursor wash mill as described in one of Claims 1 to 4, it is characterised in that：
The wash mill is provided with water fender, and water fender is arranged between adjacent two godets up and down staggeredly, with tow
Parallel in adjacent two seal wire roller group traffic directions up and down, tow passes through between shower and water fender.
6. the wash mill of carbon fibre precursor as claimed in claim 5, it is characterised in that：
Desalination water pot, desalted water delivery pump, plate type heat exchanger connect rinsing tank and circulating water chennel respectively after being sequentially connected.
7. a kind of washing methods of carbon fibre precursor wash mill using as described in one of claim 1~6, it is characterised in that
Methods described includes：
1) after desalted water heating, it is delivered to rinsing tank；
2) desalted water enters rinsing machine circulating water chennel by overflow in rinsing tank, in circulating water chennel overflow, before direction and tow
Enter in opposite direction；
3) tow enters rinsing machine after pickling processes, and shower water is emitted into atomized water from spray nozzle, and tow is washed；
4) is rinsed after tow is scrubbed into potcher, the flow direction phase of tow direction of advance and desalted water in potcher
Instead.
8. washing methods as claimed in claim 7, it is characterised in that：
Desalination coolant-temperature gage is 45-55 DEG C；
It is 50-60 DEG C to spray coolant-temperature gage.
9. washing methods as claimed in claim 7, it is characterised in that：
As-spun fibre tow residence time in the wash mill is 60-144 seconds.
10. washing methods as claimed in claim 9, it is characterised in that：
As-spun fibre tow is 1-5 seconds in the rinsing tank residence time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710479377.3A CN107268215A (en) | 2017-06-22 | 2017-06-22 | A kind of carbon fibre precursor wash mill and washing methods |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710479377.3A CN107268215A (en) | 2017-06-22 | 2017-06-22 | A kind of carbon fibre precursor wash mill and washing methods |
Publications (1)
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| CN108251898A (en) * | 2018-04-12 | 2018-07-06 | 江苏恒神股份有限公司 | Polyacrylonitrile-based carbon fibre oil feeding system |
| CN109680431A (en) * | 2019-01-01 | 2019-04-26 | 谢吉芳 | A kind of weaving security protection textile material flusher |
| CN110079990A (en) * | 2019-05-09 | 2019-08-02 | 威海拓展纤维有限公司 | Prepare carbon fibre precursor method for washing |
| CN111893668A (en) * | 2020-07-07 | 2020-11-06 | 山西钢科碳材料有限公司 | Homogenization treatment device and method, and preparation method of polyacrylonitrile-based carbon fiber |
| CN114250562A (en) * | 2021-12-28 | 2022-03-29 | 张家港市港鹰实业有限公司 | Improved carbon fiber precursor washing device and washing method |
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Application publication date: 20171020 |