CN103740099A - PA6 compound with stable colorability and preparation method thereof - Google Patents

PA6 compound with stable colorability and preparation method thereof Download PDF

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Publication number
CN103740099A
CN103740099A CN201310743209.2A CN201310743209A CN103740099A CN 103740099 A CN103740099 A CN 103740099A CN 201310743209 A CN201310743209 A CN 201310743209A CN 103740099 A CN103740099 A CN 103740099A
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China
Prior art keywords
stable
mixing
tinctorial property
mixture
resin
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CN201310743209.2A
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Chinese (zh)
Inventor
刘正军
张祥福
周文
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Shanghai Pret Composites Co Ltd
Zhejiang Pret New Materials Co Ltd
Chongqing Pret New Materials Co Ltd
Original Assignee
Shanghai Pret Composites Co Ltd
Zhejiang Pret New Materials Co Ltd
Chongqing Pret New Materials Co Ltd
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Priority to CN201310743209.2A priority Critical patent/CN103740099A/en
Publication of CN103740099A publication Critical patent/CN103740099A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/04—Particle-shaped
    • 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
    • C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/9258—Velocity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/9258—Velocity
    • B29C2948/9259—Angular velocity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92742—Optical properties
    • B29C2948/92752—Colour
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92761—Mechanical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92885—Screw or gear
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895—Barrel or housing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/9298—Start-up, shut-down or parameter setting phase; Emergency shut-down; Material change; Test or laboratory equipment or studies

Landscapes

  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Abstract

The invention discloses a PA6 compound with stable colorability and a preparation method thereof. The PA6 compound comprises the following raw materials by weight percent: 90-98% of PA6 resin, 0.5-5% of inorganic mineral, 0.1-3% of antioxidant and 0.5-10% of other auxiliaries. The preparation method comprises the steps of mixing the inorganic mineral, the antioxidant and other auxiliaries in a high-speed mixer for 3-5 minutes, then mixing the mixture with the PA6 resin in a common mixer for 5-10 minutes, then adding the uniformly mixed materials to a double-screw extruder, controlling the processing temperature to be 220-250 DEG C and the rotational speed of the main machine to be 20-50Hz, and then preparing various required products with a plastic injection molding machine. The aim of uniformly dispersing colorants to keep the colors consistent is achieved by mixing the colorants with the mineral powder in advance. The product has the beneficial effects of stable color, excellent performance, easiness in processing and good surface gloss.

Description

A kind of PA6 mixture with stable tinctorial property and preparation method thereof
Technical field
The present invention relates to a kind of PA6 matrix material, be specially a kind of PA6 mixture with stable tinctorial property and preparation method thereof, belong to polymer composite field.
Background technology
It is to use as chemical fibre that PA6 resin starts most, but because it has excellent processing characteristics and mechanical property, is applied to widely the industries such as automobile, electronic apparatus as engineering plastics.
Along with going deep into of PA6 resin application, the tinctorial property of PA6 requires more and more higher.Because PA6 is as hypocrystalline engineering plastics, processing temperature is high, can be used for the toner kind of dyeing limited, adds that the PA6 mobility of molten state is fine, causes with the bond properties of toner poorly, often occurs the phenomenon of aberration or color shakiness.
Based on this reason, related personnel has carried out a lot of research.Noriyoshi Watanabe improves the retention of color of PA66 in USP.5412013 by mantoquita, aramid fiber; Gerardus P.T.Vonk is less than 20% PA6 at USP.5674968 middle-end amino and improves retention of color; Rolando Umali Pagilagan etc. adds nylon to and improves colour stability in synthetic with phosphoric acid salt at USP.6191251.
By oxidation inhibitor and other auxiliary agents, can promote the painted stability of PA6, but in actual applications, color is unstable or often occur, and illustrate that simple these auxiliary agents of interpolation can not address this problem completely.
Summary of the invention
Goal of the invention of the present invention is for a kind of PA6 mixture with stable tinctorial property is provided, to reduce the colour-change of even eliminating in injection moulding process.
Another object of the present invention is for the preparation method of above-mentioned matrix material is provided.
Object of the present invention can be achieved by the following technical programs.
A PA6 mixture with stable tinctorial property, is comprised of the raw material of following weight percent:
Figure BDA0000449102060000021
In the PA6 mixture with stable tinctorial property of the present invention, PA6 resin is the open loop polycondensate of hexanolactam, and its relative viscosity number is 2.0～3.0.
In the PA6 mixture with stable tinctorial property of the present invention, inorganic mineral is that one or more in glass microballon, talcum powder, calcium carbonate, wollastonite, kaolin and clay are mixed, and its diameter is less than 100 microns.
In the PA6 mixture with stable tinctorial property of the present invention, oxidation inhibitor is phenols and phosphinate composite antioxidant, and its ratio is 1/5～5/1.
In the PA6 mixture with stable tinctorial property of the present invention, other auxiliary agents are one or more mixing in silane coupling agent, tinting material, fire retardant and lubricant.
Prepare the above-mentioned method with the PA6 mixture of stable tinctorial property, concrete steps are as follows:
1) the various materials that take by above-mentioned component proportioning;
2) by the inorganic mineral taking, oxidation inhibitor and other auxiliary agents at high speed mixer mixing 3-5 minute, then in common mixing machine, mix 5-10 minute with the PA6 resin weighing up, then the material mixing is added to twin screw extruder, processing temperature is at 220～250 ℃, engine speed is 20～50 hertz, then with injection molding machine of plastic, makes various desired products.
The present invention, by tinting material and breeze are mixed in advance, reaches the target that dispersed tinting material keeps solid colour.The PA6 mixture colour stable with stable tinctorial property of the present invention, excellent performance, easily processing, surface luster is good.
Embodiment
Below by embodiment and comparative example, further illustrate the present invention, do not violating under aim of the present invention, the present invention should be not limited to the content that following experimental example is specifically expressed.
Embodiment and comparative example raw materials are as follows:
PA6 resin, M2000, Xin Hui Meida Company;
PA6 resin, M2500, Xin Hui Meida Company;
PA6 resin, YH800, Yueyang petro-chemical corporation;
Talcum powder, HTP2, Italian IMIFABI
Wollastonite, HJ2000-3, Jiangxi Hua Jietai
Tinting material, zinc sulphide HD, German Sachtleben
Tinting material, transparent green, German Bayer
Tinting material, carbon black DL430, U.S. CABOT
Lubricant, OP wax, Switzerland Ke Laien
Oxidation inhibitor, 168 and 1010, Ciba fine chemicals.
Other auxiliary agents such as the breeze taking, oxidation inhibitor, tinting material, at high speed mixer mixing 3-5 minute, are then mixed to 5-10 minute with the PA6 resin weighing up in common mixing machine; The raw material mixing is placed in to dual-screw-stem machine, through melt extruding, granulation.By the section particle obtaining, in the convection oven of 105 ℃ after dry 4 hours, with day HT1150B injection moulding machine sample preparation of sea, Ningbo, injection moulding machine Temperature Setting is: first 245 ℃, in 240 ℃, latter 230 ℃.
Measurement of Material Mechanical Performance is tested according to iso standard: the batten of test tensile strength is 170*10*4mm, by ISO527-2, is undertaken, and speed is 50mm/min; The batten of test notched Izod impact strength is 80*10*4mm, by ISO179-1, undertaken, and v-notch, pendulum is 4J.
The chromatism test of material is according to spectrograph testing standard colour table and material colour table color difference (△ E) for DIN54001, and batten is 65 * 50 * 4mm colour table.
Embodiment 1～5
In mixture, various raw-material weight percents are as shown in table 1, and the temperature of twin screw extruder is respectively (from spout to extrusion die): 230 ℃, and 230 ℃, 235 ℃, 240 ℃, 245 ℃.Engine speed is 35 hertz.Injection moulding colour table carries out at twice, beats for the first time after colour table, keeps temperature, carries out injection moulding colour table for the second time after 30 minutes.
Table 1 embodiment 1-5 formula and material property table
Figure BDA0000449102060000051
Note: twice △ E value difference is apart from less, and the stability of account for color is better.
Comparative example 1-3:
In mixture, various raw-material weight percents are as shown in table 1, and other auxiliary agents such as the oxidation inhibitor taking, tinting material, at high speed mixer mixing 3-5 minute, are then mixed to 5-10 minute with the PA6 resin weighing up in common mixing machine; The raw material mixing is placed in to dual-screw-stem machine, through melt extruding, granulation.The temperature of twin screw extruder is respectively (from spout to extrusion die): 230 ℃, and 230 ℃, 235 ℃, 240 ℃, 245 ℃.Engine speed is 35 hertz.Injection moulding colour table carries out at twice, beats for the first time after colour table, keeps temperature, carries out injection moulding colour table for the second time after 30 minutes.
Table 1 comparative example 1-3 formula and material property table
Figure BDA0000449102060000052
Figure BDA0000449102060000061
Note: twice △ E value difference is apart from less, and the stability of account for color is better.
From the test result of embodiment and comparative example aberration, by the breeze toner that can effectively be scattered here and there, guarantee that aberration is stable, keep the stable with consistent of moulding color.

Claims (6)

1. a PA6 mixture with stable tinctorial property, is characterized in that: the raw material by following weight percent forms:
Figure FDA0000449102050000011
2. the PA6 mixture according to claim 1 with stable tinctorial property, is characterized in that: described PA6 resin is the open loop polycondensate of hexanolactam, and its relative viscosity number is 2.0～3.0.
3. the PA6 mixture according to claim 1 with stable tinctorial property, is characterized in that: described inorganic mineral is one or more mixing in glass microballon, talcum powder, calcium carbonate, wollastonite, kaolin and clay, and its diameter is less than 100 microns.
4. the PA6 mixture according to claim 1 with stable tinctorial property, is characterized in that: described oxidation inhibitor is phenols and phosphinate composite antioxidant, and its ratio is 1/5～5/1.
5. the PA6 mixture according to claim 1 with stable tinctorial property, is characterized in that: other described auxiliary agents are one or more mixing in silane coupling agent, tinting material, fire retardant and lubricant.
6. prepare a method described in claim 1 with the PA6 mixture of stable tinctorial property, it is characterized in that: concrete steps are as follows:
1) the various raw materials that take by above-mentioned component proportioning;
2) by the inorganic mineral taking, oxidation inhibitor and other auxiliary agents at high speed mixer mixing 3-5 minute, then in common mixing machine, mix 5-10 minute with the PA6 resin weighing up, then the material mixing is added to twin screw extruder, processing temperature is at 220～250 ℃, engine speed is 20～50 hertz, then with injection molding machine of plastic, makes various desired products.
CN201310743209.2A 2013-12-28 2013-12-28 PA6 compound with stable colorability and preparation method thereof Pending CN103740099A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11293106A (en) * 1998-04-09 1999-10-26 Mitsubishi Eng Plast Corp Reinforced polyamide resin composition
CN1269745A (en) * 1997-09-05 2000-10-11 巴斯福股份公司 Method for producing dyed moulding materials
CA2105566C (en) * 1991-03-06 2003-09-30 Carl E. Altman Heat stable film composition comprising polyepsiloncaprolactam
CN102492293A (en) * 2011-12-04 2012-06-13 上海金发科技发展有限公司 Low temperature resistance stained glass fiber reinforcement nylon 6 and preparation method thereof
CN102732018A (en) * 2012-07-03 2012-10-17 金发科技股份有限公司 Nylon 66 composite and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2105566C (en) * 1991-03-06 2003-09-30 Carl E. Altman Heat stable film composition comprising polyepsiloncaprolactam
CN1269745A (en) * 1997-09-05 2000-10-11 巴斯福股份公司 Method for producing dyed moulding materials
JPH11293106A (en) * 1998-04-09 1999-10-26 Mitsubishi Eng Plast Corp Reinforced polyamide resin composition
CN102492293A (en) * 2011-12-04 2012-06-13 上海金发科技发展有限公司 Low temperature resistance stained glass fiber reinforcement nylon 6 and preparation method thereof
CN102732018A (en) * 2012-07-03 2012-10-17 金发科技股份有限公司 Nylon 66 composite and preparation method thereof

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Application publication date: 20140423