CN115418111B - Flow grain master batch, flow grain material and preparation method - Google Patents
Flow grain master batch, flow grain material and preparation method Download PDFInfo
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- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- C08J2400/00—Characterised by the use of unspecified polymers
- C08J2400/12—Polymers characterised by physical features, e.g. anisotropy, viscosity or electrical conductivity
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- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/06—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
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- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention discloses a flow grain master batch, a flow grain material and a preparation method thereof, and relates to the field of polymer materials. The flow line master batch comprises the following components in parts by weight: LCP resin: 70-85 parts; PET resin: 3-8 parts; and (3) a compatilizer: 3-7 parts; coloring agent: 9-15 parts; the melt flow rate of the compatibilizer is 0.5-8g/10min measured at 190℃and 2.16 kg. According to the method, the Liquid Crystal Polymer (LCP) master batch and the PA66 material are mixed and injection molded by using different melting points of the LCP master batch and the PA66 material, so that the high-temperature liquid crystal polymer is softened and dispersed in the low-temperature PA66 material, different colorants are selected, the liquid crystal polymer with different colors is special, the liquid crystal polymer effect is realized after injection molding, the traditional spraying, silk screen printing and other processes can be replaced, and the cost is lower and the processing process is more environment-friendly.
Description
Technical Field
The invention relates to the field of polymer materials, in particular to a flow grain master batch, a flow grain material and a preparation method thereof.
Background
The PA66 is also called nylon 66, polyamide 66 or nylon 66, is formed by mutually and alternately polycondensing hexamethylenediamine molecules and adipic acid molecules, has excellent heat resistance and mechanical property, has the characteristics of high strength and high impact resistance, and can be widely applied to the related fields of aerospace, automobiles, electronics, electric appliances, buildings, body-building equipment, electric tools, industrial components, agricultural machinery and the like.
Because of the ultrahigh heat resistance of the PA66, the processing temperature of the PA66 is required to be 260 ℃ or above, the flow grain master batch is completely melted in the PA66 material at a higher temperature, the flow grain effect cannot occur, and the application of the PA66 material in the flow grain material product is limited because of the fact that the flow grain master batch applied to the PA66 material is rarely available in the market at present.
Disclosure of Invention
The invention provides a flow grain master batch, a flow grain material and a preparation method thereof, which are used for solving the technical problem that the flow grain material is difficult to produce due to the fact that the processing temperature of the current PA66 material is too high.
In order to solve the technical problems, one of the purposes of the invention is to provide a flow line master batch which comprises the following components in parts by weight:
LCP resin: 70-85 parts;
PET resin: 3-8 parts;
and (3) a compatilizer: 3-7 parts;
coloring agent: 9-15 parts;
the melt flow rate of the maleic anhydride grafted ethylene-octene copolymer elastomer is 0.5-8g/10min measured at 190 ℃ under 2.16kg and astm d-1238 standard. .
By adopting the scheme, the flow grain master batch has higher melting point, can adapt to the high-temperature processing condition of PA66, and selects different colorants to achieve the special effect of flow grains with different colors, so that the high-temperature flow grain master batch is softened and dispersed in the low-temperature PA66 material, and the appearance of a molded part is in a flow grain shape after injection molding; the melting point of the LCP resin in the flow grain master batch is obviously higher than that of PA66, insoluble plaques can appear in a PA66 system at the temperature of more than 280 ℃, and the PET resin is used for modifying the LCP resin, so that the melting point of the flow grain master batch is reduced to the temperature at which flow grains can be softened in the PA66 system, and the flow grain master batch is prevented from being completely dissolved or insoluble blocks appear in the PA66 system, and the flow grain effect is generated.
Preferably, the colorant is one or more of white pigment, black pigment, red pigment, yellow pigment, blue pigment and cyan-blue pigment.
Preferably, the colorant is one or more of colorant a, colorant b and colorant c; the colorant a is prepared from white pigment, yellow pigment, blue pigment and cyan pigment according to the mass ratio of (3-8): (5-12): (12-18) compounding (0-2); the colorant b is compounded by white pigment and yellow pigment according to the mass ratio of (3-8) (13-21); the colorant c is compounded by white pigment, black pigment, yellow pigment and red pigment according to the mass ratio of (8-12): (0-2): (3-8): (2-5).
As a preferable scheme, the colorant a is compounded by vulcanized HD-S, 2GTI, 4702PG and K7104LW according to the mass ratio of 5:8:15:1; the colorant b is prepared from zinc sulfide HD-S, 2GTI and Yellow K1310 according to the mass ratio of 5:15:2, compounding; the colorant c is prepared from zinc sulfide HD-S, M717, YELLOWK1310 and Oracet cube Red350 FA according to the mass ratio of 10:1:5: and 3, compounding.
Preferably, the compatilizer is a maleic anhydride grafted ethylene-octene copolymer elastomer.
Preferably, the melting point of the flow grain master batch is 260-280 ℃.
As a preferable scheme, the intrinsic viscosity of the PET resin is 0.50-1.20dl/g, and the PET resin is detected by using GB/T14190-2008 fiber grade polyester chip (PET) test method.
As a preferable scheme, the anti-oxidant also comprises 0.3 to 5 parts by weight of anti-oxidant, wherein the anti-oxidant is one or more of phenols, phosphites, sulfur-containing antioxidants and amine antioxidants.
In order to solve the technical problems, a second object of the present invention is to provide a method for preparing a master batch with flow patterns, comprising the following steps:
(1) Mixing LCP resin, PET resin, compatilizer, colorant and other components in a mixer for 3-5 min;
(2) Putting the uniformly mixed materials into double-screw extrusion equipment, extruding and granulating after mixing, melting and homogenizing, wherein the length-diameter ratio of an extrusion screw of the extrusion equipment is 48:1-65:1, the temperature of a charging barrel of the extrusion equipment is 270-290 ℃, the rotating speed of a host machine is 500-700 r/min, and cooling to obtain the flow grain master batch.
In order to solve the technical problems, the invention provides a flow grain material, wherein the flow grain master batch and the PA66 are prepared according to the mass ratio of (8-15): (85-92) compounding; the melt flow rate of PA66 was determined to be 70-270g/10min at 275℃under 2.16kg and GB/T3682 standards.
Through adopting above-mentioned scheme, this application utilizes the melting point difference of LCP masterbatch and PA66 material, lets the flow line masterbatch of high temperature soften the dispersion in PA66 material of low temperature, and the colorant in the flow line masterbatch makes the finished piece outward appearance after moulding plastics become the flow line form, can replace traditional spraying and processes such as silk screen printing, and the cost is lower processing technology more environmental protection.
In order to solve the technical problems, the fourth object of the present invention is to provide a method for preparing a flow pattern material, comprising the following steps: adding the flow line master batch into PA66 resin, uniformly mixing, and then injection molding, wherein the injection molding temperature is 250-270 ℃, the injection molding back pressure is 0-0.5MPa, and the injection molding pressure is 40-60MPa, so as to obtain the flow line material.
In order to solve the technical problems, the fifth object of the present invention is to provide an application of the moire material in the housing of home appliances and electronic and electric products, such as the housing of electric cooker, the panel of air conditioner, the housing of charger, the housing of absorber, etc.
Compared with the prior art, the embodiment of the invention has the following beneficial effects:
the method has the advantages that the flow grain master batch and the PA66 material are different in melting point, the high-temperature flow grain master batch is softened and dispersed in the low-temperature PA66 material, different colorants are selected, the flow grain special effect of different colors is achieved, the flow grain effect is achieved after injection molding, the traditional spraying, silk screen printing and other processes can be replaced, and the cost is lower and the processing process is more environment-friendly.
Drawings
Fig. 1: photographing the surface of a material with flow marks in the first embodiment of the invention;
fig. 2: photographing the surface of one of the flow line materials in the fourth embodiment of the invention;
fig. 3: photographing the surface of one of the flow line materials in the fifth embodiment of the invention;
fig. 4: photographing the surface of one of the flow line materials in the fourth comparative example;
fig. 5: photographing the surface of one of the flow line materials in the fifth comparative example;
fig. 6: the results of photographing the surface of one of the flow mark materials of the comparative example one of the present invention were obtained.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Table 1 below shows the sources of the raw materials in the examples and comparative examples of the present application, and the hindered phenol antioxidants were obtained commercially, and the same hindered phenol antioxidants were used in parallel experiments, unless otherwise specified.
TABLE 1 sources and Properties of raw materials in examples and comparative examples of the present application
Preparation examples 1 to 6
The flow line master batch comprises the components shown in table 2, wherein the components comprise LCP resin, PET resin, compatilizer, hindered phenol antioxidant and colorant; the compatilizer is maleic anhydride grafted ethylene-octene copolymer elastomer; the antioxidant is 1098; the colorant comprises one or more of colorant a, colorant b, and colorant c; colorant a included zinc sulfide HD-S, 2GTI, 4702PG, and K7104LW in a mass ratio of 5:8:15:1; the colorant b comprises a mass ratio of 5:15: zinc sulfide HD-S, 2GTI, and Yellow K1310; the colorant c comprises a mass ratio of 10:1:5:3, zinc sulfide HD-S, M717, YELLOWK1310 and Oracet cube Red350 FA; the hindered phenol antioxidant is 1098.
The preparation method of the flow line master batch comprises the following steps:
(1) Sufficiently drying the LCP resin and the PET resin by a hot air drying box at the drying temperature of 120 ℃ for 1 hour;
(2) Weighing the raw materials according to the proportion, and mixing the LCP resin, the PET resin, the compatilizer, the antioxidant and the colorant in a mixer for 5min;
(3) The evenly mixed materials are put into a double-screw extruder, extrusion granulation is carried out after mixing, melting and homogenization, the length-diameter ratio of extrusion screws of the double-screw extruder is 52:1, the material barrel of the extruder is 280 ℃, the rotating speed of a host machine is 600r/min, and flow line master batches are obtained after cooling, and the melting points are shown in table 2 according to the measurement of ISO 11357-1/-3 standard.
TABLE 2 flow line master batches of Components content and melting Point in preparation examples 1 to 6 and comparative preparation examples 1 to 6
Examples 1 to 6 and comparative examples 1 to 10
The flow line material comprises the following components in percentage by mass (85-92): PA66 and flow line master batch of (8-15), comprising the following preparation steps: and adding the flow grain master batch obtained in the preparation example or the comparative preparation example into PA66 resin, uniformly mixing, and then injection molding at the injection molding temperature of 260 ℃ and the injection molding back pressure of 0.3MPa and the injection molding pressure of 50 MPa to obtain the flow grain material with the flow grain effect on the surface.
TABLE 3 Components and contents in examples 1-6 and comparative examples 1-10
Performance test
1. Flow line effect: according to the combination of the flow mark effect and the sensory evaluation of the surface of the injection molding product, the evaluation results are shown in table 4, and the evaluation standards are as follows:
A. the flow lines are clear, have layering effect and have good evaluation grade, as shown in figures 1-3;
B. the streak lines are slightly blurred, the layering sense is not strong, and the evaluation grade is general, as shown in fig. 6;
C. no moire effect, rated poor, as shown in fig. 4-5.
2. Non-meltable particulate evaluation criteria: infusible particulate matter refers to plaque like particulate matter on the surface as shown in fig. 4-5.
TABLE 4 Performance test results for examples 1-6 and comparative examples 1-10
As can be seen from the performance test results of example 1 and comparative example 1 in table 4, the PET resin added to the flow line master batch can lower the melting point of the LCP, and the content of the PET resin is too high to make the melting point of the master batch close to or lower than that of PA66, so that the master batch is compatible in PA66 and cannot generate the flow line effect, while the content of the PET resin is too low to cause the melting point of the LCP to be too high, so that the master batch can generate insoluble matters in PA66, and therefore, the melting point of the flow line master batch is improved by using the PET resin, so that the melting point of the flow line master batch is higher than that of PA66, and the temperature of the master batch is higher than that of PA66, so that the flow line effect is softened in a PA66 system, and the insoluble matters cannot occur.
As can be seen from the performance test results of example 1 and comparative examples 2-3 in Table 4, the melting points of the LCP master batch and the PA66 material are different, so that the high-temperature flow grain master batch is softened and dispersed in the low-temperature PA66 material, the appearance of the molded part is in a flow grain effect after injection molding, and the melting point of the resin in the master batch is too low or the addition amount of the LCP resin is too small, so that the melting point of the final flow grain master batch is reduced, and the material is completely dissolved in the PA66 injection molding process, so that the flow grain effect cannot be generated.
As can be seen from the results of the performance tests of example 1 and comparative example 4 in table 4, the content of the LCP resin is critical, and since the melting point of the LCP resin is too high, modification by the PET resin is required to lower the melting point, the content of the LCP resin is too high, insoluble plaques appear in the PA66 system, and the flow lines remain worse and disappear when the content is too low.
As is clear from the results of the performance tests of example 1 and comparative examples 5 to 6 in Table 4, the melt index of the compatibilizer affects the flow effect of the product, and the melt index is too high, the compatibility of the material is better, and the flow effect is general when the flow is easily lost.
As can be seen from the performance test results of example 1 and comparative examples 7-8 in Table 4, too high or too low an addition ratio of the flow mark master batch in the PA66 material system affects the flow mark effect of the product, and insoluble plaques appear when the content is too high, the flow mark is poor to keep and vanish when the content is too low.
As is clear from the results of performance tests of example 1 and comparative examples 9 to 10 in Table 4, too low a melt index of the PA66 material body affects the flow pattern effect of the product, and too low a melt index of PA66 is poor in fluidity, the flow pattern is poor to remain, and the flow pattern disappears.
The foregoing embodiments have been provided for the purpose of illustrating the general principles of the present invention, and are not to be construed as limiting the scope of the invention. It should be noted that any modifications, equivalent substitutions, improvements, etc. made by those skilled in the art without departing from the spirit and principles of the present invention are intended to be included in the scope of the present invention.
Claims (7)
1. The flow line master batch is characterized by comprising the following components in parts by weight:
LCP resin: 70-85 parts;
PET resin: 3-8 parts;
and (3) a compatilizer: 3-7 parts;
coloring agent: 9-15 parts;
the melt flow rate of the compatilizer is 0.5-8g/10min at 190 ℃ in 2.16kg, the compatilizer is a maleic anhydride grafted ethylene-octene copolymer elastomer, and the melting point of the flow grain master batch is 260-280 ℃.
2. A flowline master as claimed in claim 1 wherein the colourant is one or more of colourant a, colourant b and colourant c; the colorant a is prepared from white pigment, yellow pigment, blue pigment and cyan pigment according to the mass ratio of (3-8): (5-12): (12-18) compounding (0-2); the colorant b is compounded by white pigment and yellow pigment according to the mass ratio of (3-8) (13-21); the colorant c is compounded by zinc sulfide white pigment, black pigment, yellow pigment and red pigment according to the mass ratio of (8-12): (0-2): (3-8): (2-5).
3. The flow mark master batch according to claim 1, further comprising 0.3-5 parts by weight of an antioxidant, wherein the antioxidant is one or more of phenols, phosphites, sulfur-containing antioxidants and amine antioxidants.
4. A method for preparing the flow mark master batch according to any one of claims 1 to 3, comprising the steps of:
(1) Mixing LCP resin, PET resin, compatilizer, colorant and other components in a mixer for 3-5 min;
(2) Putting the uniformly mixed materials into double-screw extrusion equipment, extruding and granulating after mixing, melting and homogenizing, wherein the length-diameter ratio of an extrusion screw of the extrusion equipment is 48:1-65:1, the temperature of a charging barrel of the extrusion equipment is 270-290 ℃, the rotating speed of a host machine is 500-700 r/min, and cooling to obtain the flow grain master batch.
5. A flow mark material, which is characterized by comprising the flow mark master batch according to any one of claims 1-3 and PA66 according to the mass ratio (8-15): (85-92) and the melt flow rate of the PA66 is 70-270g/10min at 275 ℃ and 2.16 kg.
6. A method of producing a flow mark material according to claim 5, comprising the steps of: adding the flow line master batch into PA66 resin, uniformly mixing, and then injection molding, wherein the injection molding temperature is 250-270 ℃, the injection molding back pressure is 0-0.5MPa, and the injection molding pressure is 40-60MPa, so as to obtain the flow line material.
7. Use of the flow mark material according to claim 5 in home appliance housings and electronic and electric products.
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| CN114634636A (en) * | 2022-02-22 | 2022-06-17 | 金发科技股份有限公司 | Color master batch with fluorescent flow pattern effect and preparation method and application thereof |
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