CN104910566B - A kind of preparation method of polymer masterbatch and fiber with moisture absorption coloring function - Google Patents
A kind of preparation method of polymer masterbatch and fiber with moisture absorption coloring function Download PDFInfo
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- CN104910566B CN104910566B CN201510299169.6A CN201510299169A CN104910566B CN 104910566 B CN104910566 B CN 104910566B CN 201510299169 A CN201510299169 A CN 201510299169A CN 104910566 B CN104910566 B CN 104910566B
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- moisture absorption
- coloring function
- absorption coloring
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Abstract
The invention provides a kind of polymer masterbatch with moisture absorption coloring function and the preparation method of fiber.The preparation method of the described polymer masterbatch with moisture absorption coloring function, it is characterised in that including:Step 1:Porous nano powder, Triallyl isocyanurate, polyethyleneglycol diacrylate, polyalkylene glycol acrylate monomethyl ether ester, initiator, wet sensitive colour changing powder and discoloration sensitizer are placed in aqueous solvent, using the scattered method of depressurizing ultrasonic, reacted at 70 80 DEG C 2~5 hours, most obtain the composite functional material with moisture absorption coloring function after centrifugal dehydration afterwards;Step 2:By the above-mentioned composite functional material with moisture absorption coloring function through dried process after, with polymer chips through twin-screw be blended granulate, obtain with moisture absorption coloring function polymer masterbatch.Moisture absorption coloring function material of the invention with similar microcapsule structure, there is heat-resist, stable performance, and preparation process is simple, with low cost.
Description
Technical field
The invention belongs to the preparation field of coloring function fiber, more particularly to a kind of polymer with moisture absorption coloring function
The preparation method of master batch and its fiber.
Background technology
After chameleon fibre generally refers to be subject to the external conditions such as light, thermal and magnetic, electricity or moisture, can actively change itself
The functional fibre of color.At present, what report was more mainly has photoinduction and the major class product of temperature-induced chameleon fibre two.For inhaling
Polymer and the fiber report of wet induced discoloration fiber are less, and using the method for surface post processing more than its preparation process.Country
The B of patent of invention CN 101962913 disclose a kind of reversible electrochromic composite fibre and preparation method thereof, that is, employ table
The method of face coating.The B of national inventing patent CN 102304857 report a kind of chameleon fibre fabric based on graft polymerization method
Processing technology, then using Final finishing chemical surface grafting and coating color changing media.But either coated on surface, or come to the surface
Process, and is likely to the poisonous intermediate monomer of residual or heavy metal ion, and there is a problem of the degree of enduring hardships of coat.
Regarding to the issue above, it is carrier that the present invention uses porous nano powder, to wet sensitive colour changing agent under ultrasonic reduced pressure
Dispensed, used polyalkylene glycol acrylate monomethyl ether ester to lead wet chain, discoloration sensitizer is strengthened colour developing effect, be prepared for having
The polymer masterbatch and fiber with moisture absorption coloring function of high thermal stability.For the functionalization for realizing general fiber provides think of
Road.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of polymer masterbatch and its fibre with moisture absorption coloring function
The preparation method of dimension, the method is packaged using porous nano powder to wet sensitive colour changing agent and its sensitizer, forms similar micro-
The structure of capsule, and the structure has more heat resistance;The polyalkylene glycol acrylate monomethyl ether ester used in encapsulant has fine
Water imbibition, can promote for colour developing change support being provided.The polymer masterbatch of moisture absorption coloring function of the present invention can be with
Apply in the general fiber art such as polypropylene, polyvinyl alcohol, polyester, polyamide well.
In order to solve the above-mentioned technical problem, the invention provides a kind of system of the polymer masterbatch with moisture absorption coloring function
Preparation Method, it is characterised in that including:
Step 1:By porous nano powder, Triallyl isocyanurate, polyethyleneglycol diacrylate, the poly- second of acrylic acid
Glycol monomethyl ether ester, initiator, wet sensitive colour changing powder and discoloration sensitizer are placed in aqueous solvent, using the scattered side of depressurizing ultrasonic
Method, reacts 2~5 hours at 70-80 DEG C, most obtains the complex function material with moisture absorption coloring function after centrifugal dehydration afterwards
Material;
Step 2:By the above-mentioned composite functional material with moisture absorption coloring function through dried process after, with polymer chips
It is blended through twin-screw and is granulated, obtains the polymer masterbatch with moisture absorption coloring function.
Preferably, in described step 1 porous nano powder, Triallyl isocyanurate, the propylene of polyethylene glycol two
The ratio of acid esters, initiator, wet sensitive colour changing powder, discoloration sensitizer, polyalkylene glycol acrylate monomethyl ether ester and aqueous solvent is 20
~40: 4~8: 5~10: 0.1~1: 20~40: 5~10: 25.9~45.9: 200mL.
Preferably, described porous nano powder is in porous silica, multilayer montmorillonite, aeroge and diatomite
One or two are composited, and its particle diameter is 50~600nm.
Preferably, described polymer chips is one kind of polypropylene, polyvinyl alcohol, polyester and polyamide section.
Preferably, described initiator is azo-bis-isobutyrate hydrochloride or ammonium persulfate.
Preferably, described wet sensitive colour changing powder be cobalt chloride, the complex of hexamethylenetetramine, mass ratio be 50~
99: 1~50.
Preferably, described discoloration sensitizer is phosphoamide.
Preferably, the quality of described composite functional material and polymer chips with moisture absorption coloring function for 5: 95~
15∶85。
Present invention also offers a kind of preparation method of the polymer fiber with moisture absorption coloring function, it is characterised in that
Developed the color with moisture absorption including the polymer masterbatch of the above-mentioned polymer fiber with moisture absorption coloring function is obtained through melt spinning
The polymer fiber of function.
Compared with prior art, the beneficial effects of the invention are as follows:
(1) moisture absorption coloring function material of the invention with similar microcapsule structure, with heat-resist, stable performance
Advantage, it is and preparation process is simple, with low cost.
(2) moisture absorption coloring function material prepared by the present invention possesses conduit pipe, can help to functional agglomerate and fiber
Colour developing effect.
(3) moisture absorption coloring function fiber prepared by the present invention, prepares simple, degree of the enduring hardships problem without surface coating, and not
Poisonous intermediate monomer or heavy metal ion can be produced.
(4) the modified thinking of moisture absorption coloring function prepared by the present invention, can well be applied to polypropylene, polyvinyl alcohol, gather
The functional modification field of the general fiber such as urethane, polyester, polyamide, polyphenylene sulfide.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Polyethyleneglycol diacrylate described in various embodiments of the present invention is purchased from lark prestige Science and Technology Ltd., and its number is divided equally
Son amount is 250~750.
Polyalkylene glycol acrylate monomethyl ether ester described in various embodiments of the present invention is with reference to national inventing patent CN
102516471 B synthesize, and its number-average molecular weight is 1000~10000.
Embodiment 1
A kind of preparation method of the polymer masterbatch with moisture absorption coloring function, specially:
First, by the multilayer montmorillonite (particle diameter is about 600nm) of 20g, the Triallyl isocyanurate of 8g, 5g poly- second
(cobalt chloride accounts for cooperation for omega-diol diacrylate, the initiator ammonium persulfate of 1g, the cobalt chloride of 40g, hexamethylenetetramine complex
Amount of substance 80%), the discoloration sensitizer phosphoamide of 5g, the polyalkylene glycol acrylate monomethyl ether ester of 21g, be added to 200ml and go
In ionized water, using the scattered method of depressurizing ultrasonic (pressure 200Pa~500Pa, 20~40KHz of supersonic frequency), 75 are warming up to
DEG C reaction 5 hours.The powder body material of moisture absorption coloring function is obtained after centrifugal dehydration, it is standby through 80 DEG C of dryings 12 hours.
By the polyamide of the moisture absorption coloring function powder of the 15g of dried process and 85g through double screw extruder 240~260
DEG C blending granulation, obtains the polymer masterbatch with moisture absorption coloring function, and obtain moisture absorption coloring function through melt spinning machine
Fypro, wherein 260~280 DEG C of spinning temperature, spin 800~3500m/min of speed.Find after tested, the fiber of preparation can
Pink is changed into by purple in the case where humidity is more than 40% environment.
Embodiment 2
A kind of preparation method of the polymer masterbatch with moisture absorption coloring function, specially:First, by porous the two of 40g
Silica (particle diameter is about 50nm), the Triallyl isocyanurate of 4g, the polyethyleneglycol diacrylate of 10g, 0.1g draw
(cobalt chloride is accounted for and coordinates amount of substance for hair agent azo-bis-isobutyrate hydrochloride, the cobalt chloride of 20g, hexamethylenetetramine complex
90%), discoloration sensitizer phosphoamide, the polyalkylene glycol acrylate monomethyl ether ester of 15.9g of 10g, are added to 200ml deionized waters
In, using the scattered method of depressurizing ultrasonic (pressure 200Pa~500Pa, 20~40KHz of supersonic frequency), it is warming up to 75 DEG C of reactions 2
Hour.The powder body material of moisture absorption coloring function is obtained after centrifugal dehydration, it is standby through 80 DEG C of dryings 12 hours.By dried process
260~280 DEG C of blending granulations of the moisture absorption coloring function powder of 5g and the polyester double screw extruder of 95g, obtain aobvious with moisture absorption
The polymer masterbatch of color function, and the Fypro of moisture absorption coloring function, wherein spinning temperature 270 are obtained through melt spinning machine
~300 DEG C, spin 800~3500m/min of speed.Find after tested, find after tested, the fiber of preparation can be more than 50% ring in humidity
Pink is changed into by purple under border.
Embodiment 3
A kind of preparation method of the polymer masterbatch with moisture absorption coloring function, specially:
First, by the diatomite (particle diameter is about 600nm) of 30g, the Triallyl isocyanurate of 4g, 5g polyethylene glycol
Diacrylate, the initiator ammonium persulfate of 1g, the wet sensitive colour changing powder cobalt chloride of 30g, hexamethylenetetramine complex (chlorination
Cobalt account for coordinate amount of substance 95%), the discoloration sensitizer phosphoamide of 10g, the polyalkylene glycol acrylate monomethyl ether ester of 20g, add
To in 200ml deionized waters, using the scattered method of depressurizing ultrasonic (pressure 200Pa~500Pa, 20~40KHz of supersonic frequency),
75 DEG C are warming up to react 4 hours.The powder body material of moisture absorption coloring function is obtained after centrifugal dehydration, it is standby through 80 DEG C of dryings 12 hours
With.
By the polypropylene of the moisture absorption coloring function powder of the 10g of dried process and 90g through double screw extruder 180~200
DEG C blending granulation, obtains the polymer masterbatch with moisture absorption coloring function, and obtain moisture absorption coloring function through melt spinning machine
Fypro, wherein 200~230 DEG C of spinning temperature, spin 800~2500m/min of speed.Find after tested, find after tested, make
Standby fiber can be changed into pink in the case where humidity is more than 50% environment by purple.
Embodiment 4
A kind of preparation method of the polymer masterbatch with moisture absorption coloring function, specially:
First, by the multilayer montmorillonite (particle diameter is about 400nm) of 10g, the diatomite (particle diameter is about 400nm) of 10g, 5g
Triallyl isocyanurate, the polyethyleneglycol diacrylate of 5g, the initiator azo-bis-isobutyrate hydrochloride of 1g, 40g
Cobalt chloride, hexamethylenetetramine complex (cobalt chloride is accounted for and coordinates the 98% of amount of substance), the discoloration sensitizer phosphoamide of 5g, 24g
Polyalkylene glycol acrylate monomethyl ether ester, be added in 200ml deionized waters, using the scattered method (pressure of depressurizing ultrasonic
200Pa~500Pa, 20~40KHz of supersonic frequency), it is warming up to 75 DEG C and reacts 3 hours.Moisture absorption colour developing is obtained after centrifugal dehydration
The powder body material of function, it is standby through 80 DEG C of dryings 12 hours.
By the moisture absorption coloring function powder of the 10g of dried process and the polyvinyl alcohol (swelling treatment, containing 5%~10% of 90g
Solvent) through 95~105 DEG C of blending granulations of double screw extruder, the polymer masterbatch with moisture absorption coloring function is obtained, and through molten
Melt the Fypro that spinning-drawing machine obtains moisture absorption coloring function, wherein 100~115 DEG C of spinning temperature, 500~1500m/ of spinning speed
min。
Find after tested, the fiber of preparation can be changed into pink in the case where humidity is more than 40% environment by purple.
Claims (8)
1. a kind of preparation method of the polymer masterbatch with moisture absorption coloring function, it is characterised in that including:
Step 1:By porous nano powder, Triallyl isocyanurate, polyethyleneglycol diacrylate, polyalkylene glycol acrylate
Monomethyl ether ester, initiator, wet sensitive colour changing powder and discoloration sensitizer are placed in aqueous solvent, using the scattered method of depressurizing ultrasonic,
Reacted at 70-80 DEG C 2~5 hours, most obtain the composite functional material with moisture absorption coloring function after centrifugal dehydration afterwards;Institute
Porous nano powder, Triallyl isocyanurate, polyethyleneglycol diacrylate, initiator, wet sensitive in the step of stating 1 become
The ratio of toner body, discoloration sensitizer, polyalkylene glycol acrylate monomethyl ether ester and aqueous solvent is 20~40g: 4~8 g: 5~10
G: 0.1~1 g: 20~40 g: 5~10 g: 25.9~45.9 g: 200mL;
Step 2:By the above-mentioned composite functional material with moisture absorption coloring function through dried process after, with polymer chips through double
Screw extruder blending granulation, obtains the polymer masterbatch with moisture absorption coloring function.
2. there is the preparation method of the polymer masterbatch of moisture absorption coloring function as claimed in claim 1, it is characterised in that described
Porous nano powder be composited for one or two in porous silica, multilayer montmorillonite, aeroge and diatomite,
Its particle diameter is 50~600nm.
3. there is the preparation method of the polymer masterbatch of moisture absorption coloring function as claimed in claim 1, it is characterised in that described
Polymer chips for polypropylene, polyvinyl alcohol, polyester and polyamide section one kind.
4. there is the preparation method of the polymer masterbatch of moisture absorption coloring function as claimed in claim 1, it is characterised in that described
Initiator be ammonium persulfate or azo-bis-isobutyrate hydrochloride.
5. there is the preparation method of the polymer masterbatch of moisture absorption coloring function as claimed in claim 1, it is characterised in that described
Wet sensitive colour changing powder be cobalt chloride, the complex of hexamethylenetetramine, mass ratio be 50~99: 1~50.
6. there is the preparation method of the polymer masterbatch of moisture absorption coloring function as claimed in claim 1, it is characterised in that described
Discoloration sensitizer be phosphoamide.
7. there is the preparation method of the polymer masterbatch of moisture absorption coloring function as claimed in claim 1, it is characterised in that described
Composite functional material with moisture absorption coloring function and the quality of polymer chips be 5: 95~15: 85.
8. a kind of preparation method of the polymer fiber with moisture absorption coloring function, it is characterised in that including by claim 1-7
Any one of the polymer masterbatch with moisture absorption coloring function obtain poly- with moisture absorption coloring function through melt spinning
Compound fiber.
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CN106046244B (en) * | 2016-05-30 | 2018-07-24 | 广州海谷电子科技有限公司 | Non-electrolyte family macromolecule wet sensitive resin and preparation method thereof and the electrically conductive ink and moisture sensor prepared based on wet sensitive resin |
CN106381567B (en) * | 2016-08-31 | 2018-08-31 | 浙江省现代纺织工业研究院 | A kind of manufacturing method of liquid phase dyeable polypropylene fibre |
CN106835307A (en) * | 2016-11-25 | 2017-06-13 | 深圳中凝科技有限公司 | The preparation method that fused mass directly spinning adds airsetting glue fiber online |
CN108066163A (en) * | 2017-12-19 | 2018-05-25 | 东华大学 | It is a kind of using polyethyleneglycol diacrylate as sun-proof microcapsules of wall material and preparation method thereof |
CN108587140A (en) * | 2017-12-27 | 2018-09-28 | 重庆普利特新材料有限公司 | A kind of preparation method of the polyamides implant of antistatic, automatic colour developing colour change function |
CN108178903A (en) * | 2017-12-27 | 2018-06-19 | 重庆普利特新材料有限公司 | A kind of polyesters composite material of antistatic, automatic colour developing colour change function and preparation method thereof |
CN108178872A (en) * | 2017-12-27 | 2018-06-19 | 重庆普利特新材料有限公司 | A kind of PP composite material with antistatic, automatic colour developing colour change function and preparation method thereof |
CN111304773A (en) * | 2020-04-01 | 2020-06-19 | 百事基材料(青岛)股份有限公司 | Easy-to-dye modified polyamide fiber |
CN112964650B (en) * | 2021-02-05 | 2022-09-02 | 武汉纺织大学 | Fiber-based humidity sensor based on moisture absorption and color change and preparation method thereof |
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CN101962913B (en) * | 2009-07-22 | 2012-01-04 | 复旦大学 | Reversible electrochromism composite fiber and preparation method thereof |
CN102304857B (en) * | 2011-06-03 | 2013-05-08 | 鹏程实业有限公司 | Chameleon fiber fabric processing technology |
CN103898592B (en) * | 2014-02-26 | 2016-05-04 | 东华大学 | A kind of preparation method of electrochromic intelligent fiber |
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Application publication date: 20150916 Assignee: Jiangsu Wenfeng Chemical Fiber Group Co., Ltd. Assignor: Donghua University Contract record no.: 2019310000033 Denomination of invention: Preparation method of polymermaster batch and fiber having moisture absorption colorating function Granted publication date: 20170606 License type: Exclusive License Record date: 20190417 |