CN106333569B - A kind of polyimides Rachael blanket and its non-aqueous solvent dyeing method - Google Patents

A kind of polyimides Rachael blanket and its non-aqueous solvent dyeing method Download PDF

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CN106333569B
CN106333569B CN201610704765.2A CN201610704765A CN106333569B CN 106333569 B CN106333569 B CN 106333569B CN 201610704765 A CN201610704765 A CN 201610704765A CN 106333569 B CN106333569 B CN 106333569B
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polyimides
rachael blanket
dyeing
reactive dye
modified
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CN106333569A (en
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毛森贤
陈玉霜
刘荣道
毛青山
陈金霞
吴明贤
俞宏斌
韩彬
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Zhejiang Truelove Blanket Industry Technology Co Ltd
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Zhejiang Truelove Blanket Industry Technology Co Ltd
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    • A—HUMAN NECESSITIES
    • A47—FURNITURE; DOMESTIC ARTICLES OR APPLIANCES; COFFEE MILLS; SPICE MILLS; SUCTION CLEANERS IN GENERAL
    • A47G—HOUSEHOLD OR TABLE EQUIPMENT
    • A47G9/00—Bed-covers; Counterpanes; Travelling rugs; Sleeping rugs; Sleeping bags; Pillows
    • A47G9/02—Bed linen; Blankets; Counterpanes
    • A47G9/0207—Blankets; Duvets
    • A47G9/0223—Blankets
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • 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
    • D06P1/0032—Determining dye recipes and dyeing parameters; Colour matching or monitoring
    • 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
    • D06P1/38—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 reactive dyes
    • 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
    • D06P1/90—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 dyes dissolved in organic solvents or aqueous emulsions thereof
    • D06P1/92—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 dyes dissolved in organic solvents or aqueous emulsions thereof in organic solvents
    • D06P1/928—Solvents other than hydrocarbons
    • 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
    • D06P3/008—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated using reactive dyes
    • 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
    • D06P3/82—Textiles which contain different kinds of fibres
    • D06P3/8204—Textiles which contain different kinds of fibres fibres of different chemical nature
    • D06P3/8295—Textiles which contain different kinds of fibres fibres of different chemical nature mixtures of fibres containing nitrile and ester groups
    • 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
    • D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
    • 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
    • D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
    • D06P5/002—Locally enhancing dye affinity of a textile material by chemical means
    • 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
    • D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
    • D06P5/20—Physical treatments affecting dyeing, e.g. ultrasonic or electric
    • 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
    • D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
    • D06P5/22—Effecting variation of dye affinity on textile material by chemical means that react with the fibre

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Coloring (AREA)

Abstract

The invention discloses a kind of polyimides Rachael blanket and its non-aqueous solvent dyeing method, the polyimides Rachael blanket is using 20%~60% polyimide fiber and 40%~80% acrylic fiber mixed yarn as suede yarn, make and form using 100% dacron thread as bottom silk weaving, its non-aqueous solvent dyeing includes following steps：(1) preparation of modifying agent suspension system；(2) water retting；(3) modification；(4) alkali steeping；(5) preparation of reactive dye emulsion；(6) dyeing of polyimides Rachael blanket；(7) recovery of modified waste liquid and dyeing waste liquid.The present invention introduces amino, imino group and hydroxyl by structurally-modified, provides dye seat for the dyeing of reactive dye, realizes dyeing of the reactive dye on polyimides Rachael blanket, in addition, modified and dyeing devil liquor recovery is convenient, advantageously reduces discharge of wastewater, realizes green dyeing.

Description

A kind of polyimides Rachael blanket and its non-aqueous solvent dyeing method
Technical field
The invention belongs to dope dyeing technical field, more particularly, to a kind of polyimides Rachael blanket and its non-aqueous Agent colouring method.
Background technology
Feature woollen blanket is an importance of woollen blanket industry technology development.Polyimides is combination property having most preferably One of machine high polymer material, high temperature resistant is up to more than 400 DEG C, and it is -200~300 DEG C that temperature range, which is used for a long time, better by its Dielectric properties, fire resistance, mechanical property and radiation resistance it is had a wide range of applications in industry-by-industry.With poly- Acid imide has the power of extraordinary feel, thermal property, fire resistance and brilliance for the woven Rachael blanket of raw material Learn performance.But for dyeing, polyimide material also has natural deficiency, and macromolecular arranged regular, fibre structure are tight Close, glass transition temperature is up to more than 350 DEG C, lack on molecular structure can reactive group, and polyimide material has Natural yellow, dyeing difficulty is very big.In general for lack on molecular structure can more than the material of reactive group using point Scattered dyestuff is dyed, and also common demands are higher than the glass transition temperature of material to dyeing temperature.Conventional disperse dyestuff HTHP Dyeing, its dyeing temperature is 120~130 DEG C, well below the glass transition temperature of polyimide fiber, in the dyeing temperature Lower disperse dyes molecule is hardly entered inside polyimide fiber.
The problem of being difficult to dyeing for polyimide fiber, existing patent is disclosed.Patent CN105133378A discloses one kind Polyimide fiber product disperse dyeing dyeing accelerant, being swelled for polyimide fiber, increase point are promoted using dyeing accelerant Dissipate the dye-uptake of dyestuff；Patent CN105603719A discloses the preparation method that chemical reduction method easily contaminates polyimides fabric, proposes Polyimides fabric is subjected to molten alkaline reduction solution processing first, then carries out the dyeing of disperse dyes；CN103541214A is public The method for improving polyimide fiber basic dyeing performance is opened, is proposed in the presence of catalyst, to polyimides Fiber carries out carboxylated modification, then addition carrier is dyed to the polyimide fiber of carboxylated in basic-dyeable fibre dye bath, Upper dye of the basic-dyeable fibre to polyimide fiber is realized by the effect of ionic bond.All multi-methods are real all on certain procedures above Show the coloring to polyimide fiber and product, but still it is noted that the glass transition temperature of polyimide material is remote Higher than dyeing temperature and the great hydrophobicity of polyimide molecule, polyimides can only be made using hydrophilic dyeing accelerant or carrier Outer layer is swelled so that the dyeing of disperse dyes often occurs over just the top layer of fiber, this namely a kind of dyeing it is " white Core " phenomenon, the utilization rate of disperse dyes is relatively low.Utilize reducing process（Use sodium dithionite, sodium dithionate or vulcanization Sodium）Polyimide fiber is handled, this can produce larger structure to polyimide fiber and destroy, and make mechanical property significantly Degree declines.In addition, carrying out carboxylated modification to polyimide fiber, come by the ionic bond formed between dyestuff and fibrous material Contaminated in realization, its dyefastness is also not ideal enough.In addition, using water as solvent, be not only unfavorable for polyimide fiber be swelled with Beneficial to the dyeing of fiber, it is modified complicated in waste water or dyeing waste-water, and intractability is also larger, and it, which is directly discharged, also will Produce larger environmental pollution.
The content of the invention
To overcome existing polyimide fiber dyeing difficult, the problem of Color is undesirable, the present invention provides a kind of poly- Acid imide Rachael blanket and its non-aqueous solvent dyeing method, can both overcome polyimide fiber dyeing difficult, Color Undesirable the problem of, dyeing of the reactive dye on polyimide fiber is realized, the utilization of reactive dye can also be greatly improved Rate, particularly nonaqueous solvents reclaim convenient, and this advantageously reduces discharge of wastewater, realize green dyeing.
The present invention is realized by following technology：
A kind of polyimides Rachael blanket includes following percentage by weight fiber：
Bottom silk：Dacron thread 100%,
Suede yarn：Polyimide fiber 20%~60%, acrylic fiber 40%~80%.
Preferably, described polyimides Rachael blanket is using polyimide fiber and acrylic fiber mixed yarn as suede Yarn, using dacron thread the bottom of as, silk is weaved on double-needle bed raschel tricot machine forms.
Polyimide fiber possesses good spinnability, and the textile that all kinds of special occasions are used can be made.Due to tool There are high-low temperature resistant characteristic, anti-flammability, not molten drop, from fiery self-extinguishment and splendid heat-insulated character.Polyimides fabric skin adaptability It is good, permanent fire retardant, and also dimensionally stable, security are good, service life is long, are compared with other fibers, the heat conduction system of material in itself Number is low, is also excellent temperature insulating material.However, the polyimide fiber market price is higher, carried out using pure polyimide fiber The weaving cost of Rachael blanket is higher, it is difficult to adapt to market needs.The present invention is fine by using polyimide fiber and acrylic fibers Mixed yarn is tieed up, can reach reduces the purpose of cost.Moreover, the mixed yarn can also improve polyimides Rachael blanket Lint sense, keep the original performance of the woollen blanket on the basis of, the thermal property of woollen blanket is further enhanced.
Preferably, the polyimides Rachael blanket non-aqueous solvent dyeing comprises the following steps：
（1）The preparation of modifying agent suspension system：Mixed base, structural modification agent, emulsifying agent are added in nonaqueous solvents, It is dispersed under ultrasonic assistant, form modifying agent suspension system；
（2）Water retting：Polyimides Rachael blanket is immersed in the water, dipping is finished, dried, the polyamides after drying The moisture content of imines Rachael blanket is 50%~70%；By the dipping of 5~10 minutes, in the table of polyimides Rachael blanket A certain amount of water is adsorbed in face, in this, as mixed base, the solvent of structural modification agent, realizes that mixed base, structural modification agent are sub- to acyl The modification of amine Rachael blanket structure；
（3）Modification：By step（2）In gained polyimides Rachael blanket immersion nonaqueous solvents, at 40~80 DEG C Under the conditions of, pre-swollen is handled 2~8 hours, then using bath raio as 1：30~50 immersion steps（1）Gained modifying agent suspension system In, processing is modified under the auxiliary of ultrasonic wave, modification temperature is 40~80 DEG C, and modification time is 1~3 hour, has been modified Finish, wash and be dried to obtain modified polyimide Rachael blanket；
（4）Alkali steeping：By step（3）In gained modified polyimide Rachael blanket immersion sodium carbonate liquor, during dipping Between be 10~30 minutes, dipping is finished, roll compacting, the modified polyimide Rachael blanket moisture content after roll compacting be 50%~ 80%；
（5）The preparation of reactive dye emulsion：Prepare 1~10g/L reactive dye solution and with volume ratio 1：100~200 Mixed with nonaqueous solvents, reactive dye solution is dispersed in nonaqueous solvents under ultrasonic assistant, form reactive dye breast Shape liquid；
（6）Dyeing：Take step（4）Gained modified polyimide Rachael blanket is with bath raio 1 after roll compacting：30~50 immersion steps Suddenly（5）Dyed in gained reactive dye emulsion, dyeing temperature is 40~80 DEG C, dyeing time is 1~2 hour, and dye finishes, Take out, wash and be drying to obtain dyeing polyimides Rachael blanket；
（7）The recovery of modified waste liquid and dyeing waste liquid：Collection step（3）And step（6）Gained is modified waste liquid and dyeing is useless Liquid, stands 24~48 hours, standing is finished, in the modified waste liquid, and mixed base and structural modification agent are precipitated to the bottom of container, Emulsifying agent is layered with nonaqueous solvents, is recovered by filtration and is obtained mixed base, then divides liquid recovery to obtain emulsifying agent and nonaqueous solvents, the dye In color waste liquid, reactive dye solution is layered with nonaqueous solvents, and point liquid reclaims and obtains reactive dye solution and and nonaqueous solvents.
In this manual, step（1）The middle emulsifying agent used, which can be played, improves modifying agent suspension system stability Effect, makes to keep the stabilization of 3~5 hours through the dispersed modifying agent suspension system of ultrasonic wave.Polyimide fiber molecule pole Has hydrophobicity, using step（3）The described nonaqueous solvents with apolar character plays a part of being swelled to it, makes fiber knot The regularity of structure has declined with compactness, the mesh for being modified and dyeing to polyimide fiber in favor of mixed base and reactive dye 's.Step（3）Can enter the polyimide fiber structural regularity after being swelled, compactness using the booster action of ultrasonic wave One step declines, and mixed base and the uniform simultaneously quick adsorption of structural modification agent should be able to be promoted extremely using the cavitation and thermal effect of ultrasonic wave Polyimides and acrylic fiber surface, and be dissolved in faster speed in the absorption water of the fiber surface.Come from molecular structure See, the group that can be reacted with reactive dye is all lacked on polyimide fiber and acrylic fiber molecular structure, reactive dye are utilized Carry out the no practical significance of dyeing.It is that of the invention one is important to realize dyeing of the reactive dye to polyimides Rachael blanket Content.For from principle, mixed base has the effect of hydrolysis to the molecular structure of imide bond, promotes polyimide molecule knot Generate amino and imino group on structure, structural modification agent under the initiation of mixed base by the reaction with cyano group acrylic fibers molecule knot Amino and hydroxyl are introduced on structure, this polyimides and acrylic fibers for causing after modified all possess the dye with reactive dye dyestuff Seat, the dyeing for reactive dye in polyimides Rachael blanket provides precondition.Step（4）It is middle by modified polyimide Rachael blanket immersion sodium carbonate liquor makes the carpeted surface adsorb sodium carbonate liquor, during dyeing, and reactive dye will In the sodium carbonate liquor that polyimides Rachael blanket surface is transferred to from nonaqueous solvents, the activity with basic character is formed Dye solution.Dyeing course be bath raio be 1：1~4 tinge in bath is carried out, relative to the bath raio of common dyeing（1：30~ 100）, the bath raio substantially increases dye-uptake of the reactive dye to polyimides Rachael blanket.In the present invention, reactive dye pair The dye-uptake of polyimides Rachael blanket reaches more than 80%.
A kind of polyimides Rachael blanket disclosed by the invention and its non-aqueous solvent dyeing method, in nonaqueous solvents, Amino and hydroxyl are introduced by structurally-modified introduced in polyimide fiber on amino and imino group, the molecular structure of acrylic fibers, In this, as the dye seat of reactive dye, and finally realize dyeing of the reactive dye to polyimides Rachael blanket, activity dye Material is connected by covalent bond with polyimides Rachael blanket, with preferable dyefastness.
Preferably, the nonaqueous solvents be petroleum ether, toluene, dimethylbenzene, thiacyclohexane, the siloxanes of ten dimethyl of straight chain five, One or more in prestox D5, decamethylcyclopentaandoxane, the siloxanes of ten pregnancy basic ring six.Using hydrophobicity Strong nonaqueous solvents is conducive to being swelled for polyimide fiber, and the dyeing of modification and reactive dye for polyimide fiber is provided Condition.
Preferably, the emulsifying agent is glycerin monostearate, distearin, Sucrose acetoisobutyrate, mountain Pears alcohol acid anhydride aliphatic acid, methyl glycol fatty acid ester, secondary octyl phenol polyethenoxy ether, diglycerol polypropylene glycol ether, polyoxyethylene One or more in sugar alcohol acid anhydride monostearate, the consumption of emulsifying agent is the 0.2%~1% of nonaqueous solvents cumulative volume.
Preferably, the power of the ultrasonic wave is 250~500W, and rated frequency is 40KHz or 50KHz, and the time 1~3 is small When.
Preferably, described mixed base is a kind of and sodium acid carbonate, sodium carbonate, the phosphoric acid in sodium hydroxide and potassium hydroxide One kind in sodium and potassium carbonate is mixed to get with phase homogenous quantities, and the consumption of the mixed base is the modifying agent suspension system The 0.5%~2% of gross mass.The modification of polyimide fiber is conducive to using mixed base to keep polyimides Rachael blanket sheet The intrinsic mechanical performance of body, also can cause agent as structural modification agent to what the molecular structure of acrylic fibers was modified.
Preferably, the structural modification agent is the one or two of hydroxylamine chloride and hydroxylamine hydrochloride, the structural modification agent Consumption be the modifying agent suspension system gross mass 1%~3%.
Preferably, the washing is originally water washing, and the consumption of detergent is polyimides Rachael blanket gross weight 1%~3%, wash time is 30~60 minutes, and the detergent is neutral detergent.Be conducive to being adsorbed to using neutral detergent The elution of nonaqueous solvents in polyimides Rachael blanket.
Preferably, the concentration of the sodium carbonate liquor is 1~5g/L.Sodium carbonate is in reactive dye to polyimides La Sheer The effect of fixation is served in the dyeing course of woollen blanket, is made in the active group and polyimides Rachael blanket of reactive dye Amino or imino group reaction, form covalent bond.
The beneficial effects of the present invention are：（1）Realized using nonaqueous solvents and ultrasonic wave to hard-packed polyamides Being swelled for imines, greatly improves the structurally-modified effect of polyimides；（2）Using modified in polyimide fiber, acrylic fibers fibre Amino, imino group and hydroxyl are introduced in dimension, upper dye of the reactive dye in polyimides Rachael blanket is realized；（3）Non-aqueous The use of agent improves the dye-uptake and dye utilization rate of reactive dye, and the recovery process of modified waste water and dyeing waste-water is simple, It is easy to operate.
Embodiment
With reference to specific embodiment, to a kind of polyimides Rachael blanket and its non-aqueous described in the present patent application Agent colouring method.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this hair It is bright.
Embodiment 1
To 1Kg polyimides Rachael blankets（Bottom silk is 100% dacron thread, and suede yarn is containing 30% polyimide fiber and 70% The mixed yarn of acrylic fiber, fabric weight is 300g/m2）Mixing alkali modification and reactive brilliant red x-3b are carried out under nonaqueous solvents （It is commercially available）Dyeing.
Weigh 150g sodium hydroxides, 150g sodium carbonate, 150g hydroxylamine chlorides and 90mL glycerin monostearates and pour into 30L Mixed liquor is obtained in decamethylcyclopentaandoxane, supersonic generator is opened（Power 300W, rated frequency 40KHz）To the mixing Liquid carries out ultrasonication, and ultrasonic time is 1 hour, and modifying agent suspension system is made.Weigh 1Kg polyimides Rachael blankets It is immersed in the water, room temperature, dip time is 10 minutes, and dipping is finished, dries, the polyimides Rachael blanket after drying contains Water rate is 50%.Polyimides Rachael blanket after immersion is directly immersed in 60 DEG C of decamethylcyclopentaandoxane and carried out in advance Swelling treatment 6 hours, pre-swollen is finished, and takes the polyimides Rachael blanket with bath raio 1：The prepared modifying agent of 30 immersions hangs Floating body system is modified, and supersonic generator is opened while immersion（Power 500W, rated frequency 50KHz）Modification liquid is carried out Ultrasonic assistant, modification temperature is controlled at 60 DEG C, after being modified 2 hours, is taken out modified polyimides Rachael blanket, is put into Household automatic washing machine is washed, and adds 10g neutral detergents, and wash time is 30 minutes.Washing is finished, and is dried modified poly- After acid imide Rachael blanket and immerse in 2g/L sodium carbonate liquors, room temperature, dipping is after 30 minutes, using padding machine to modified polyamides Imines Rachael blanket carries out roll compacting, sodium carbonate is penetrated into the fibrous inside of polyimides Rachael blanket, changing after roll compacting Property polyimides Rachael blanket moisture control is 60%.Prepare 5g/L reactive brilliant red x-3b solution 300mL and add 30L ten Mixed liquor is obtained in methyl D5, supersonic generator is opened（Power 300W, rated frequency 40KHz）To the mixed liquor Ultrasonication is carried out, ultrasonic time is 60 minutes, and reactive dye emulsion is made.Learn from else's experience the modification after roll compacting sodium carbonate liquor Polyimides Rachael blanket is with bath raio 1：Dyed in the obtained reactive dye emulsion of 30 immersions, dyeing temperature is 40 DEG C, dyeing time is 1 hour, and dye finishes, and takes out the polyimides Rachael blanket contaminated and is put into household automatic washing machine progress Washing, adds 20g neutral detergents, and wash time is that can wash away the loose colour on polyimides Rachael blanket surface in 45 minutes, Washing is finished, and is drying to obtain red polyimides Rachael blanket.
Modified waste liquid and dyeing waste liquid are collected respectively, are stored at room temperature 24 hours, standing is finished, in modified waste liquid, hydroxide Sodium, sodium carbonate and hydroxylamine chloride solid powder are precipitated to the bottom of container, glycerin monostearate and decamethylcyclopentaandoxane Substantially layering is produced, sodium hydroxide, sodium carbonate and hydroxylamine chloride solid mixed-powder is filtrated to get, then obtain by a point liquid recovery Glycerin monostearate and decamethylcyclopentaandoxane；Dye in waste liquid, reactive brilliant red x-3b solution and the silica of decamethyl ring five Alkane is layered, and is reclaimed by point liquid and is obtained reactive brilliant red x-3b solution and decamethylcyclopentaandoxane.Reclaim obtained various reagents It can be reused with solution.
Test modified fabricK/SValue and reactive brilliant red x-3b dyed fabricK/SValue, soaping fastness and friction jail Degree, as a result as shown in table 1.
Embodiment 2
To 1Kg polyimides Rachael blankets（Bottom silk is 100% dacron thread, and suede yarn is containing 50% polyimide fiber and 50% The mixed yarn of acrylic fiber, fabric weight is 250g/m2）Mixing alkali modification and Reactive dye red M-3BE are carried out under nonaqueous solvents （It is commercially available）Dyeing.
300g potassium hydroxide, 300g potassium carbonate, 300g hydroxylamine hydrochlorides and 150mL distearins is weighed to pour into Mixed liquor is obtained in the siloxanes of ten dimethyl of 40L straight chains five, supersonic generator is opened（Power 400W, rated frequency 50KHz） Ultrasonication is carried out to the mixed liquor, ultrasonic time is 1.5 hours, and modifying agent suspension system is made.Weigh 1Kg polyimides Rachael blanket is immersed in the water, room temperature, and dip time is 5 minutes, and dipping is finished, and is dried, and the polyimides after drying is drawn She Er woollen blankets moisture content is 70%.Polyimides Rachael blanket after immersion is directly immersed in 80 DEG C of the silica of ten dimethyl five Carry out pre-swollen in alkane to handle 8 hours, pre-swollen is finished, and takes the polyimides Rachael blanket with bath raio 1：40 immersions are prepared Modifying agent suspension system be modified, supersonic generator is opened while immersion（Power 400W, rated frequency 40KHz）It is right Modification liquid carries out ultrasonic assistant, and modification temperature is controlled at 80 DEG C, after being modified 3 hours, takes out modified polyimides and draws house That woollen blanket, is put into household automatic washing machine and is washed, and adds 20g neutral detergents, and wash time is 60 minutes.Wash Finish, dry after modified polyimide Rachael blanket and immerse in 3g/L sodium carbonate liquors, room temperature, dipping is used after 10 minutes Padding machine carries out roll compacting to modified polyimide Rachael blanket, sodium carbonate is penetrated into the fiber of polyimides Rachael blanket Portion, the modified polyimide Rachael blanket moisture control after roll compacting is 50%.Prepare 3g/L Reactive dye red M-3BE solution 250mL And add mixed liquor is obtained in 50L decamethylcyclopentaandoxanes, open supersonic generator（Power 500W, rated frequency 50KHz）Ultrasonication is carried out to the mixed liquor, ultrasonic time is 90 minutes, and reactive dye emulsion is made.Learn from else's experience roll compacting carbon Modified polyimide Rachael blanket after acid sodium solution is with bath raio 1：Carried out in the obtained reactive dye emulsion of 50 immersions Dyeing, dyeing temperature is 60 DEG C, and dyeing time is 2 hours, and dye finishes, and takes out the polyimides Rachael blanket contaminated and is put into family expenses Automatic washing machine is washed, and adds 30g neutral detergents, and wash time is that can wash away polyimides La Sheermao in 60 minutes The loose colour on blanket surface, washing is finished, and is drying to obtain deep red polyimides Rachael blanket.
Modified waste liquid and dyeing waste liquid are collected respectively, are stored at room temperature 48 hours, standing is finished, in modified waste liquid, hydroxide Potassium, potassium carbonate and hydroxylamine hydrochloride solid powder are precipitated to the bottom of container, distearin and the siloxanes of ten dimethyl five Substantially layering is produced, potassium hydroxide, potassium carbonate and hydroxylamine hydrochloride solid mixed-powder is filtrated to get, then obtain by a point liquid recovery Distearin and the siloxanes of ten dimethyl five；Dye in waste liquid, Reactive dye red M-3BE solution and the siloxanes of ten dimethyl five Layering, is reclaimed by point liquid and obtains Reactive dye red M-3BE solution and the siloxanes of ten dimethyl five.Reclaim obtained various reagents and molten Liquid can be reused.
Test modified fabricK/SValue and Reactive dye red M-3BE dyed fabricK/SValue, soaping fastness and crock fastness, As a result as shown in table 1.
Comparative example 1
To 1Kg polyimides Rachael blankets（Bottom silk is 100% dacron thread, and suede yarn is containing 30% polyimide fiber and 70% The mixed yarn of acrylic fiber, fabric weight is 300g/m2）Reactive brilliant red x-3b is carried out under nonaqueous solvents（It is commercially available）Dyeing.
Reactive brilliant red x-3b dyeing is carried out to polyimides Rachael blanket with reference in the colouring method implemented in row 1.
Blanket fabric before test dyeK/SValue and reactive brilliant red x-3b dyed fabricK/SValue, soaping fastness and friction Fastness, as a result as shown in table 1.
Comparative example 2
To 1Kg polyimides Rachael blankets（Bottom silk is 100% dacron thread, and suede yarn is containing 50% polyimide fiber and 50% The mixed yarn of acrylic fiber, fabric weight is 250g/m2）Reactive dye red M-3BE is carried out under nonaqueous solvents（It is commercially available）Dyeing.
Reactive dye red M-3BE dyeing is carried out to polyimides Rachael blanket with reference to the colouring method implemented in row 2.
Blanket fabric before test dyeK/SValue and Reactive dye red M-3BE dyed fabricK/SValue, soaping fastness and friction jail Degree, as a result as shown in table 1.
Table 1 before modified after polyimides Rachael blanketK/SIt is worth and dyes woollen blanketK/SValue and color fastness
As can be seen from Table 1, polyimides Rachael blanket has the color of certain depth in itself, if drawing polyimides She Er woollen blankets are directly dyed, and its dye level slightly has raising, and its reason is that dyestuff passes through physical absorption or Hydrogen Binding Adsorption To the surface of the woollen blanket, make to contaminate on reactive dye to polyimides Rachael blanket with physical absorption or hydrogen bond, its adhesion It is very weak, therefore dyed fabric color fastness is very low, and less than 3 grades, actual use needs can not be met completely.After modified, exist In two embodiments, the color depth of polyimides Rachael blanket has declined, and its reason is in the presence of mixed base Acylimino on the backbone structure of polyimides have issued hydrolysis, the conjugated system of polyimide molecule is received destruction, So that the color depth of blanket fabric has declined, it on the other hand also illustrate that mixed base to polyimide modified effective Property.The coloration result of modified polyimide Rachael blanket is shown using reactive brilliant red x-3b, Reactive dye red M-3BE, fabricK/ SValue, dyefastness are greatly improved, and dyefastness reaches more than 4.5 grades, and higher fastness is because reactive dye It is, by covalent bond structure, to form firm relation with modified polyimide, and it is higherK/SValue is due to changing for mixed base Property provide substantial amounts of dye seat for reactive dye, on reactive dye contaminate polyimides Rachael blanket provide condition.

Claims (9)

1. a kind of polyimides Rachael blanket, it is characterized in that, the polyimides Rachael blanket includes following weight percent Compare fiber：
Bottom silk：Dacron thread 100%,
Suede yarn：Polyimide fiber 20%~60%, acrylic fiber 40%~80%；
The polyimides Rachael blanket non-aqueous solvent dyeing comprises the following steps：
（1）The preparation of modifying agent suspension system：Mixed base, structural modification agent, emulsifying agent are added in nonaqueous solvents, in ultrasound It is dispersed under ripple auxiliary, form modifying agent suspension system；
（2）Water retting：Polyimides Rachael blanket is immersed in the water, dipping is finished, dried, the polyimides after drying The moisture content of Rachael blanket is 50%~70%；
（3）Modification：By step（2）In gained polyimides Rachael blanket immersion nonaqueous solvents, in 40~80 DEG C of conditions Under, pre-swollen is handled 2~8 hours, then using bath raio as 1：30~50 immersion steps（1）In gained modifying agent suspension system, Processing is modified under the auxiliary of ultrasonic wave, modification temperature is 40~80 DEG C, and modification time is 1~3 hour, and modification is finished, and is washed Wash and be dried to obtain modified polyimide Rachael blanket；
（4）Alkali steeping：By step（3）In gained modified polyimide Rachael blanket immersion sodium carbonate liquor, dip time is 10~30 minutes, dipping was finished, roll compacting, and the modified polyimide Rachael blanket moisture content after roll compacting is 50%~80%；
（5）The preparation of reactive dye emulsion：Prepare 1~10g/L reactive dye solution and with volume ratio 1：100~200 with it is non- Aqueous solvent is mixed, and reactive dye solution is dispersed in nonaqueous solvents under ultrasonic assistant, forms reactive dye emulsion；
（6）Dyeing：Take step（4）Gained modified polyimide Rachael blanket is with bath raio 1 after roll compacting：30~50 immersion steps （5）Dyed in gained reactive dye emulsion, dyeing temperature is 40~80 DEG C, dyeing time is 1~2 hour, and dye finishes, and takes Go out, wash and be drying to obtain dyeing polyimides Rachael blanket；
（7）The recovery of modified waste liquid and dyeing waste liquid：Collection step（3）And step（6）Gained is modified waste liquid and dyeing waste liquid, quiet Put 24~48 hours, standing is finished, in the modified waste liquid, mixed base and structural modification agent are precipitated to the bottom of container, emulsification Agent is layered with nonaqueous solvents, is recovered by filtration and is obtained mixed base, then divides liquid recovery to obtain emulsifying agent and nonaqueous solvents, and the dyeing is given up In liquid, reactive dye solution is layered with nonaqueous solvents, and point liquid reclaims and obtains reactive dye solution and and nonaqueous solvents.
2. a kind of polyimides Rachael blanket according to claim 1, it is characterized in that, described polyimides La Sheer Woollen blanket is that, using polyimide fiber and acrylic fiber mixed yarn as suede yarn, the bottom of by of dacron thread, silk is in double-needle bed raschel tricot machine Upper weaving is formed.
3. a kind of polyimides Rachael blanket according to claim 1, it is characterized in that, the nonaqueous solvents is oil Ether, toluene, dimethylbenzene, thiacyclohexane, the siloxanes of ten dimethyl of straight chain five, prestox D5, decamethylcyclopentaandoxane, One or more in the siloxanes of ten pregnancy basic ring six.
4. a kind of polyimides Rachael blanket according to claim 1, it is characterized in that, the emulsifying agent is monostearate Glyceride, distearin, Sucrose acetoisobutyrate, sorbitan fatty acid, methyl glycol fatty acid ester, secondary octyl phenol One or more in APEO, diglycerol polypropylene glycol ether, polyoxyethylene sorbitan monostearate, emulsifying agent Consumption be nonaqueous solvents cumulative volume 0.2%~1%.
5. a kind of polyimides Rachael blanket according to claim 1, it is characterized in that, the power of the ultrasonic wave is 250~500W, rated frequency is 40KHz or 50KHz, 1~3 hour time.
6. a kind of polyimides Rachael blanket according to claim 1, it is characterized in that, described mixed base is hydroxide One kind in a kind of and sodium acid carbonate, sodium carbonate, sodium phosphate and potassium carbonate in sodium and potassium hydroxide is mixed with phase homogenous quantities Conjunction is obtained, and the consumption of the mixed base is the 0.5%~2% of the modifying agent suspension system gross mass.
7. a kind of polyimides Rachael blanket according to claim 1, it is characterized in that, the structural modification agent is chlorination The one or two of azanol and hydroxylamine hydrochloride, the consumption of the structural modification agent is the 1% of the modifying agent suspension system gross mass ~3%.
8. a kind of polyimides Rachael blanket according to claim 1, it is characterized in that, the washing is originally to wash Wash, the consumption of detergent is the 1%~3% of polyimides Rachael blanket gross weight, wash time is 30~60 minutes, described to wash Agent is washed for neutral detergent.
9. a kind of polyimides Rachael blanket according to claim 1, it is characterized in that, the concentration of the sodium carbonate liquor For 1~5g/L.
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CN105002647A (en) * 2015-06-16 2015-10-28 长兴虹波纺织有限公司 Production process for Raschel blanket
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