CN107130445B - A method of improving dyeing polyimide fiber mechanical property - Google Patents
A method of improving dyeing polyimide fiber mechanical property Download PDFInfo
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- CN107130445B CN107130445B CN201710355406.5A CN201710355406A CN107130445B CN 107130445 B CN107130445 B CN 107130445B CN 201710355406 A CN201710355406 A CN 201710355406A CN 107130445 B CN107130445 B CN 107130445B
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- dyeing
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- polyimide fiber
- imidization
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- 239000000835 fiber Substances 0.000 title claims abstract description 125
- 238000004043 dyeing Methods 0.000 title claims abstract description 66
- 239000004642 Polyimide Substances 0.000 title claims abstract description 61
- 229920001721 polyimide Polymers 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 29
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims abstract description 36
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000126 substance Substances 0.000 claims abstract description 24
- 229920005575 poly(amic acid) Polymers 0.000 claims abstract description 23
- 125000002091 cationic group Chemical group 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000005530 etching Methods 0.000 claims abstract description 13
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000007363 ring formation reaction Methods 0.000 claims abstract description 6
- 239000000975 dye Substances 0.000 claims description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000654 additive Substances 0.000 claims description 7
- 230000000996 additive effect Effects 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 239000000908 ammonium hydroxide Substances 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 7
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 6
- 150000001768 cations Chemical class 0.000 abstract description 6
- 230000007423 decrease Effects 0.000 abstract description 4
- 230000002787 reinforcement Effects 0.000 abstract description 3
- 239000012783 reinforcing fiber Substances 0.000 abstract description 3
- 238000007788 roughening Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 8
- 239000004952 Polyamide Substances 0.000 description 6
- 238000005576 amination reaction Methods 0.000 description 6
- 239000004744 fabric Substances 0.000 description 6
- 229920002647 polyamide Polymers 0.000 description 6
- 125000005462 imide group Chemical group 0.000 description 5
- 150000002466 imines Chemical class 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002166 wet spinning Methods 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000010010 raising Methods 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- UPLPHRJJTCUQAY-WIRWPRASSA-N 2,3-thioepoxy madol Chemical compound C([C@@H]1CC2)[C@@H]3S[C@@H]3C[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@](C)(O)[C@@]2(C)CC1 UPLPHRJJTCUQAY-WIRWPRASSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- -1 and still Substances 0.000 description 1
- 230000003471 anti-radiation Effects 0.000 description 1
- 239000000981 basic dye Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000006210 cyclodehydration reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/16—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dispersed, e.g. acetate, dyestuffs
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
- D06M11/59—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with ammonia; with complexes of organic amines with inorganic substances
- D06M11/60—Ammonia as a gas or in solution
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/76—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon oxides or carbonates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/188—Monocarboxylic acids; Anhydrides, halides or salts thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/35—Heterocyclic compounds
- D06M13/355—Heterocyclic compounds having six-membered heterocyclic rings
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/02—Material containing basic nitrogen
- D06P3/024—Material containing basic nitrogen using dispersed dyes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Coloring (AREA)
Abstract
The present invention relates to a kind of methods for improving dyeing polyimide fiber mechanical property, method includes the following steps: polyamic acid fiber is infiltrated in acetic anhydride/pyridine solution, carry out chemical imidization；The fiber drying of chemical imidization, thermal cyclization are obtained into polyimide fiber；Polyimide fiber is pre-processed using alkaline etching；Dispersible cationic dyeing is used after being washed, being dried, and is washed, is dried after dyeing.The present invention reduces the defect sturcture of fiber using chemically and thermally imidization simultaneously, improves the uniformity of imidization degree, reinforcing fiber mechanical property；Polyimide fiber surface roughening is made using alkaline etching, and the diffusing reflection reinforcement to the total reflection decrease of light, and open the part imide bond of fiber surface, being conducive to the cation on next step dye molecule can effectively solve the problems, such as that polyimide fiber dyeing is difficult in conjunction with carboxyl generation ionic bond.Simple process, the fiber colour depth dyed is high, good color fastness, and mechanical property is good.
Description
Technical field
The invention belongs to textile dyeing fields, and in particular to a kind of side for improving dyeing polyimide fiber mechanical property
Method.
Background technique
Polyimides (PI) is a kind of polymer material that chemical stability is fabulous, with excellent mechanical performances and heat-resisting
Performance, dielectric properties outstanding and the performances such as anti-radiation, it is each to be widely used in Aeronautics and Astronautics, microelectronics, seperation film and laser etc.
The critical material in field.
But with the development of science and technology, propose higher, harsher requirement to material, dyed polymers fibre how is improved
The mechanical property of dimension receives the extensive concern of people.
At present polyimide fiber mainly pass through polyamic acid (PAA) wet spinning through thermal cyclization obtain polyimides fibre
Dimension, is handled fiber surface using alkaline etching, reusing basic dye makes fibre staining.But due in heat treatment process,
The cyclodehydration of PAA is concentrated mainly on fiber sheath, and the removing of fibrous inside imidization small molecule water cause hole defect and
Imidization is uneven, and alkaline etching process destroys seriously the imide ring on surface.Therefore, in order to lower fibrous inside defect,
Imidization uniform level is improved, the mechanical property for improving coloured fibre becomes the key of problem.
In addition, it is sub- that chemistry is added in PAA spinning solution mostly in the prior art in traditional PAA wet spinning technology
Amination reagent, then hot imidization obtains polyimide fiber again, but since polyimides is exhausted insoluble in DMAc, DMF, NMP etc.
Most of organic solvents, so the dosage of chemical imidization reagent is less, the imidization degree for obtaining polyimide fiber compares
Low, mechanical property is also poor.Existing another kind technology is first hot imidization, then chemical imidization obtains polyimides fibre
Dimension, but due in such method chemical imidization process can remove small molecule water, cause fiber surface defect, can equally make fiber
Performance decline.
Summary of the invention
In order to overcome the above-mentioned problems in the prior art, the present invention provides a kind of raisings to dye polyimide fiber
The method of mechanical property, to improve dyeing polyimide fiber mechanical property, this method use simultaneously chemical imidization with
Hot imidization reduces the defect sturcture of fiber, improves the uniformity of imidization degree, reinforcing fiber mechanical property；Using alkali
Etching makes polyimide fiber surface roughening, and the diffusing reflection reinforcement to the total reflection decrease of light, and makes fiber surface
Part imide ring open, be conducive to have in conjunction with carboxyl ionic bond can occur for cation on next step dye molecule
Effect solves the problems, such as that polyimide fiber dyeing is difficult, and since the alkaline etching time is shorter, to the imide ring knot of fibrous inside
Structure destruction is limited, so its mechanical property also can largely be retained.
In order to realize above-mentioned purpose of the invention, spy is adopted the following technical scheme that
A method of dyeing polyimide fiber mechanical property is improved, is included the following steps:
(a) polyamic acid (PAA) fiber is infiltrated in acetic anhydride/pyridine solution, carries out chemical imidization；
(b) by the fiber drying of chemical imidization, thermal cyclization, polyimides (PI) fiber is obtained；
(c) polyimide fiber is pre-processed using alkaline etching；
(d) dispersible cationic dyeing is used after pretreated fiber is washed, dried, and is washed after dyeing, drying is
It can.
Further, in order to improve the uniformity of fibrous inside imidization degree, acetic anhydride/pyridine described in step (a) is molten
Liquid volume ratio is acetic anhydride/pyridine=2:1-1:2, infiltrating time 4h-24h.
Further, it is screened through many experiments, the polyimide fiber mechanical property obtained using the following conditions is more outstanding,
The drying process used in step (b) are as follows: fiber is at the uniform velocity passed through to the tube furnace that temperature is 60-100 DEG C, time 1-5min；
Thermal cyclization process are as follows: PAA fiber is at the uniform velocity first passed through into the tube furnace that temperature is 150-300 DEG C, time 1-5min；Then will
PAA fiber at the uniform velocity passes through the tube furnace that temperature is 350-550 DEG C, time 1-5min.
Further, in order to improve the depth of color of fiber, color fastness makes fiber surface generate more carboxyls, in order to
Occur in conjunction with ionic bond with the cation on dye molecule later, during the alkaline etching of use: polyimide fiber is put into
In lye, bath raio 1:60-1:200 is ultrasonically treated 10-80min at 20 DEG C -80 DEG C, wherein lye is that sodium hydroxide is molten
One or more of solution such as liquid, potassium hydroxide solution, ammonium hydroxide, sodium carbonate.
Further, in order to keep the cation on dye molecule more abundant in conjunction with the ionic bond of carboxyl, dispersible cationic dye
The additive amount of material is the 1%-7% of the polyimides fabric weight, and dyeing dye liquor pH value used is 4-6, the bath raio of dyeing
For 1:50-1:200；When dyeing, heating rate is 1-3 DEG C/min, and the temperature of dyeing is 100-160 DEG C, soaking time 20-
100min。
Further, after dyeing, fiber is cleaned, is dried, water-washing process are as follows: in 40 DEG C -60 DEG C of deionized water,
It is ultrasonically treated 20-40min；Drying course are as follows: dry 30-80min in 60-80 DEG C of baking oven.
Compared with prior art, the invention has the benefit that
1) chemical imidization process is added in the method for the present invention during traditional hot imidization, reduces the defect of fiber
Structure improves the uniformity of imidization degree, has the mechanical property of fiber and largely improves.
2) the method for the present invention is modified fiber surface using alkaline etching process, is conducive on next step dye molecule
In conjunction with carboxyl ionic bond can occur for cation, dye level is high, good color fastness；At the same time, not to fibrous inner structure
There is too havoc, is that the mechanical property of fiber is effectively maintained, mechanical property is good.
3) the method for the present invention simple process, strong operability.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated, but the present invention is not limited to following embodiments.
The person that is not specified actual conditions in embodiment, carries out according to conventional conditions or manufacturer's recommended conditions.Agents useful for same or instrument are not
Production firm person is indicated, is the conventional products (explanation: in following embodiments, " without change that can be obtained by commercially available purchase
Polyimide fiber before learning imidization dyeing " is the strong mechanical performance polyimides fibre obtained using conventional wet spinning process
Dimension, " polyimide fiber after dyeing without chemical imidization " is the dyeing polyimides obtained using conventional coloring method
Fiber).
Embodiment one
1) polyamic acid (PAA) fiber is infiltrated in acetic anhydride/pyridine solution that volume ratio is 2:1, it is sub- carries out chemistry
Amination, infiltrating time 12h；
2) fiber of chemical imidization is cleaned, is then at the uniform velocity dried by the tube furnace that temperature is 80 DEG C, the time
For 1min；Fiber is at the uniform velocity passed through to the tube furnace that temperature is 200 DEG C, time 2min；Then at the uniform velocity it is by temperature by fiber
420 DEG C of tube furnace, time 4min；
3) polyimide fiber is put into lye, bath raio 1:150 is ultrasonically treated 60min at 60 DEG C；
4) it is washed, dispersible cationic dyeing is used after dry, the additive amount of dispersible cationic dyestuff is the polyamides
The 6% of imines fabric weight, dyeing dye liquor pH value used is 5, and the bath raio of dyeing is 1:150；When dyeing, heating rate 2
DEG C/min, and the temperature of dyeing is 160 DEG C, soaking time 80min, after dyeing in 60 DEG C of deionized water, ultrasonic treatment
30min；Drying course are as follows: dry 80min in 60 DEG C of baking oven, the polyimide fiber after being dyed.And with without
Imidization dye it is front/rear, dyed by imidization before mechanical property, the dyeability of fiber make comparisons, see such as following table 1-1,1-
2。
The mechanical property of table 1-1 polyimide fiber
The dyeability of table 1-2 polyimide fiber
As can be seen from the above table, if having little effect by dyeability of the chemical imidization to fiber, still, change
Learning promotion of the imidization to fibrous mechanical property, the good results are evident, and dyeing course influence that fibrous mechanical property is changed compared with
It is small.
Embodiment two
1) polyamic acid (PAA) fiber is infiltrated in acetic anhydride/pyridine solution that volume ratio is 1:1, it is sub- carries out chemistry
Amination；
2) fiber of chemical imidization is cleaned, is then at the uniform velocity dried by the tube furnace that temperature is 100 DEG C, the time
For 2min；Fiber is at the uniform velocity passed through to the tube furnace that temperature is 150 DEG C, time 3min；Then at the uniform velocity it is by temperature by fiber
350 DEG C of tube furnace, time 5min；
3) polyimide fiber is put into lye, bath raio 1:150 is ultrasonically treated 60min at 40 DEG C；
4) it is washed, dispersible cationic dyeing is used after dry, the additive amount of dispersible cationic dyestuff is the polyamides
The 4% of imines fabric weight, dyeing dye liquor pH value used is 5, and the bath raio of dyeing is 1:150；When dyeing, heating rate 1
DEG C/min, and the temperature of dyeing is 100 DEG C, soaking time 100min, after dyeing in 40 DEG C of deionized water, ultrasonic treatment
20min；Drying course are as follows: dry 80min in 60 DEG C of baking oven, the polyimide fiber after being dyed.And with without
Imidization dye it is front/rear, dyed by imidization before mechanical property, the dyeability of fiber make comparisons, see such as following table 2-1,2-
2。
The mechanical property of table 2-1 polyimide fiber
The dyeability of table 2-2 polyimide fiber
As can be seen from the above table, if having little effect by dyeability of the chemical imidization to fiber, still, change
Learning promotion of the imidization to fibrous mechanical property, the good results are evident, and dyeing course influence that fibrous mechanical property is changed compared with
It is small.
Embodiment three
1) polyamic acid (PAA) fiber is infiltrated in acetic anhydride/pyridine solution that volume ratio is 1:2, it is sub- carries out chemistry
Amination；
2) fiber of chemical imidization is cleaned, is then at the uniform velocity dried by the tube furnace that temperature is 60 DEG C, the time
For 5min；Fiber is at the uniform velocity passed through to the tube furnace that temperature is 300 DEG C, time 1min；Then at the uniform velocity it is by temperature by fiber
510 DEG C of tube furnace, time 2min；
3) polyimide fiber is put into lye, bath raio 1:60 is ultrasonically treated 20min at 80 DEG C；
4) it is washed, dispersible cationic dyeing is used after dry, the additive amount of dispersible cationic dyestuff is the polyamides
The 1% of imines fabric weight, dyeing dye liquor pH value used is 4, and the bath raio of dyeing is 1:60；When dyeing, heating rate 3
DEG C/min, and the temperature of dyeing is 160 DEG C, soaking time 20min, after dyeing in 20 DEG C of deionized water, ultrasonic treatment
40min；Drying course are as follows: dry 30min in 80 DEG C of baking oven, the polyimide fiber after being dyed.And with without
Imidization dye it is front/rear, dyed by imidization before mechanical property, the dyeability of fiber make comparisons, see such as following table 3-1,3-
2。
The mechanical property of table 3-1 polyimide fiber
The dyeability of table 3-2 polyimide fiber
As can be seen from the above table, if having little effect by dyeability of the chemical imidization to fiber, still, change
Learning promotion of the imidization to fibrous mechanical property, the good results are evident, and dyeing course influence that fibrous mechanical property is changed compared with
It is small.
Example IV
1) polyamic acid (PAA) fiber is infiltrated in acetic anhydride/pyridine solution that volume ratio is 2:1, it is sub- carries out chemistry
Amination；
2) fiber of chemical imidization is cleaned, is then at the uniform velocity dried by the tube furnace that temperature is 100 DEG C, the time
For 1min；Fiber is at the uniform velocity passed through to the tube furnace that temperature is 230 DEG C, time 1min；Then at the uniform velocity it is by temperature by fiber
450 DEG C of tube furnace, time 2min；
3) polyimide fiber is put into lye, bath raio 1:200 is ultrasonically treated 30min at 80 DEG C；
4) it is washed, dispersible cationic dyeing is used after dry, the additive amount of dispersible cationic dyestuff is the polyamides
The 7% of imines fabric weight, dyeing dye liquor pH value used is 6, and the bath raio of dyeing is 1:200；When dyeing, heating rate 3
DEG C/min, and the temperature of dyeing is 130 DEG C, soaking time 60min, after dyeing in 60 DEG C of deionized water, ultrasonic treatment
40min；Drying course are as follows: dry 60min in 50 DEG C of baking oven, the polyimide fiber after being dyed.And with without
Imidization dye it is front/rear, dyed by imidization before mechanical property, the dyeability of fiber make comparisons, see such as following table 4-1,4-
2。
The mechanical property of table 4-1 polyimide fiber
The dyeability of table 4-2 polyimide fiber
As can be seen from the above table, if having little effect by dyeability of the chemical imidization to fiber, still, change
Learning promotion of the imidization to fibrous mechanical property, the good results are evident, and dyeing course influence that fibrous mechanical property is changed compared with
It is small.
Embodiment five
1) polyamic acid (PAA) fiber is infiltrated in acetic anhydride/pyridine solution that volume ratio is 2:1, it is sub- carries out chemistry
Amination；
2) fiber of chemical imidization is cleaned, is then at the uniform velocity dried by the tube furnace that temperature is 80 DEG C, the time
For 1min；Fiber is at the uniform velocity passed through to the tube furnace that temperature is 320 DEG C, time 2min；Then at the uniform velocity it is by temperature by fiber
550 DEG C of tube furnace, time 1min；
Polyimide fiber is put into lye, bath raio 1:120 is ultrasonically treated 60min at 60 DEG C；
It is washed, dispersible cationic dyeing is used after dry, the additive amount of dispersible cationic dyestuff is that the polyamides is sub-
The 6% of amine fabric weight, dyeing dye liquor pH value used is 6, and the bath raio of dyeing is 1:120；When dyeing, heating rate be 2 DEG C/
Min, the temperature of dyeing is 160 DEG C, soaking time 80min, after dyeing in 60 DEG C of deionized water, is ultrasonically treated 40min；
Drying course are as follows: dry 60min in 50 DEG C of baking oven, the polyimide fiber after being dyed.And with without imidization
Dye it is front/rear, dyed by imidization before mechanical property, the dyeability of fiber make comparisons, see such as following table 5-1,5-2.
The mechanical property of table 5-1 polyimide fiber
The dyeability of table 5-2 polyimide fiber
As can be seen from the above table, if having little effect by dyeability of the chemical imidization to fiber, still, change
Learning promotion of the imidization to fibrous mechanical property, the good results are evident, and dyeing course influence that fibrous mechanical property is changed compared with
It is small.
To sum up embodiment is as it can be seen that the method provided by the invention for improving dyeing polyimide fiber mechanical property, passing through
Learning imidization reduces the defect sturcture of fiber, improves the uniformity of imidization degree, reinforcing fiber mechanical property；Using alkali
Etching makes polyimide fiber surface roughening, and the diffusing reflection reinforcement to the total reflection decrease of light, and makes fiber surface
Part imide ring open, be conducive to have in conjunction with carboxyl ionic bond can occur for cation on next step dye molecule
Effect solves the problems, such as that polyimide fiber dyeing is difficult, and since the alkaline etching time is shorter, to the imide ring knot of fibrous inside
Structure destruction is limited, so its mechanical property also can largely be retained.Polyamides is dyed using raising provided by the invention
The method of imine fiber mechanical property has little effect the dyeability of fiber, and still, chemical imidization is to fiber mechanics
The good results are evident for the promotion of performance, has achieved the purpose that improve dyeing polyimide fiber mechanical property.
Although the present invention is illustrate and described with specific embodiment, however it will be appreciated that without departing substantially from essence of the invention
Many other change and modification can be made in the case where mind and range.Therefore, it means that wrap in the following claims
Include all such changes and modifications belonged in the scope of the invention.
Claims (2)
1. a kind of method for improving dyeing polyimide fiber mechanical property, includes the following steps:
(a) polyamic acid fiber is infiltrated in acetic anhydride/pyridine solution, carries out chemical imidization；
(b) by the fiber drying of chemical imidization, thermal cyclization, polyimide fiber is obtained；
(c) polyimide fiber is pre-processed using alkaline etching；
(d) dispersible cationic dyeing is used after pretreated fiber is washed, dried, and is washed, is dried after dyeing；
Acetic anhydride described in step (a)/pyridine solution volume ratio is acetic anhydride/pyridine=2:1-1:2, and fiber infiltrating time is
4h-24h；
The drying process used in step (b) are as follows: fiber is at the uniform velocity passed through to the tube furnace that temperature is 60-120 DEG C, time 1-
5min；
The thermal cyclization process used in step (b) are as follows: polyamic acid fiber is at the uniform velocity first passed through into the tubular type that temperature is 150-300 DEG C
Furnace, time 1-5min；Then polyamic acid fiber is at the uniform velocity passed through into the tube furnace that temperature is 350-550 DEG C, time 1-
5min；
The alkaline etching process used in step (c) are as follows: polyimide fiber is put into lye, bath raio 1:60-1:200,
10-80min is ultrasonically treated at 20 DEG C -80 DEG C, wherein lye is sodium hydroxide solution, potassium hydroxide solution, ammonium hydroxide, sodium carbonate
One or more of solution；
The additive amount of dispersible cationic dyestuff described in step (d) is the 1%-7% of polyimide fiber weight, is dyed used
Dye liquor pH value is 4-6, and the bath raio of dyeing is 1:50-1:200；
In step (d) when dyeing, heating rate is 1-3 DEG C/min, and the temperature of dyeing is 100-160 DEG C, soaking time 20-
100min。
2. a kind of method for improving dyeing polyimide fiber mechanical property according to claim 1, which is characterized in that step
Suddenly water-washing process described in (d) are as follows: in 40 DEG C -60 DEG C of deionized water, be ultrasonically treated 20-40min；The drying course
Are as follows: 30-80min is dried in 60-80 DEG C of baking oven.
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| CN107723826B (en) * | 2017-11-03 | 2020-01-14 | 东华大学 | Method for continuously producing colored polyimide fibers by two-step method |
| CN108772933A (en) * | 2018-06-12 | 2018-11-09 | 阜南县腾博工艺品有限公司 | A kind of colouring method of enhancing cotton stalk mechanical property |
| CN109235073A (en) * | 2018-09-29 | 2019-01-18 | 青岛亿天环保科技有限公司 | A kind of cationic dyeing method of polyimide fiber |
| CN110130120A (en) * | 2019-04-12 | 2019-08-16 | 武汉纺织大学 | A method of for high-performance textile low temperature dyeing |
| CN111387646B (en) * | 2020-02-18 | 2022-03-25 | 李宁（中国）体育用品有限公司 | Ribbon and preparation method thereof |
| CN113529272B (en) * | 2020-04-17 | 2023-04-28 | 北京化工大学 | Polyimide nanofiber membrane with carboxyl functional elements on surface and preparation method thereof |
| CN113445331A (en) * | 2021-07-22 | 2021-09-28 | 绍兴市柯桥区东纺纺织产业创新研究院 | Dyeing method for improving dyeing performance of polyimide fibers |
| CN113818097A (en) * | 2021-10-21 | 2021-12-21 | 江苏先诺新材料科技有限公司 | Polyimide fiber and method for producing polyimide fiber |
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