CN110883975A - Preparation method of low-roughness high-CTI-value flame-retardant polyamide composite material - Google Patents
Preparation method of low-roughness high-CTI-value flame-retardant polyamide composite material Download PDFInfo
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- CN110883975A CN110883975A CN201911077974.9A CN201911077974A CN110883975A CN 110883975 A CN110883975 A CN 110883975A CN 201911077974 A CN201911077974 A CN 201911077974A CN 110883975 A CN110883975 A CN 110883975A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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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
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/047—Reinforcing macromolecular compounds with loose or coherent fibrous material with mixed fibrous material
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
-
- 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
- B29C2948/92514—Pressure
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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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/9258—Velocity
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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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
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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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92809—Particular value claimed
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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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
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
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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
- C08K5/49—Phosphorus-containing compounds
- C08K5/5399—Phosphorus bound to nitrogen
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-containing compounds
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
Abstract
The application discloses a preparation method of a low-roughness high-CTI-value flame-retardant polyamide composite material, which sequentially comprises the following steps: s1, preparing the following raw materials in parts by weight: 30-70 parts of semi-aromatic polyamide, 5-30 parts of composite flame retardant, 2-15 parts of flame retardant synergist, 5-30 parts of potassium titanate whisker, 5-30 parts of boron nitride whisker, 0.1-5 parts of antioxidant and 0.1-5 parts of lubricant; s2, mixing the semi-aromatic polyamide, the antioxidant and the lubricant through a high-speed mixer, then feeding the mixture through a main feeder from a main feed opening of a double-screw extruder, mixing the composite flame retardant and the flame-retardant synergist, then feeding the mixture through the main feeder from the main feed opening of the double-screw extruder, respectively feeding the potassium titanate whiskers and the boron nitride whiskers through a vibrating feeder from a first side feed opening and a second side feed opening of the double-screw extruder, and carrying out melt mixing extrusion granulation. Compared with the traditional glass fiber reinforced red phosphorus flame-retardant PA66 material, the prepared composite material has the advantages of lower surface roughness and higher CTI value.
Description
Technical Field
The invention relates to the field of engineering plastic composite materials, in particular to a preparation method of a low-roughness high-CTI-value flame-retardant polyamide composite material.
Background
With the development of science and technology, the safety of human life is more and more focused by society, in order to improve the safety reliability of electronic products, especially the safety reliability of insulating materials used in humid environment, the index of high CTI (comparative tracking index) is more and more important, especially in the field of polyamide materials commonly used for electrical parts at present, when the surface of the material is humid and has impurities, and under the action of a higher electric field, the surface of the material forms a conductive circuit due to carbonization, and finally equipment short circuit or even fire is caused, so that the preparation of polyamide engineering plastics with high CTI value has a very positive significance. At present, the common preparation method of the polyamide material with the high CTI value is to add halogen-free phosphorus-nitrogen flame retardants such as red phosphorus master batches and melamine urate into polyamide, or inorganic flame retardants such as aluminum hydroxide and magnesium hydroxide or halogenated flame retardants such as brominated polystyrene and corresponding flame retardant synergists, and utilize the gas-phase or solid-phase flame retardant mechanism of the flame retardants to improve the heat resistance of the material, absorb the heat generated by leakage current, reduce the generation and accumulation of free carbon, further reduce the flashover discharge chance of the surface of the material and improve the CTI value of the material.
The existing polyamide material with a high CTI value has various problems, in particular to the problems of hydrogen phosphide toxic gas and color matching limitation (black-red limitation), high surface roughness and unstable CTI value of a glass fiber reinforced flame-retardant polyamide material during extrusion processing of a red phosphorus master batch flame-retardant formula.
Disclosure of Invention
According to the invention, semi-aromatic polyamide is used as matrix resin, a composite flame retardant (a halogen-free organic phosphinate and phosphazene flame retardant composite type) is added, and white potassium titanate whiskers and boron nitride whiskers are used as filling and reinforcing materials, so that the prepared composite material has lower surface roughness and higher CTI value compared with the traditional glass fiber reinforced red phosphorus flame retardant PA66 material.
In order to achieve the above object, the present invention provides the following technical solutions.
The embodiment of the application discloses a preparation method of a low-roughness high-CTI-value flame-retardant polyamide composite material, which sequentially comprises the following steps:
the method sequentially comprises the following steps:
s1, preparing the following raw materials in parts by weight: 30-70 parts of semi-aromatic polyamide, 5-30 parts of composite flame retardant, 2-15 parts of flame retardant synergist, 5-30 parts of potassium titanate whisker, 5-30 parts of boron nitride whisker, 0.1-5 parts of antioxidant and 0.1-5 parts of lubricant;
s2, mixing the semi-aromatic polyamide, the antioxidant and the lubricant through a high-speed mixer, then feeding the mixture through a main feeder from a main feed opening of a double-screw extruder, mixing the composite flame retardant and the flame-retardant synergist, then feeding the mixture through the main feeder from the main feed opening of the double-screw extruder, respectively feeding the potassium titanate whiskers and the boron nitride whiskers through a vibrating feeder from a first side feed opening and a second side feed opening of the double-screw extruder, and carrying out melt mixing extrusion granulation.
Preferably, in the preparation method of the low-roughness high-CTI-value flame-retardant polyamide composite material, the semi-aromatic polyamide is one or more of PA6T, PA9T, PA10T, PA11T, PA12T and a copolymerization modification product thereof.
Preferably, in the preparation method of the low-roughness high-CTI-value flame-retardant polyamide composite material, the composite flame retardant is prepared by compounding aluminum diethylphosphinate and hexaphenoxycyclotriphosphazene according to the mass ratio of 1: 1-2: 1.
Preferably, in the preparation method of the low-roughness high-CTI-value flame-retardant polyamide composite material, the flame-retardant synergist is one or more of zinc borate, zinc stannate, antimony trioxide, zinc oxide, calcium oxide, zinc sulfide and magnesium sulfide.
Preferably, in the preparation method of the low-roughness high-CTI-value flame-retardant polyamide composite material, the boron nitride whiskers are boron nitride fibers subjected to surface treatment by a coupling agent, the fiber length is 20-50 μm, and the diameter is 0.1-5 μm.
Preferably, in the preparation method of the low-roughness high-CTI-value flame-retardant polyamide composite material, the antioxidant is IRGANOX 168 and 1098.
Preferably, in the preparation method of the low-roughness high-CTI flame-retardant polyamide composite material, the lubricant is one or more of pentaerythritol stearate, aliphatic metal salt and organic silicone powder.
Preferably, in the preparation method of the low-roughness high-CTI-value flame-retardant polyamide composite material, the rotating speed of the rotary mixer is 60-120 rpm, the mixing time is 5-10 min, the output of the double-screw extruder is 50-200 Kg/h, the rotating speed is 100-300 rpm, the temperature of the machine barrel is 300 +/-20 ℃, the temperature of the machine head is 310 +/-10 ℃, and the extraction pressure of a vacuum section is-0.08 +/-0.02 MPa.
The invention has the advantages that semi-aromatic polyamide is adopted as matrix resin, the composite flame retardant (halogen-free organic phosphinate and phosphazene flame retardant composite type) is added, the white potassium titanate whisker and the boron nitride whisker are used as filling and reinforcing materials, and the prepared composite material has lower surface roughness and higher CTI value compared with the traditional glass fiber reinforced red phosphorus flame retardant PA66 material.
Detailed Description
Technical solutions in the embodiments of the present invention will be described in detail below, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
An exemplary illustration of 2 sets of examples is provided below, and the examples are compared to a typical comparative example (PA 66/30% GF/red phosphorus) for performance.
The preparation method of the embodiment 1 and the embodiment 2 is the same, but the components are different in content, and the preparation method comprises the following steps: mixing the semi-aromatic polyamide, the antioxidant and the lubricant through a high-speed mixer, then feeding the mixture from a main feed opening of a double-screw extruder through a main feeder, then mixing the composite flame retardant and the flame-retardant synergist through the main feeder, then feeding the mixture from the main feed opening of the double-screw extruder through the main feeder, respectively feeding the potassium titanate whiskers and the boron nitride whiskers through a vibrating feeder from a first side feed opening and a second side feed opening of the double-screw extruder, and carrying out melt mixing extrusion granulation. The rotating speed of the rotary mixer is 60-120 rpm, the mixing time is 5-10 min, the output of the double-screw extruder is 50-200 Kg/h, the rotating speed is 100-300 rpm, the temperature of the machine barrel is 300 +/-20 ℃, the temperature of the machine head is 310 +/-10 ℃, and the extraction pressure of a vacuum section is-0.08 +/-0.02 MPa.
In the preparation method, the semi-aromatic polyamide is one or more of PA6T, PA9T, PA10T, PA11T, PA12T and copolymerization modifications thereof. The composite flame retardant is compounded by aluminum diethylphosphinate produced by Claine and hexaphenoxycyclotriphosphazene produced by Otsuka in a chemical manner according to the mass ratio of 1: 1-2: 1. The flame-retardant synergist is one or more of zinc borate, zinc stannate, antimony trioxide, zinc oxide, calcium oxide, zinc sulfide and magnesium sulfide. The potassium titanate whisker is of a TISMO D series produced by Japanese red-Density chemical products. The boron nitride whisker is boron nitride fiber subjected to surface treatment by a coupling agent, the fiber length is 20-50 mu m, and the diameter is 0.1-5 mu m. The antioxidant is IRGANOX 168, 1098 produced by BASF. The lubricant is one or more of pentaerythritol stearate, aliphatic metal salt and organic silicone powder.
The specific composition of examples 1 and 2 is shown in the following table:
the properties of examples 1-2 and of a typical comparative example (PA 66/30% GF/red phosphorus) were compared and the results were as follows:
| item | Example 1 | Example 2 | Comparative example |
| Tensile Strength (MPa) | 125 | 135 | 140 |
| Flexural Strength (MPa) | 175 | 180 | 190 |
| Surface roughness Ra (mum) | 0.512 | 0.517 | 1.561 |
| Flame-retardant rating UL941.6mm | V-0 | V-0 | V-0 |
| Relative creepage tracking index (V) | 500 | 550 | 450 |
The properties of the composite material prepared according to the invention are such that the surface roughness and CTI values exceed those of a typical comparative example (PA 66/30% GF/red phosphorus).
The present embodiments are to be considered as illustrative and not restrictive, and the scope of the patent is to be determined by the appended claims.
Claims (8)
1. A preparation method of a low-roughness high-CTI-value flame-retardant polyamide composite material is characterized by sequentially comprising the following steps of:
s1, preparing the following raw materials in parts by weight: 30-70 parts of semi-aromatic polyamide, 5-30 parts of composite flame retardant, 2-15 parts of flame retardant synergist, 5-30 parts of potassium titanate whisker, 5-30 parts of boron nitride whisker, 0.1-5 parts of antioxidant and 0.1-5 parts of lubricant;
s2, mixing the semi-aromatic polyamide, the antioxidant and the lubricant through a high-speed mixer, then feeding the mixture through a main feeder from a main feed opening of a double-screw extruder, mixing the composite flame retardant and the flame-retardant synergist, then feeding the mixture through the main feeder from the main feed opening of the double-screw extruder, respectively feeding the potassium titanate whiskers and the boron nitride whiskers through a vibrating feeder from a first side feed opening and a second side feed opening of the double-screw extruder, and carrying out melt mixing extrusion granulation.
2. The preparation method of the low-roughness high-CTI-value flame-retardant polyamide composite material as claimed in claim 1, wherein the semi-aromatic polyamide is one or more of PA6T, PA9T, PA10T, PA11T, PA12T and a copolymerization modification thereof.
3. The preparation method of the low-roughness high-CTI-value flame-retardant polyamide composite material as claimed in claim 1, wherein the composite flame retardant is prepared by compounding aluminum diethylphosphinate and hexaphenoxycyclotriphosphazene according to a mass ratio of 1: 1-2: 1.
4. The preparation method of the low-roughness high-CTI-value flame-retardant polyamide composite material as claimed in claim 1, wherein the flame-retardant synergist is one or more of zinc borate, zinc stannate, antimony trioxide, zinc oxide, calcium oxide, zinc sulfide and magnesium sulfide.
5. The preparation method of the low-roughness high-CTI-value flame-retardant polyamide composite material as claimed in claim 1, wherein the boron nitride whiskers are boron nitride fibers subjected to surface treatment by a coupling agent, the fiber length is 20-50 μm, and the diameter is 0.1-5 μm.
6. The method for preparing the low-roughness high-CTI-value flame-retardant polyamide composite material as claimed in claim 1, wherein the antioxidant is IRGANOX 168, 1098.
7. The preparation method of the low-roughness high-CTI flame-retardant polyamide composite material as claimed in claim 1, wherein the lubricant is one or more of pentaerythritol stearate, aliphatic metal salt and silicone powder.
8. The preparation method of the low-roughness high-CTI-value flame-retardant polyamide composite material as claimed in claim 1, wherein the rotating speed of the rotary mixer is 60-120 rpm, the mixing time is 5-10 min, the output of the double-screw extruder is 50-200 Kg/h, the rotating speed is 100-300 rpm, the barrel temperature is 300 +/-20 ℃, the head temperature is 310 +/-10 ℃, and the vacuum section extraction pressure is-0.08 +/-0.02 MPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911077974.9A CN110883975A (en) | 2019-11-06 | 2019-11-06 | Preparation method of low-roughness high-CTI-value flame-retardant polyamide composite material |
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| CN201911077974.9A CN110883975A (en) | 2019-11-06 | 2019-11-06 | Preparation method of low-roughness high-CTI-value flame-retardant polyamide composite material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113004688A (en) * | 2021-02-04 | 2021-06-22 | 张家港大塚化学有限公司 | Preparation process of high-performance polyamide composite material for halogen-free flame-retardant LED |
| CN114957985A (en) * | 2022-06-17 | 2022-08-30 | 张家港大塚化学有限公司 | Preparation method of microcapsule phosphazene flame retardant-based halogen-free flame-retardant polyamide composite material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113004688A (en) * | 2021-02-04 | 2021-06-22 | 张家港大塚化学有限公司 | Preparation process of high-performance polyamide composite material for halogen-free flame-retardant LED |
| CN114957985A (en) * | 2022-06-17 | 2022-08-30 | 张家港大塚化学有限公司 | Preparation method of microcapsule phosphazene flame retardant-based halogen-free flame-retardant polyamide composite material |
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Application publication date: 20200317 |