CN105603719A - Preparation method of easy-to-dye polyimide fabric employing chemical reduction method - Google Patents

Preparation method of easy-to-dye polyimide fabric employing chemical reduction method Download PDF

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Publication number
CN105603719A
CN105603719A CN201610158990.0A CN201610158990A CN105603719A CN 105603719 A CN105603719 A CN 105603719A CN 201610158990 A CN201610158990 A CN 201610158990A CN 105603719 A CN105603719 A CN 105603719A
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China
Prior art keywords
fabric
polyimides
preparation
polyimide
reducing agent
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Pending
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CN201610158990.0A
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Chinese (zh)
Inventor
刘水平
鲁双
傅佳佳
朱亚楠
葛明桥
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Jiangnan University
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Jiangnan University
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Priority to CN201610158990.0A priority Critical patent/CN105603719A/en
Publication of CN105603719A publication Critical patent/CN105603719A/en
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    • 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
    • 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 System
    • 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
    • D06M11/51Treating 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 sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/52Treating 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 sulfur, selenium, tellurium, polonium or compounds thereof with selenium, tellurium, polonium or their compounds; with sulfur, dithionites or compounds containing sulfur and halogens, with or without oxygen; by sulfohalogenation with chlorosulfonic acid; by sulfohalogenation with a mixture of sulfur dioxide and free halogens
    • 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
    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • 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
    • 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
    • D06P3/004Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated using dispersed dyes
    • 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

Abstract

The invention relates to a preparation method of easy-to-dye polyimide fabric employing a chemical reduction method. The method comprises the following steps: (1) processing the polyimide fabric with an alkaline reducing liquid, to be specific, putting the polyimide fabric into a compressive container containing the alkaline reducing liquid, wherein the pressure is 0.1-0.2MPa, the temperature is 100-110 DEG C and the processing time is 10-60 minutes; and (2) washing the polyimide fabric: taking out and washing the polyimide fabric processed by the alkaline reducing solution for 6-10 times, and drying in an oven at 70-100 DEG C for 1-2 hours, wherein the alkaline reducing liquid is a mixed solution of sodium hydroxide or sodium carbonate and a reducing agent; the molar ratio of the sodium hydroxide or sodium carbonate to the reducing agent is 2 to 1; the molar percent concentration of the sodium hydroxide or sodium carbonate is 0.1%-10%; and the molar percent concentration of the reducing agent is 0.05%-5%. The polyimide fabric is changed into dyeable fabric from un-dyed fabric on the basis of not damaging the physical and chemical properties of the polyimide fabric; and the problem that polyimide is difficult to dye is solved.

Description

Chemical reduction method easily dyes the preparation method of polyimides fabric
Technical field
The present invention relates to the preparation method that a kind of chemical reduction method easily dyes polyimides fabric, belong to function weavingMaterial technology field.
Background technology
Polyimides satisfactory mechanical property, and both can bear the temperature up to 400 DEG C, again can be at-200 DEG CFollowing ultralow temperature keeps normal performance, also has good insulating properties, can say that overall performance is very goodGood. Due to these good performances, the development prospect of polyimides is also very considerable.
According to the difference of the monomer of composition polyimides, polyimides can be divided into the not aliphatic poly containing phenyl ringThe semi-aromatic polyimides that acid imide, a kind of monomer contain phenyl ring and two kinds of monomers are all containing the aromatic series of phenyl ringThree kinds of polyimides. And according to thermal property, can be divided into thermoplasticity and Thermocurable polyimide.
Polyimides is the polymer that contains imide ring structure (formula 1) on molecule main chain. Fragrance adoptionAcid imide can be by diversified monomer composition, and this makes its structure present variation. And polyimides simultaneouslyHave again outstanding combination property, this is that many macromolecular materials are too far behind to catch up. And it is diversified syntheticMethod and manufacturing process, can produce in a large number polyimides and be not subject to condition restriction. Multiple advantage aboveMake polyimide material have broad application surface, and in some high-tech areas as Aero-Space, electronics workIndustry, nanometer, laser etc., polyimides fabric is great Zhan brilliance especially.
Aromatic polyimide, because its unique chemical constitution has excellent combination property, mainly comprises:Good heat endurance, by 3,3 ', 4,4 '-bibenzene tetracarboxylic dianhydride (BPDA) and p-phenylenediamine (PPD) (PDA) instituteThe heat decomposition temperature of the polyimides of preparation is up to 600 DEG C[3]; Excellent resistance to low temperature, even at liquid heliumIn can embrittlement yet; Good dimensional stability and mechanical property; Excellent radiation resistance; Good insulationProperty and dielectricity; Excellent anti-flammability and low toxicity and good biocompatibility. Polyimides hasExcellent properties makes its extensive concern that has obtained people, develops the polyimides product of various ways; At presentThe polyimides product of successfully commercially producing has: film, fiber and engineering plastics etc.
At field of textiles, polyimide fiber has good good prospect, because it has better spinning property, in conjunction withThe premium properties of himself, can be applied to togs field. The good heat-proof quality of polyimides makesMust by its make protective clothing for proximity fire fighting be through very comfortable with it, and skin and its conformability better. Due toThe stability of polyimides, the clothing that has polyimides fabric to make is also long service time, not yielding,Very safe again. Meanwhile, application quantity, the demand of polyimides fabric aspect industrial and protective clothing is all very large,The much special work position of China all needs industrial and protective clothing in the time of work, and the demand of this respect is annualExceed 350,000 covers. Make so many industrial and protective clothings, the clothes that have heat-resistant fireproof performance that need every yearDress uses fiber up to 300 tons of left and right. Can say that the application of polyimides aspect clothes has very large advantage.
At nonwoven manufacture view, polyimide fiber also fully develops talents. The soldier of armoured force, racing driver, flyThe clothes that the special industries such as office staff need a large amount of fire-proof flame-retardant fibres to make at work, has polyimides faceThe nonwoven of material spinning is the optimal material that is applied to this part. The nonwoven that polyimide fiber is manufactured oftenCombining nano technology, forms high-tech nanometer product, has thermal property, very comfortable again, can the army of being used inWith national defence fields such as clothes, anti-chemical and biological weapons high-performance apparel, efficient smog protective face masks, also can come into peopleThe people masses' life, makes some and can eliminate the leisure type clothes of abnormal body odour.
Be difficult to dyeing but polyimides fabric will well apply also to need to solve, textile application is subject toA difficult problem for restriction.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of chemical reduction method easily to dye poly-The preparation method of acid imide fabric, adopt alkaline reduction solution to polyimides fabric carry out chemical modification andProcess, polyimide fiber surface produces a large amount of active groups after treatment, and obtains complex surface, increasesAdded and adhesion and the dye-uptake of dye molecule, acquisition can be dyed polyimides fabric.
According to technical scheme provided by the invention, a kind of chemical reduction method easily dyes the preparation side of polyimides fabricMethod, is characterized in that, comprises the following steps:
(1) polyimides fabric alkaline reduction solution-treated: polyimides fabric is put into and also filled alkalescenceIn the compression resistanted container tank of originality solution, pressure is 0.1-0.2Mpa, and temperature is 100-110 DEG C, and the processing time is10-60min;
(2) polyimides fabric washing: the polyimides fabric through alkaline reduction solution-treated is taken outWash 6-10 time and dry, drying and carry out in 70-100 DEG C of baking oven, drying time is 1-2h.
Further, also comprise the processing of polyimides dyeing fabric: the polyimides fabric after drying is adoptedDisperse dyes dye, and dyeing condition is 130-135 DEG C of water-bath, 0.3-0.5MPa, and dyeing time is 1-2h.
Further, described alkaline reduction solution is the mixed solution of NaOH or sodium carbonate and reducing agent,Wherein the mol ratio of NaOH or sodium carbonate and reducing agent is 2:1, mole percentage of NaOH or sodium carbonateConcentration is 0.1-10%, and the mole percent concentration of reducing agent is 0.05-5%.
Further, described reducing agent is sodium dithionite, sodium dithionate or vulcanized sodium.
The present invention on the basis of not damaging polyimides fabric physics and chemistry performance, make polyimides fabric byCan not dyeing, become can dyed shell fabrics, has solved the problem that polyimides is difficult to dyeing, and due to alkalescence alsoThe effect of originality solution makes fabric surface form a large amount of active groups, and amino wherein not only can dyestuffMolecule combination, has more very strong sterilizing function, can improve the antibacterial and sterilizing function of polyimides fabric,When having increased fabric added value, also expand its application within the scope of weaving.
Brief description of the drawings
Fig. 1 is the electron-microscope scanning figure of comparative example.
Fig. 2 is the electron-microscope scanning figure of embodiment 1.
Fig. 3 is the electron-microscope scanning figure of embodiment 2.
Fig. 4 is the electron-microscope scanning figure of embodiment 3.
Fig. 5 is the electron-microscope scanning figure of embodiment 4.
Fig. 6 is the electron-microscope scanning figure of embodiment 5.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1-5: a kind of chemical reduction method easily dyes the preparation method of polyimides fabric, comprises the following steps:
(1) polyimides fabric alkaline reduction solution-treated: polyimides fabric is put into and contained just like table 1In the compression resistanted container tank of shown alkaline reduction solution, pressure is 0.1-0.2MPa, and temperature is 100-110 DEG C,Time is 10-60min;
(2) polyimides fabric washing: will get through the polyimides fabric of alkaline reduction solution-treatedGo out to wash 6-10 time and dry, drying and carry out in 70-100 degree Celsius of baking oven, drying time is 1-2h.
Table 1
Test case 1: sem test
Respectively the sample of embodiment 1-5 and comparative example is carried out to sem test, result is respectively as Fig. 1-Fig. 6Shown in. As can see from Figure 1, without the fiber in the polyimides fabric of alkaline reduction solution-treatedSmooth surface can be seen from Fig. 2-6, and the fiber surface after alkaline reduction solution-treated presents multipleHydridization. Complicated surface more easily makes dye molecule upload, and has improved the dye-uptake of fabric; And through alkaliThe active group that property reducing solution fiber surface after treatment produces due to the fracture of macromolecular chain is as aminoWith hydroxyl being reduced etc., there is very strong activity, can be combined with dye molecule, increase the look of fabricFastness.
Test case 2: Washing inspection
The polyimides fabric of embodiment 1-5 and comparative example is dyeed, to judge alkali treatment effect. AdoptDisperse dyes, dyeing condition is 130-135 DEG C of water-bath, 0.3-0.5MPa, dyeing time is 1-2h. Specifically dyeMaterial and auxiliary agent, dyeing heating process be as Table 2,3:
Table 2 color additive
Dye well auxiliary agent Ratio/mass percentage concentration (%)
100%S_4RL 0.08
100%_5BL 0.08
HGL is dark blue 0.2
98% glacial acetic acid 0.78
TF-212 levelling agent 0.19
DM_1364 degreaser 0.51
Table 3 heating process that dyes
As shown in table 4 to the Washing assay after polyimides dyeing fabric.
Table 4
As can be seen from Table 4, the polyimides fabric Washing of process alkaline reduction solution-treatedBeing improved of undressed polyimides fabric, after alkaline reduction solution-treated, polyimidesThe dyeability of fabric is improved.

Claims (4)

1. chemical reduction method easily dyes a preparation method for polyimides fabric, it is characterized in that, comprises the following steps:
(1) polyimides fabric alkaline reduction solution-treated: polyimides fabric is put into the compression resistanted container tank that fills alkaline reduction solution, pressure is 0.1-0.2Mpa, temperature is 100-110 DEG C, the processing time is 10-60min;
(2) polyimides fabric washing: the polyimides fabric through alkaline reduction solution-treated is taken out to washing 6-10 time and dries, dry and carry out in 70-100 DEG C of baking oven, drying time is 1-2h.
2. chemical reduction method as claimed in claim 1 easily dyes the preparation method of polyimides fabric, it is characterized in that: also comprise the processing of polyimides dyeing fabric: adopt disperse dyes to dye the polyimides fabric after drying, dyeing condition is 130-135 DEG C of water-bath, 0.3-0.5MPa, dyeing time is 1-2h.
3. chemical reduction method as claimed in claim 1 easily dyes the preparation method of polyimides fabric, it is characterized in that: described alkaline reduction solution is the mixed solution of NaOH or sodium carbonate and reducing agent, wherein the mol ratio of NaOH or sodium carbonate and reducing agent is 2:1, the mole percent concentration of NaOH or sodium carbonate is 0.1-10%, and the mole percent concentration of reducing agent is 0.05-5%.
4. chemical reduction method as claimed in claim 3 easily dyes the preparation method of polyimides fabric, it is characterized in that: described reducing agent is sodium dithionite, sodium dithionate or vulcanized sodium.
CN201610158990.0A 2016-03-17 2016-03-17 Preparation method of easy-to-dye polyimide fabric employing chemical reduction method Pending CN105603719A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106930117A (en) * 2017-04-14 2017-07-07 江南大学 A kind of cationic dyeing method of polyimide fiber
CN110468582A (en) * 2019-08-19 2019-11-19 江苏工程职业技术学院 A kind of polyimide nonwoven fabric from color changing method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005264378A (en) * 2004-03-19 2005-09-29 Hanayama Kogyo Kk Method for producing polyester-based fabric
CN103541214A (en) * 2013-10-21 2014-01-29 绍兴文理学院 Method for improving basic dye dyeing property of polyimide fiber
CN104532622A (en) * 2014-12-19 2015-04-22 东华大学 Method for dyeing aromatic polyimide fiber with disperse dye
CN105401401A (en) * 2015-12-08 2016-03-16 江南大学 Preparation method of chemical surface modification easily-dyed polyimide fabric

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005264378A (en) * 2004-03-19 2005-09-29 Hanayama Kogyo Kk Method for producing polyester-based fabric
CN103541214A (en) * 2013-10-21 2014-01-29 绍兴文理学院 Method for improving basic dye dyeing property of polyimide fiber
CN104532622A (en) * 2014-12-19 2015-04-22 东华大学 Method for dyeing aromatic polyimide fiber with disperse dye
CN105401401A (en) * 2015-12-08 2016-03-16 江南大学 Preparation method of chemical surface modification easily-dyed polyimide fabric

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张欣: "聚酰亚胺表面化学改性的红外光谱研究", 《河北工业科技》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106930117A (en) * 2017-04-14 2017-07-07 江南大学 A kind of cationic dyeing method of polyimide fiber
CN110468582A (en) * 2019-08-19 2019-11-19 江苏工程职业技术学院 A kind of polyimide nonwoven fabric from color changing method

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Application publication date: 20160525