CN107130445B - A method of improving dyeing polyimide fiber mechanical property - Google Patents

A method of improving dyeing polyimide fiber mechanical property Download PDF

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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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fiber
dyeing
mechanical property
polyimide fiber
imidization
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CN107130445A (en
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武德珍
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JIANGSU XIANNUO NEW MATERIAL TECHNOLOGY Co Ltd
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JIANGSU XIANNUO NEW MATERIAL TECHNOLOGY Co Ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/16General 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
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/32Treating 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
    • D06M11/36Treating 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
    • D06M11/38Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/58Treating 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
    • D06M11/59Treating 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
    • D06M11/60Ammonia as a gas or in solution
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/73Treating 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
    • D06M11/76Treating 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
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/188Monocarboxylic acids; Anhydrides, halides or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating 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
    • D06M13/35Heterocyclic compounds
    • D06M13/355Heterocyclic compounds having six-membered heterocyclic rings
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/02Material containing basic nitrogen
    • D06P3/024Material containing basic nitrogen using dispersed dyes
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic 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

A method of improving dyeing polyimide fiber mechanical property
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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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

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105542458A (en) * 2016-01-19 2016-05-04 北京化工大学 High-strength high-toughness polyimide resin matrix composite and preparation method thereof

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1932091A (en) * 2006-09-28 2007-03-21 东华大学 Prepn process of polyimide fiber
CN101676321B (en) * 2008-09-18 2011-10-12 比亚迪股份有限公司 Method for preparing polyimide films
CN103541214B (en) * 2013-10-21 2016-05-11 绍兴文理学院 For improving the method for polyimide fiber basic dyeing performance
CN104532622B (en) * 2014-12-19 2016-08-24 东华大学 A kind of method of polyimide fiber disperse dyeing
CN104928790A (en) * 2015-06-08 2015-09-23 北京化工大学 Method for preparing polyimide fibers
CN105951435B (en) * 2016-06-06 2018-01-02 盐城工学院 A kind of colouring method of modified polyimide fabric

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105542458A (en) * 2016-01-19 2016-05-04 北京化工大学 High-strength high-toughness polyimide resin matrix composite and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
聚酰亚胺纤维的制备及结构与性能;高晋;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20040915(第3期);第B016-130页

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