CN104910566A - Preparation method of polymermaster batch and fiber having moisture absorption colorating function - Google Patents
Preparation method of polymermaster batch and fiber having moisture absorption colorating function Download PDFInfo
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- CN104910566A CN104910566A CN201510299169.6A CN201510299169A CN104910566A CN 104910566 A CN104910566 A CN 104910566A CN 201510299169 A CN201510299169 A CN 201510299169A CN 104910566 A CN104910566 A CN 104910566A
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Abstract
The invention provides a preparation method of a polymermaster batch and fiber having a moisture absorption colorating function. The preparation methodof a polymermaster batch having a moisture absorption colorating function is characterized by comprising the following steps: step 1, putting porous nano-powder, triallylisocyanurate, polyethylene glycol diacrylate, polyethylene glycol monomethyl etheracrylate, an initiator, humidity-sensitive color changing powder and a color changing sensitizer into water serving as a solvent; reacting for 2-5h at 70-80 DEG C by adopting a reduced-pressure ultrasonic dispersion method; and performing centrifugal dewatering to obtain a composite functional material with a moisture absorption colorating function; and step 2, drying the composite functional material with a moisture absorption colorating function; granulating the composite functional material and polymer chips together in a twin screw blending way, thus obtainingpolymermaster batch having a moisture absorption colorating function. The obtained material having moisture absorption colorating function has a microcapsule-like structure and has the advantages of good heat resistance and stable property; in addition, the preparation process is simple and the cost is low.
Description
Technical field
The invention belongs to the preparation field of coloring function fiber, particularly a kind of have the polymer masterbatch of moisture absorption coloring function and the preparation method of fiber thereof.
Background technology
Cameleon fibre initiatively can change the functional fibre of self color after generally referring to ambient conditionss such as being subject to light, thermal and magnetic, electricity or moisture.At present, report and more mainly contain photoinduction and the large series products of temperature-induced cameleon fibre two.For the polymkeric substance of moisture absorption induced discoloration fiber and fiber report less, and the method for the surperficial aftertreatment of the many employings of its preparation process.National inventing patent CN 101962913 B discloses a kind of reversible electrochromic conjugated fibre and preparation method thereof, namely have employed the method for surface-coated.National inventing patent CN 102304857 B reports a kind of Chameleon fiber fabric processing technology based on graft polymerization method, then utilize Final finishing chemical surface grafting and coating color changing media.But no matter be in surface-coated, or chemical conversion treatment, all likely residual poisonous intermediate monomer or heavy metal ion, and there is the problem of the degree of enduring hardships of coat.
For the problems referred to above, the present invention adopts porous nano powder to be carrier, under ultrasonic reduced pressure, packing is carried out to wet sensitive colour changing agent, adopt polyalkylene glycol acrylate monomethyl ether ester for leading wet chain, colour developing effect strengthened by variable color sensitizing agent, prepared the polymer masterbatch with moisture absorption coloring function and fiber with high thermal stability.For the functionalization realizing general fiber provides thinking.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind ofly has the polymer masterbatch of moisture absorption coloring function and the preparation method of fiber thereof, the method utilizes porous nano powder to encapsulate wet sensitive colour changing agent and sensitizing agent thereof, form the structure of similar microcapsule, and this structure has more thermotolerance; The polyalkylene glycol acrylate monomethyl ether ester used in encapsulants has good water-absorbent, can promote as colour developing change provides support.The polymer masterbatch of the moisture absorption coloring function that the present invention relates to can well be applied in the general fiber art such as polypropylene, polyvinyl alcohol, polyester, polymeric amide.
In order to solve the problems of the technologies described above, the invention provides a kind of preparation method with the polymer masterbatch of moisture absorption coloring function, it is characterized in that, comprising:
Step 1: porous nano powder, cyanacrylate, polyethyleneglycol diacrylate, polyalkylene glycol acrylate monomethyl ether ester, initiator, wet sensitive colour changing powder and variable color sensitizing agent are placed in aqueous solvent, adopt the method for depressurizing ultrasonic dispersion, react 2 ~ 5 hours at 70-80 DEG C, finally by obtaining the composite functional material with moisture absorption coloring function after centrifuge dehydration;
Step 2: by above-mentioned there is the composite functional material drying process of moisture absorption coloring function after, with polymer chips through the blended granulation of twin screw, obtain the polymer masterbatch with moisture absorption coloring function.
Preferably, the ratio of the porous nano powder in described step 1, cyanacrylate, polyethyleneglycol diacrylate, initiator, wet sensitive colour changing powder, variable color sensitizing agent, 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 porous silica, multilayer polynite, one or both in aerogel and diatomite are composited, and its particle diameter is 50 ~ 600nm.
Preferably, described polymer chips is the one of polypropylene, polyvinyl alcohol, polyester and polymeric amide section.
Preferably, described initiator is azo-bis-isobutyrate hydrochloride or ammonium persulphate.
Preferably, described wet sensitive colour changing powder is the title complex of cobalt chloride, hexamethylenetetramine, and mass ratio is 50 ~ 99: 1 ~ 50.
Preferably, described variable color sensitizing agent is carboxamide.
Preferably, the described composite functional material with moisture absorption coloring function and the quality of polymer chips are 5: 95 ~ 15: 85.
Present invention also offers a kind of preparation method with the polymer fiber of moisture absorption coloring function, it is characterized in that, comprise the above-mentioned polymer masterbatch with the polymer fiber of moisture absorption coloring function is obtained the polymer fiber with moisture absorption coloring function through melt-spinning.
Compared with prior art, the invention has the beneficial effects as follows:
(1) moisture absorption coloring function material of the present invention has similar microcapsule structure, have the advantage of good heat resistance, stable performance, and preparation technology is simple, with low cost.
(2) the moisture absorption coloring function material that prepared by the present invention has conduit pipe, can contribute to the colour developing effect of functional agglomerate and fiber.
(3) the moisture absorption coloring function fiber prepared of the present invention, preparation is simple, without degree of the enduring hardships problem of surface-coated, and can not produce poisonous intermediate monomer or heavy metal ion.
(4) the moisture absorption coloring function modification thinking prepared of the present invention, well can be applied to the functional modification field of the general fibers such as polypropylene, polyvinyl alcohol, urethane, polyester, polymeric amide, polyphenylene sulfide.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Polyethyleneglycol diacrylate described in various embodiments of the present invention is purchased from lark prestige Science and Technology Ltd., and its number-average molecular weight 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 synthesis, and its number-average molecular weight is 1000 ~ 10000.
Embodiment 1
There is a preparation method for the polymer masterbatch of moisture absorption coloring function, be specially:
First, by the cobalt chloride of the initiator ammonium persulfate of the polyethyleneglycol diacrylate of the cyanacrylate of the multilayer polynite (particle diameter is about 600nm) of 20g, 8g, 5g, 1g, 40g, hexamethylenetetramine title complex (cobalt chloride accounts for 80% of title complex quality), the variable color sensitizing agent carboxamide of 5g, the polyalkylene glycol acrylate monomethyl ether ester of 21g, join in 200ml deionized water, adopt the method (pressure 200Pa ~ 500Pa of depressurizing ultrasonic dispersion, ultrasonic frequency 20 ~ 40KHz), be warming up to 75 DEG C of reactions 5 hours.The powder body material of moisture absorption coloring function is obtained after centrifuge dehydration, for subsequent use through 80 DEG C of dryings 12 hours.
By the moisture absorption coloring function powder of the 15g of drying treatment and the polymeric amide of 85g through twin screw extruder 240 ~ 260 DEG C of blended granulations, obtain the polymer masterbatch with moisture absorption coloring function, and the tynex of moisture absorption coloring function is obtained through melt spinning machine, wherein spinning temperature 260 ~ 280 DEG C, spins speed 800 ~ 3500m/min.Find after tested, the fiber of preparation can change pink into by purple under humidity is greater than 40% environment.
Embodiment 2
A kind of preparation method with the polymer masterbatch of moisture absorption coloring function, be specially: first, by the porous silica (particle diameter is about 50nm) of 40g, the cyanacrylate of 4g, the polyethyleneglycol diacrylate of 10g, the initiator azo-bis-isobutyrate hydrochloride of 0.1g, the cobalt chloride of 20g, hexamethylenetetramine title complex (cobalt chloride accounts for 90% of title complex quality), the variable color sensitizing agent carboxamide of 10g, the polyalkylene glycol acrylate monomethyl ether ester of 15.9g, join in 200ml deionized water, adopt the method (pressure 200Pa ~ 500Pa of depressurizing ultrasonic dispersion, ultrasonic frequency 20 ~ 40KHz), be warming up to 75 DEG C of reactions 2 hours.The powder body material of moisture absorption coloring function is obtained after centrifuge dehydration, for subsequent use through 80 DEG C of dryings 12 hours.By polyester twin screw extruder 260 ~ 280 DEG C of blended granulations of the moisture absorption coloring function powder of the 5g of drying treatment and 95g, obtain the polymer masterbatch with moisture absorption coloring function, and the tynex of moisture absorption coloring function is obtained through melt spinning machine, wherein spinning temperature 270 ~ 300 DEG C, spins speed 800 ~ 3500m/min.Find after tested, find after tested, the fiber of preparation can change pink into by purple under humidity is greater than 50% environment.
Embodiment 3
There is a preparation method for the polymer masterbatch of moisture absorption coloring function, be specially:
First, by the wet sensitive colour changing powder cobalt chloride of the initiator ammonium persulfate of the polyethyleneglycol diacrylate of the cyanacrylate of the diatomite (particle diameter is about 600nm) of 30g, 4g, 5g, 1g, 30g, hexamethylenetetramine title complex (cobalt chloride accounts for 95% of title complex quality), the variable color sensitizing agent carboxamide of 10g, the polyalkylene glycol acrylate monomethyl ether ester of 20g, join in 200ml deionized water, adopt the method (pressure 200Pa ~ 500Pa of depressurizing ultrasonic dispersion, ultrasonic frequency 20 ~ 40KHz), be warming up to 75 DEG C of reactions 4 hours.The powder body material of moisture absorption coloring function is obtained after centrifuge dehydration, for subsequent use through 80 DEG C of dryings 12 hours.
By the moisture absorption coloring function powder of the 10g of drying treatment and the polypropylene of 90g through twin screw extruder 180 ~ 200 DEG C of blended granulations, obtain the polymer masterbatch with moisture absorption coloring function, and the tynex of moisture absorption coloring function is obtained through melt spinning machine, wherein spinning temperature 200 ~ 230 DEG C, spins speed 800 ~ 2500m/min.Find after tested, find after tested, the fiber of preparation can change pink into by purple under humidity is greater than 50% environment.
Embodiment 4
There is a preparation method for the polymer masterbatch of moisture absorption coloring function, be specially:
First, by the multilayer polynite (particle diameter is about 400nm) of 10g, the diatomite (particle diameter is about 400nm) of 10g, the cyanacrylate of 5g, the polyethyleneglycol diacrylate of 5g, the initiator azo-bis-isobutyrate hydrochloride of 1g, the cobalt chloride of 40g, hexamethylenetetramine title complex (cobalt chloride accounts for 98% of title complex quality), the variable color sensitizing agent carboxamide of 5g, the polyalkylene glycol acrylate monomethyl ether ester of 24g, join in 200ml deionized water, adopt the method (pressure 200Pa ~ 500Pa of depressurizing ultrasonic dispersion, ultrasonic frequency 20 ~ 40KHz), be warming up to 75 DEG C of reactions 3 hours.The powder body material of moisture absorption coloring function is obtained after centrifuge dehydration, for subsequent use through 80 DEG C of dryings 12 hours.
By the moisture absorption coloring function powder of the 10g of drying treatment and the polyvinyl alcohol (swelling treatment of 90g, containing 5% ~ 10% solvent) through twin screw extruder 95 ~ 105 DEG C of blended granulations, obtain the polymer masterbatch with moisture absorption coloring function, and the tynex of moisture absorption coloring function is obtained through melt spinning machine, wherein spinning temperature 100 ~ 115 DEG C, spins speed 500 ~ 1500m/min.
Find after tested, the fiber of preparation can change pink into by purple under humidity is greater than 40% environment.
Claims (9)
1. there is a preparation method for the polymer masterbatch of moisture absorption coloring function, it is characterized in that, comprising:
Step 1: porous nano powder, cyanacrylate, polyethyleneglycol diacrylate, polyalkylene glycol acrylate monomethyl ether ester, initiator, wet sensitive colour changing powder and variable color sensitizing agent are placed in aqueous solvent, adopt the method for depressurizing ultrasonic dispersion, react 2 ~ 5 hours at 70-80 DEG C, finally by obtaining the composite functional material with moisture absorption coloring function after centrifuge dehydration;
Step 2: by above-mentioned there is the composite functional material drying process of moisture absorption coloring function after, with polymer chips through the blended granulation of twin screw extruder, obtain 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 characterized in that, the ratio of the porous nano powder in described step 1, cyanacrylate, polyethyleneglycol diacrylate, initiator, wet sensitive colour changing powder, variable color sensitizing agent, 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.
3. there is the preparation method of the polymer masterbatch of moisture absorption coloring function as claimed in claim 1, it is characterized in that, described porous nano powder is porous silica, multilayer polynite, one or both in aerogel and diatomite are composited, and its particle diameter is 50 ~ 600nm.
4. have the preparation method of the polymer masterbatch of moisture absorption coloring function as claimed in claim 1, it is characterized in that, described polymer chips is the one of polypropylene, polyvinyl alcohol, polyester and polymeric amide section.
5. have the preparation method of the polymer masterbatch of moisture absorption coloring function as claimed in claim 1, it is characterized in that, described initiator is ammonium persulphate or azo-bis-isobutyrate hydrochloride.
6. have the preparation method of the polymer masterbatch of moisture absorption coloring function as claimed in claim 1, it is characterized in that, described wet sensitive colour changing powder is the title complex of cobalt chloride, hexamethylenetetramine, and mass ratio is 50 ~ 99: 1 ~ 50.
7. have the preparation method of the polymer masterbatch of moisture absorption coloring function as claimed in claim 1, it is characterized in that, described variable color sensitizing agent is carboxamide.
8. have the preparation method of the polymer masterbatch of moisture absorption coloring function as claimed in claim 1, it is characterized in that, the described composite functional material with moisture absorption coloring function and the quality of polymer chips are 5: 95 ~ 15: 85.
9. there is a preparation method for the polymer fiber of moisture absorption coloring function, it is characterized in that, comprise the polymer masterbatch with moisture absorption coloring function according to any one of claim 1-8 is obtained the polymer fiber with moisture absorption coloring function through melt-spinning.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106046244A (en) * | 2016-05-30 | 2016-10-26 | 广州海谷电子科技有限公司 | Nonelectrolyte macromolecule humidity-sensitive resin, preparation method thereof and conductive ink and humidity-sensitive sensor produced based on nonelectrolyte macromolecule humidity-sensitive resin |
| CN106381567A (en) * | 2016-08-31 | 2017-02-08 | 浙江省现代纺织工业研究院 | Method for producing liquid-phase dyeable polypropylene fiber |
| 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 |
| 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 |
| 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 |
| 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 |
| CN112964650A (en) * | 2021-02-05 | 2021-06-15 | 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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| CN101962913A (en) * | 2009-07-22 | 2011-02-02 | 复旦大学 | Reversible electrochromism composite fiber and preparation method thereof |
| CN102304857A (en) * | 2011-06-03 | 2012-01-04 | 鹏程实业有限公司 | Chameleon fiber fabric processing technology |
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Patent Citations (3)
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| CN101962913A (en) * | 2009-07-22 | 2011-02-02 | 复旦大学 | Reversible electrochromism composite fiber and preparation method thereof |
| CN102304857A (en) * | 2011-06-03 | 2012-01-04 | 鹏程实业有限公司 | Chameleon fiber fabric processing technology |
| CN103898592A (en) * | 2014-02-26 | 2014-07-02 | 东华大学 | Preparation method of electrochromic intelligent fiber |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106046244A (en) * | 2016-05-30 | 2016-10-26 | 广州海谷电子科技有限公司 | Nonelectrolyte macromolecule humidity-sensitive resin, preparation method thereof and conductive ink and humidity-sensitive sensor produced based on nonelectrolyte macromolecule humidity-sensitive resin |
| 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 |
| CN106381567A (en) * | 2016-08-31 | 2017-02-08 | 浙江省现代纺织工业研究院 | Method for producing liquid-phase dyeable polypropylene fiber |
| 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 |
| 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 |
| 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 |
| 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 |
| CN112964650A (en) * | 2021-02-05 | 2021-06-15 | 武汉纺织大学 | Fiber-based humidity sensor based on moisture absorption and color change and preparation method thereof |
| 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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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 |
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