CN108410165A - A kind of preparation method of high color fastness low melting point polyamide Masterbatch - Google Patents
A kind of preparation method of high color fastness low melting point polyamide Masterbatch Download PDFInfo
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- CN108410165A CN108410165A CN201810144084.4A CN201810144084A CN108410165A CN 108410165 A CN108410165 A CN 108410165A CN 201810144084 A CN201810144084 A CN 201810144084A CN 108410165 A CN108410165 A CN 108410165A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/06—Polyamides derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/08—Copolymers of ethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0041—Optical brightening agents, organic pigments
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The invention discloses a kind of preparation methods of high color fastness low melting point polyamide Masterbatch, it counts in parts by weight, 60 95 parts of carriers, 4 40 parts of colorants, 0.1 7 parts of dispersants are added in mixing machine and are uniformly mixed, at 200~230 DEG C, melt blending is carried out with double screw extruder, then it is granulated, the high color fastness low melting point polyamide Masterbatch is made；The wherein described carrier is made of low-melting-point copolyamides and ethylene-vinyl acetate copolymer；The low-melting-point copolyamides are made of following components：50 60 parts of 30 40 parts of caprolactam, 10 20 parts of nylon salt, diacid and diamines；The molar ratio of the wherein described diacid and diamines is 1：0.9~1.1.Masterbatch good dispersion prepared by the present invention, coloring are strong, and have good color fastness.
Description
Technical field
The invention belongs to Masterbatch technical fields, and in particular to a kind of system of high color fastness low melting point polyamide Masterbatch
Preparation Method.
Background technology
In general, polyamide is a kind of higher melting-point polymer, the most commonly used polyamide 6 and polyamide 66 it is molten
Point is respectively 220 DEG C and 260 DEG C.This is because the amide group in polyamide molecule chain can form hydrogen bond, to increase
The active force of molecule interchain.Polyamide has preferable moulding processability and excellent comprehensive performance, both can also may be used with spinning
To be processed into thin-film material, it is also used as engineering plastics.By introducing that some molecular structures are irregular or Long carbon chain is total to
Poly- unit expands its application field to influence the formation of hydrogen bond in strand.Low-melting-point copolyamides also have lower crystallization
Degree and with preferable transparency, therefore low-melting-point copolyamides mainly can be applied to thermosol, meldable fibre, setline
Deng in application.But at present for the research of the colouring method of low melting point meldable fibre and few.The dyeing of traditional Fypro
Mainly by weaving into processes such as the later printing and dyeing arrangements of cloth come what is realized, this painting methods technological process is complicated, and
It is easy to pollute the environment.It, need not be first due to the particularity of its application and for low-melting-point copolyamides fiber
It is processed into cloth, therefore this method is not particularly suited for the coloring of low-melting-point copolyamides fiber.
And color method is that pigment is mixed into spinning solution or spinning melt before spinning, and directly produces coloured chemical fiber
A kind of method, its relatively traditional colouring method is more environmentally friendly, has the tendency that ever more popular.And it is not required to first compile fiber
It is made into cloth to dye again, so the dyeing especially suitable for meldable fibre.Dye technology before being spun at present to polyester and polyethylene etc.
Comparative maturity is studied, and the research coloured before being spun to polyamide is less, the color that can be added also compares limitation, for low melting point
The researches that copolyamide colours before spinning.Coloring can use the Masterbatch that carrier is polyamide 6 to carry out before the spinning of polyamide 6
Coloring.If low-melting-point copolyamides are coloured using carrier as the Masterbatch of polyamide 6, although excellent in compatibility,
Obtained product fusing point will improve, and influence the hot molten characteristic of fiber.And if low-melting-point copolyamides are used alone as load
Body, although smaller on the influence of the fusing point of final product, obtained product colour fastness to perspiration is poor, does not meet haberdashery mark
It is accurate.
Invention content
In view of the problems of the existing technology, the present invention provides a kind of high color fastness low melting point polyamide Masterbatch
Preparation method.
The present invention uses following technical scheme：
A kind of preparation method of high color fastness low melting point polyamide Masterbatch, is counted in parts by weight, and 60-95 parts are carried
Body, 4-40 part colorant, 0.1-7 parts of dispersants are added in mixing machine and are uniformly mixed, and at 200~230 DEG C, use twin-screw extrusion
Machine carries out melt blending, is then granulated, and the high color fastness low melting point polyamide Masterbatch is made；
The wherein described carrier is made of low-melting-point copolyamides and ethylene-vinyl acetate copolymer；
The low-melting-point copolyamides are made of following components：
30-40 parts of caprolactam
10-20 parts of nylon salt
50-60 parts of diacid and diamines；
The molar ratio of the wherein described diacid and diamines is 1：0.9~1.1, preferably 1：1.
Further, the weight part ratio of the low-melting-point copolyamides and ethylene-vinyl acetate copolymer is 3~9：1.
In some embodiments, the weight part ratio of the low-melting-point copolyamides and ethylene-vinyl acetate copolymer is 3~4：1；
In some embodiments, the weight part ratio of the low-melting-point copolyamides and ethylene-vinyl acetate copolymer is 4~6：1；One
In a little embodiments, the weight part ratio of the low-melting-point copolyamides and ethylene-vinyl acetate copolymer is 7~9：1.
Further, the diacid is one or more in adipic acid, decanedioic acid, heneicosanedioic acid, dodecanedioic acid.
In some embodiments, the diacid is adipic acid；In some embodiments, the diacid is decanedioic acid；In some embodiments
In, the diacid is heneicosanedioic acid；In some embodiments, the diacid is dodecanedioic acid.
Further, the diamines is decamethylene diamine and/or dodecamethylene diamine.In some embodiments, the diamines is the last of the ten Heavenly stems
Diamines；In some embodiments, the diamines is dodecamethylene diamine；In some embodiments, the diamines is decamethylene diamine and ten
Dioxane diamines.
Further, the molecular weight of the ethylene-vinyl acetate copolymer is 1000~10000.
Further, the vinyl acetate moiety content in the ethylene-vinyl acetate copolymer is 20~40%, flowing
Property and flexibility match with whole system.
Further, the colorant is organic pigment or organic dyestuff, including the organic face of phthalocyanine organic pigment, anthraquinone
Material, solvent dye.In some embodiments, the colorant is phthalocyanine blue (vat blue 15：3)；In some embodiments, institute
It is pigment blue 60 to state colorant；In some embodiments, the colorant is dyestuff indigo plant RA.
Further, the dispersant is polyethylene glycol, Metallic stearates, aluminium titanium composite coupler, trihydroxy methyl second
It is one or more in alkane.
Further, the preparation method of the low-melting-point copolyamides includes the following steps：By caprolactam, nylon66 fiber
Salt, diacid and diamines are added to according to proportioning in reaction kettle, are passed through nitrogen and are displaced air in reaction kettle, then gradually heating
To 210~230 DEG C, polymerisation is carried out under nitrogen protection, as reaction carries out, pressure gradually rises to 0.8~1.2MPa,
0.5~1.5h is kept at this pressure, then again unloads the pressure of reaction kettle to normal pressure in 1h, then reacts 2~4h dischargings,
Pelletizing is carried out with pelleter using after bosh, 12~18h of cold water soak is then first used, then in 75~85 DEG C of baking oven
Middle 20~30h of drying.
It is further preferred that the preparation method of the low-melting-point copolyamides includes the following steps：By caprolactam, nylon
66 salt, diacid and diamines are added to according to proportioning in polymerization reaction kettle, are passed through nitrogen 20min and are displaced air in reaction kettle,
Then 220 DEG C are gradually heating to, carries out polymerisation under nitrogen protection, as reaction carries out, pressure gradually rises to 0.8~
1.2MPa keeps 1h at this pressure, then again unloads the pressure of reaction kettle to normal pressure in 1h, then reacts 2~4h dischargings
Tape is obtained, which carries out pelletizing after bosh with pelleter, cold water soak 16h is then first used, then at 80 DEG C
Baking oven in it is dry for 24 hours.
Further, the fusing point of the low-melting-point copolyamides is 105~120 DEG C.
The high color fastness low melting point polyamide Masterbatch obtained belongs to low melting point Masterbatch；In some embodiments
In, the fusing point of the Masterbatch is less than 140 DEG C；In some embodiments, the fusing point of the Masterbatch is less than 130 DEG C；In some implementations
In example, the fusing point of the Masterbatch is less than 120 DEG C；In some embodiments, the fusing point of the Masterbatch is less than 110 DEG C.
The present invention provides a kind of good dispersion, strong and with good color fastness the low melting point polyamide color masterbatch of coloring
Grain.The carrier selected by Masterbatch in the present invention is that low-melting-point copolyamides and ethylene-polyvinyl acetate copolymer (EVA) are total
Mixed object, the presence of EVA can be such that colorant is effectively dispersed in carrier, and be well bonded with carrier, to improve
The color fastness of product.
Take the low-melting-point copolyamides of the low melting point polyamide Masterbatch and 80~95 parts by weight of 5~20 parts by weight
It is mixed, then carries out composite spinning, finally obtain coloured low-melting-point copolyamides fiber.
Compared with prior art, beneficial effects of the present invention：Low-melting-point copolyamides fibre is solved using colouring before spinning
The coloring problem of dimension, wherein Masterbatch carrier select the copolymerization of low-melting-point copolyamides and ethylene-vinyl acetate copolymer (EVA)
Object, with use conventional higher melting-point polyamide 6 (220.6 DEG C of fusing point) as carrier compared with, low-melting-point copolyamides are to rear
The fusing point of continuous fiber influences smaller.And EVA can improve the binding force between colorant and carrier, be spun using the Masterbatch
The fiber obtained after silk has preferable color fastness, can apply in garment industry.
Specific implementation mode
In order to preferably explain the present invention, it is described further in conjunction with following specific examples, but the present invention is unlimited
In specific embodiment.
Embodiment 1
It is 105 DEG C of low-melting-point copolyamides by the fusing point of 72 parts by weight, the ethylene-vinyl acetate copolymer of 20 parts by weight
(EVA), the phthalocyanine blue (vat blue 15 of 6 parts by weight：3) with the polyethylene glycol of 2 parts by weight, double screw extruder is used at 200 DEG C
Melt blending is carried out, is then granulated, high color fastness low melting point polyamide blue master batch is prepared.
Embodiment 2
It is 120 DEG C of low-melting-point copolyamides by the fusing point of 76 parts by weight, the ethylene-vinyl acetate copolymer of 15 parts by weight
(EVA), 5 parts by weight pigment blue 60s and 4 parts by weight aluminium titanium composite couplers are uniformly mixed in mixing machine, with double at 210 DEG C
Screw extruder carries out melt blending, is then granulated, high color fastness low melting point polyamide blue master batch is prepared.
Embodiment 3
It is 110 DEG C of low-melting-point copolyamides by the fusing point of 80 parts by weight, the ethylene-vinyl acetate copolymer of 10 parts by weight
(EVA), the dyestuff indigo plant RA of 7 parts by weight and the Metallic stearates of 3 parts by weight, which are added in mixing machine, is uniformly mixed, at 230 DEG C,
Melt blending is carried out with double screw extruder, is then granulated, high color fastness low melting point polyamide blue master batch is prepared.
Color fastness is tested
The low melting point of the Masterbatch of the embodiment 1-3 of 5~20 parts by weight and 80~95 parts by weight is copolymerized acyl respectively
Amine is mixed, and composite spinning is then carried out, and obtains low-melting-point copolyamides fiber sample.Comparative example 1 is same as Example 1,
Ethylene-vinyl acetate copolymer is only free of in the Masterbatch of comparative example 1.
Each sample is stitched together with STANDARD ADJACENT FABRIC respectively.According to 105 E04 of standard ISO《Colour fastness to perspiration
Test method》With 105 E02 of standard ISO《Resistance to colour fastness to water test method》Fabric after suture is put into different tests
30min is impregnated in liquid.Test solution extra on fabric is first slightly removed after immersion, and then fabric is placed in two in experimental provision
Block has pressure (fabric pressure be 12.5KPa) between the tablet of authorized pressure, and 4h is handled at (37 ± 2) DEG C.It goes again
Except pressure, sample and adjacent fabric are unfolded, is laid in the baking oven no more than 60 DEG C and dries.Finally sample is evaluated with gray card
The staining of discoloration and adjacent fabric.It fades and staining fastness is divided into 5 grades, 5 grades preferably, and 1 grade worst.Test result is listed in table 1.
Table 1：Color fastness test result.
From the results of view, in sweat stain and briny environment, the color fastness of comparative example 1 is poor, occurs on adjacent fabric
Apparent blue.And in embodiment 1-3, good color fastness is shown under various test conditions, stickers lining is knitted after test
There is not apparent staining phenomenon in object, shows that EVA is added in Masterbatch carrier can effectively promote the color of final products
Fastness.
Above is only a specific embodiment of the present invention, it is not intended to limit the scope of the invention, every utilization
The equivalent transformation that the present invention makees is applied directly or indirectly in other relevant technical fields, is similarly included in the present invention's
Among scope of patent protection.
Claims (10)
1. a kind of preparation method of high color fastness low melting point polyamide Masterbatch, which is characterized in that it counts in parts by weight, it will
60-95 parts of carriers, 4-40 parts of colorants, 0.1-7 parts of dispersants are added in mixing machine and are uniformly mixed, and at 200~230 DEG C, use
Double screw extruder carries out melt blending, is then granulated, and the high color fastness low melting point polyamide Masterbatch is made；
The wherein described carrier is made of low-melting-point copolyamides and ethylene-vinyl acetate copolymer；
The low-melting-point copolyamides are made of following components：
30-40 parts of caprolactam
10-20 parts of nylon salt
50-60 parts of diacid and diamines；
The molar ratio of the wherein described diacid and diamines is 1：0.9~1.1.
2. the preparation method of high color fastness low melting point polyamide Masterbatch according to claim 1, which is characterized in that institute
The weight part ratio for stating low-melting-point copolyamides and ethylene-vinyl acetate copolymer is 3~9：1.
3. the preparation method of high color fastness low melting point polyamide Masterbatch according to claim 1, which is characterized in that institute
It is one or more in adipic acid, decanedioic acid, heneicosanedioic acid, dodecanedioic acid to state diacid.
4. the preparation method of high color fastness low melting point polyamide Masterbatch according to claim 1, which is characterized in that institute
It is decamethylene diamine and/or dodecamethylene diamine to state diamines.
5. the preparation method of high color fastness low melting point polyamide Masterbatch according to claim 1, which is characterized in that institute
The molecular weight for stating ethylene-vinyl acetate copolymer is 1000~10000.
6. the preparation method of high color fastness low melting point polyamide Masterbatch according to claim 1, which is characterized in that institute
It is 20~40% to state the vinyl acetate moiety content in ethylene-vinyl acetate copolymer.
7. the preparation method of high color fastness low melting point polyamide Masterbatch according to claim 1, which is characterized in that institute
It includes phthalocyanine organic pigment, anthraquinone organic pigment, solvent dye to state colorant.
8. the preparation method of high color fastness low melting point polyamide Masterbatch according to claim 1, which is characterized in that institute
It is one or more in polyethylene glycol, Metallic stearates, aluminium titanium composite coupler, trimethylolethane to state dispersant.
9. the preparation method of high color fastness low melting point polyamide Masterbatch according to claim 1, which is characterized in that institute
The preparation method for stating low-melting-point copolyamides includes the following steps：By caprolactam, nylon salt, diacid and diamines according to proportioning
It is added in reaction kettle, is passed through nitrogen and displaces air in reaction kettle, be then gradually heating to 210~230 DEG C, protected in nitrogen
Shield is lower to carry out polymerisation, and as reaction carries out, pressure gradually rises to 0.8~1.2MPa, keep 0.5 at this pressure~
Then 1.5h again unloads the pressure of reaction kettle to normal pressure in 1h, then react 2~4h dischargings, using being used after bosh
Pelleter carries out pelletizing, then first uses 12~18h of cold water soak, then dry 20~30h in 75~85 DEG C of baking oven.
10. the preparation method of high color fastness low melting point polyamide Masterbatch according to claim 1, which is characterized in that
The fusing point of the low-melting-point copolyamides is 105~120 DEG C.
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| CN109970969A (en) * | 2019-04-10 | 2019-07-05 | 山东广垠新材料有限公司 | A kind of preparation method of ternary polymerization low melting point nylon |
| CN110878139A (en) * | 2018-09-06 | 2020-03-13 | 华峰集团有限公司 | Low-melting-point high-flow ternary random copolymer polyamide modified base resin and preparation method thereof |
| CN111909508A (en) * | 2020-08-25 | 2020-11-10 | 温州大学 | Copolyamide hot-melt adhesive resin and preparation method thereof |
| CN114685818A (en) * | 2020-12-31 | 2022-07-01 | 中国纺织科学研究院有限公司 | Preparation method of polyamide color master batch carrier resin and polyamide color master batch |
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| CN110878139A (en) * | 2018-09-06 | 2020-03-13 | 华峰集团有限公司 | Low-melting-point high-flow ternary random copolymer polyamide modified base resin and preparation method thereof |
| CN110878139B (en) * | 2018-09-06 | 2022-06-17 | 华峰集团有限公司 | Low-melting-point high-flow ternary random copolymer polyamide modified base resin and preparation method thereof |
| CN109970969A (en) * | 2019-04-10 | 2019-07-05 | 山东广垠新材料有限公司 | A kind of preparation method of ternary polymerization low melting point nylon |
| CN109970969B (en) * | 2019-04-10 | 2021-06-22 | 山东广垠新材料有限公司 | Preparation method of terpolymer low-melting-point nylon |
| CN111909508A (en) * | 2020-08-25 | 2020-11-10 | 温州大学 | Copolyamide hot-melt adhesive resin and preparation method thereof |
| CN111909508B (en) * | 2020-08-25 | 2022-04-12 | 温州大学 | Copolyamide hot-melt adhesive resin and preparation method thereof |
| CN114685818A (en) * | 2020-12-31 | 2022-07-01 | 中国纺织科学研究院有限公司 | Preparation method of polyamide color master batch carrier resin and polyamide color master batch |
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