CN108410165B - Preparation method of color master batch for high-color-fastness low-melting-point polyamide - Google Patents
Preparation method of color master batch for high-color-fastness low-melting-point polyamide Download PDFInfo
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- CN108410165B CN108410165B CN201810144084.4A CN201810144084A CN108410165B CN 108410165 B CN108410165 B CN 108410165B CN 201810144084 A CN201810144084 A CN 201810144084A CN 108410165 B CN108410165 B CN 108410165B
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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
-
- 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
Abstract
The invention discloses a preparation method of a color master batch for high-color fastness low-melting-point polyamide, which comprises the following steps of adding 60-95 parts by weight of a carrier, 4-40 parts by weight of a colorant and 0.1-7 parts by weight of a dispersant into a mixer, uniformly mixing, carrying out melt blending by using a double-screw extruder at the temperature of 200-230 ℃, and then carrying out granulation to prepare the color master batch for high-color fastness low-melting-point polyamide; wherein the carrier is made of a low melting point copolyamide and an ethylene-vinyl acetate copolymer; the low melting copolyamide is made from the following components: 30-40 parts of caprolactam, 10-20 parts of nylon 66 salt and 50-60 parts of diacid and diamine; wherein the molar ratio of diacid to diamine is 1: 0.9 to 1.1. The color master batch prepared by the invention has good dispersibility, strong colorability and good color fastness.
Description
Technical Field
The invention belongs to the technical field of color master batches, and particularly relates to a preparation method of a color master batch for high-color-fastness low-melting-point polyamide.
Background
Generally, polyamide is a relatively high melting polymer, with polyamide 6 and polyamide 66 most commonly having melting points of 220 ℃ and 260 ℃, respectively. This is because the amide groups in the polyamide molecular chain can form hydrogen bonds, thereby increasing the force between the molecular chains. The polyamide has good molding processability and excellent comprehensive performance, can be spun, can be processed into a film material, and can also be used as engineering plastics. The formation of hydrogen bonds in molecular chains is influenced by introducing some copolymerization units with irregular molecular structures or long carbon chains, and the application field of the copolymer is expanded. The low melting point copolyamide also has lower crystallinity and better transparency, so the low melting point copolyamide can be mainly applied to hot melt adhesives, hot melt fibers, fishing lines and the like. However, the dyeing method of the low-melting-point hot-melt fiber is not much researched at present. The traditional polyamide fiber dyeing is mainly realized through the processes of printing, dyeing, finishing and the like after weaving into cloth, and the coloring method has complex process flow and is easy to cause pollution to the environment. Furthermore, the low-melting-point copolyamide fibers do not need to be processed into a cloth in advance due to the special application, and therefore, the method is not suitable for coloring the low-melting-point copolyamide fibers.
The dyeing method before spinning is a method for directly producing colored chemical fibers by mixing pigments into spinning solution or spinning melt, is more environment-friendly compared with the traditional dyeing method, and has a tendency of becoming popular day by day. And the dyeing process does not need to weave the fibers into cloth and then dye the cloth, so the dyeing process is particularly suitable for dyeing the hot-melt fibers. At present, the research on dyeing technologies before spinning such as polyester, polyethylene and the like is relatively mature, the research on dyeing before spinning of polyamide is less, the added color is relatively limited, and the research on dyeing before spinning of low-melting-point copolyamide is less. The polyamide 6 can be colored before spinning by using a color master batch with the carrier being polyamide 6. When the low-melting-point copolyamide is colored with a color master batch in which the carrier is polyamide 6, although the compatibility is excellent, the melting point of the obtained product is increased, and the hot-melt performance of the fiber is affected. On the other hand, if the low-melting-point copolyamide is used as a carrier, the influence on the melting point of the final product is small, but the obtained product has poor perspiration stain fastness and does not meet the standard of clothing.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a color master batch for high-color-fastness low-melting-point polyamide.
The invention adopts the following technical scheme:
a preparation method of a color master batch for high-color fastness low-melting-point polyamide comprises the steps of adding 60-95 parts by weight of a carrier, 4-40 parts by weight of a coloring agent and 0.1-7 parts by weight of a dispersing agent into a mixer, uniformly mixing, carrying out melt blending by using a double-screw extruder at the temperature of 200-230 ℃, and then carrying out granulation to prepare the color master batch for high-color fastness low-melting-point polyamide;
wherein the carrier is made of a low melting point copolyamide and an ethylene-vinyl acetate copolymer;
the low melting copolyamide is made from the following components:
caprolactam 30-40 parts
10-20 parts of nylon 66 salt
50-60 parts of diacid and diamine;
wherein the molar ratio of diacid to diamine is 1: 0.9 to 1.1, preferably 1: 1.
further, the weight part ratio of the low-melting-point copolyamide to the ethylene-vinyl acetate copolymer is 3-9: 1. in some embodiments, the weight ratio of the low-melting-point copolyamide to the ethylene-vinyl acetate copolymer is 3-4: 1; in some embodiments, the weight ratio of the low-melting-point copolyamide to the ethylene-vinyl acetate copolymer is 4-6: 1; in some embodiments, the weight ratio of the low-melting-point copolyamide to the ethylene-vinyl acetate copolymer is 7-9: 1.
further, the diacid is one or more of adipic acid, sebacic acid, undecanedioic acid and dodecanedioic acid. In some embodiments, the diacid is adipic acid; in some embodiments, the diacid is sebacic acid; in some embodiments, the diacid is undecanedioic acid; in some embodiments, the diacid is dodecanedioic acid.
Further, the diamine is decamethylene diamine and/or dodecane diamine. In some embodiments, the diamine is decamethylene diamine; in some embodiments, the diamine is dodecanediamine; in some embodiments, the diamines are decamethylene diamine and dodecane diamine.
Further, the molecular weight of the ethylene-vinyl acetate copolymer is 1000-10000.
Furthermore, the content of a vinyl acetate part in the ethylene-vinyl acetate copolymer is 20-40%, and the fluidity and the flexibility of the ethylene-vinyl acetate copolymer are matched with those of the whole system.
Further, the colorant is an organic pigment or an organic dye, and comprises a phthalocyanine organic pigment, an anthraquinone organic pigment and a solvent type dye. In some embodiments, the colorant is phthalocyanine blue (vat blue 15: 3); in some embodiments, the colorant is pigment blue 60; in some embodiments, the colorant is dye blue RA.
Further, the dispersing agent is one or more of polyethylene glycol, metal stearate, aluminum-titanium composite coupling agent and trimethylolethane.
Further, the preparation method of the low-melting-point copolyamide comprises the following steps: adding caprolactam, nylon 66 salt, diacid and diamine into a reaction kettle according to a ratio, introducing nitrogen to replace air in the reaction kettle, gradually heating to 210-230 ℃, carrying out polymerization reaction under the protection of nitrogen, gradually increasing the pressure to 0.8-1.2 MPa along with the reaction, keeping the pressure for 0.5-1.5 h, then unloading the pressure of the reaction kettle to normal pressure within 1h, then carrying out reaction for 2-4 h for discharging, then carrying out granulation by a granulator after passing through a cooling water tank, then soaking for 12-18 h by cold water, and then drying for 20-30 h in an oven at 75-85 ℃.
Further preferably, the preparation method of the low melting point copolyamide comprises the following steps: adding caprolactam, nylon 66 salt, diacid and diamine into a polymerization reaction kettle according to a ratio, introducing nitrogen for 20min to replace air in the reaction kettle, then gradually heating to 220 ℃, carrying out polymerization reaction under the protection of nitrogen, gradually increasing the pressure to 0.8-1.2 MPa along with the reaction, keeping the pressure for 1h, then unloading the pressure of the reaction kettle to normal pressure within 1h, then carrying out reaction for 2-4 h to obtain a strip, carrying out granulation on the strip by a granulator after passing through a cooling water tank, then soaking the strip by cold water for 16h, and then drying the strip in an oven at 80 ℃ for 24 h.
Further, the melting point of the low-melting-point copolyamide is 105-120 ℃.
The prepared color master batch for the polyamide with high color fastness and low melting point belongs to a low melting point color master batch; in some embodiments, the melting point of the color masterbatch is less than 140 ℃; in some embodiments, the melting point of the color masterbatch is less than 130 ℃; in some embodiments, the melting point of the color masterbatch is less than 120 ℃; in some embodiments, the melting point of the color masterbatch is less than 110 ℃.
The invention provides the color master batch for low-melting-point polyamide, which has good dispersibility, strong colorability and good color fastness. The carrier selected by the color master batch is a blend of low-melting-point copolyamide and ethylene-polyvinyl acetate copolymer (EVA), and the EVA can effectively disperse the colorant in the carrier and has good bonding force with the carrier, so that the color fastness of the product is improved.
And (3) mixing 5-20 parts by weight of the color master batch for the low-melting-point polyamide and 80-95 parts by weight of the low-melting-point copolyamide, and then carrying out composite spinning to finally obtain the colored low-melting-point copolyamide fiber.
Compared with the prior art, the invention has the beneficial effects that: the coloring problem of the low-melting-point copolyamide fiber is solved by adopting a coloring method before spinning, wherein the color master batch carrier selects a copolymer of low-melting-point copolyamide and ethylene-vinyl acetate copolymer (EVA), and compared with the conventional polyamide 6 (the melting point is 220.6 ℃) with higher melting point as a carrier, the low-melting-point copolyamide has smaller influence on the melting point of the subsequent fiber. The EVA can improve the binding force between the colorant and the carrier, and the fiber obtained by spinning the color master batch has better color fastness and can be applied to the field of clothing.
Detailed Description
For better explanation of the present invention, the following specific examples are further illustrated, but the present invention is not limited to the specific examples.
Example 1
72 parts by weight of low-melting-point copolyamide with a melting point of 105 ℃, 20 parts by weight of ethylene-vinyl acetate copolymer (EVA), 6 parts by weight of phthalocyanine blue (vat blue 15: 3) and 2 parts by weight of polyethylene glycol are melted and blended by a double-screw extruder at the temperature of 200 ℃, and then granulation is carried out to prepare the high-color-fastness low-melting-point polyamide blue color master batch.
Example 2
76 parts by weight of low-melting-point copolyamide with a melting point of 120 ℃, 15 parts by weight of ethylene-vinyl acetate copolymer (EVA), 5 parts by weight of pigment blue 60 and 4 parts by weight of aluminum-titanium composite coupling agent are uniformly mixed in a mixer, and are subjected to melt blending by a double-screw extruder at 210 ℃, and then are granulated to prepare the high-color-fastness low-melting-point polyamide blue color master batch.
Example 3
Adding 80 parts by weight of low-melting-point copolyamide with a melting point of 110 ℃, 10 parts by weight of ethylene-vinyl acetate copolymer (EVA), 7 parts by weight of dye blue RA and 3 parts by weight of metal stearate into a mixing machine, uniformly mixing, performing melt blending by using a double-screw extruder at 230 ℃, and then performing granulation to prepare the high-color-fastness low-melting-point polyamide blue master batch.
Color fastness test
5-20 parts by weight of the color master batch of example 1-3 and 80-95 parts by weight of the low-melting-point copolyamide are mixed respectively, and then composite spinning is carried out to obtain a low-melting-point copolyamide fiber sample. Comparative example 1 is the same as example 1 except that the masterbatch of comparative example 1 does not contain ethylene vinyl acetate.
Each sample was separately sewn together with a standard padded fabric. The stitched fabric was immersed in different test solutions for 30min according to ISO Standard 105E 04 "test method for fastness to perspiration" and ISO Standard 105E 02 "test method for fastness to water staining". After soaking, removing the excessive test solution slightly, placing the fabric between two plates with specified pressure in an experimental device, pressing (the fabric is under 12.5KPa), and treating at 37 + -2 deg.C for 4 h. And removing the pressure, unfolding the sample and the lining fabric, and flatly spreading in an oven at the temperature of not more than 60 ℃ for drying. Finally, the color change of the sample and the staining of the lining fabric are evaluated by a gray card. The fade and stain fastnesses were rated 5, the best on grade 5 and the worst on grade 1. The test results are shown in Table 1.
Table 1: and (5) color fastness test results.
From the results, the color fastness of comparative example 1 was poor in the environments of sweat alkali and sea water, and a distinct blue color appeared on the lining fabric. In examples 1-3, the color fastness is good under various test conditions, and the adhesive lining fabric has no obvious staining phenomenon after the test, which shows that the color fastness of the final product can be effectively improved by adding EVA into the color master batch carrier.
The above description is only exemplary of the present invention and is not intended to limit the scope of the present invention, which is defined by the claims appended hereto, as well as the appended claims.
Claims (9)
1. The preparation method of the color master batch for the polyamide with high color fastness and low melting point is characterized by adding 60-95 parts by weight of carrier, 4-40 parts by weight of colorant and 0.1-7 parts by weight of dispersant into a mixer for uniform mixing, carrying out melt blending by a double screw extruder at 200-230 ℃, and then carrying out granulation to prepare the color master batch for the polyamide with high color fastness and low melting point;
wherein the carrier is made of a low melting point copolyamide and an ethylene-vinyl acetate copolymer;
the low melting copolyamide is made from the following components:
caprolactam 30-40 parts
10-20 parts of nylon 66 salt
50-60 parts of diacid and diamine;
wherein the molar ratio of diacid to diamine is 1: 0.9 to 1.1, the melting point of the low-melting-point copolyamide is 105 to 120 ℃.
2. The preparation method of the color master batch for the polyamide with high color fastness and low melting point according to claim 1, wherein the weight part ratio of the low melting point copolyamide to the ethylene-vinyl acetate copolymer is 3-9: 1.
3. the method of claim 1, wherein the diacid is one or more of adipic acid, sebacic acid, undecanedioic acid, and dodecanedioic acid.
4. The process for preparing a color masterbatch for high-colorfastness low-melting polyamide according to claim 1 wherein said diamine is decamethylene diamine and/or dodecane diamine.
5. The method for preparing the color master batch for the polyamide with high color fastness and low melting point according to claim 1, wherein the molecular weight of the ethylene-vinyl acetate copolymer is 1000-10000.
6. The preparation method of the color master batch for the polyamide with high color fastness and low melting point according to claim 1, wherein the content of vinyl acetate part in the ethylene-vinyl acetate copolymer is 20-40%.
7. The method of preparing a color masterbatch for high-colorfastness low-melting polyamide as claimed in claim 1, wherein said colorant comprises phthalocyanine organic pigment, anthraquinone organic pigment, solvent type dye.
8. The method for preparing the color master batch for the polyamide with high color fastness and low melting point according to claim 1, wherein the dispersing agent is one or more of polyethylene glycol, metal stearate, aluminum-titanium composite coupling agent and trimethylolethane.
9. The process for preparing a color masterbatch for high-colorfastness low-melting polyamide according to claim 1, characterized in that the process for preparing the low-melting copolyamide comprises the following steps: adding caprolactam, nylon 66 salt, diacid and diamine into a reaction kettle according to a ratio, introducing nitrogen to replace air in the reaction kettle, gradually heating to 210-230 ℃, carrying out polymerization reaction under the protection of nitrogen, gradually increasing the pressure to 0.8-1.2 MPa along with the reaction, keeping the pressure for 0.5-1.5 h, then unloading the pressure of the reaction kettle to normal pressure within 1h, then carrying out reaction for 2-4 h for discharging, then carrying out granulation by a granulator after passing through a cooling water tank, then soaking for 12-18 h by cold water, and then drying for 20-30 h in an oven at 75-85 ℃.
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| 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 |
| 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 |
| 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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