CN111574828A - Nylon halogen-free flame-retardant master batch and preparation method thereof - Google Patents
Nylon halogen-free flame-retardant master batch and preparation method thereof Download PDFInfo
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- CN111574828A CN111574828A CN202010607819.XA CN202010607819A CN111574828A CN 111574828 A CN111574828 A CN 111574828A CN 202010607819 A CN202010607819 A CN 202010607819A CN 111574828 A CN111574828 A CN 111574828A
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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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- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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Abstract
The invention relates to the technical field of product detection, in particular to a nylon halogen-free flame-retardant master batch and a preparation method thereof, wherein the nylon halogen-free flame-retardant master batch comprises the following components: the flame retardant comprises polyamide, a flame retardant, an antioxidant, glass beads and silicate, wherein the content of the five components is as follows: polyamide: 30% -40%; flame retardant: 67% -30%; antioxidant: 1% -10%; glass beads: 1% -10%; silicate salt: 1% -10%. Compared with the traditional product, the invention can reach UL 94V-0 flame retardant level by higher addition ratio, the product addition ratio is lower, the deterioration of the mechanical property of the product is not obvious, and the product can also be used for sheet materials, plates and the like and has stronger practical application value.
Description
Technical Field
The invention relates to the technical field of product detection, in particular to a halogen-free flame-retardant nylon master batch and a preparation method thereof.
Background
In practical application, accessories such as corrugated pipes around engines of automobiles and high-speed rail vehicles, protective housings of electrical appliances and the like generally need to play roles in flame retardance, insulation and the like, so that safety of the engines, the electrical appliances and the like is improved powerfully, flame-retardant master batches are generally required to be added into the accessories to achieve a good flame-retardant effect, but the existing flame-retardant master batches often need to be added at a high addition ratio to achieve a UL 94V-0 flame-retardant level. In view of the above, we propose a nylon halogen-free flame-retardant master batch and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a halogen-free flame-retardant nylon master batch and a preparation method thereof, which are used for solving the problems in the background technology.
In order to achieve the purpose, the invention provides a nylon halogen-free flame-retardant master batch which comprises the following components: the flame retardant comprises polyamide, a flame retardant, an antioxidant, glass beads and silicate, wherein the content of the five components is as follows:
polyamide: 30% -40%;
flame retardant: 67% -30%;
antioxidant: 1% -10%;
glass beads: 1% -10%;
silicate salt: 1% -10%.
As a preferable technical scheme of the invention, the polyamide is selected from one of polyamide-6, polyamide-66 or polyamide-610.
As a preferred technical scheme of the invention, the material adopted by the flame retardant is powdery melamine cyanurate.
As the preferable technical scheme of the invention, the antioxidant is selected from one of zinc dialkyl dithiophosphate, zinc dialkyl dithiocarbamate, N-phenyl-alpha-naphthylamine and alkyl phenothiazine, benzotriazole derivatives or mercaptobenzothiazole derivatives.
As a preferable technical scheme of the invention, the magnetic particles in the glass beads do not exceed 0.1 percent of the total weight of the glass beads, and the content of bubbles in the glass beads is lower than 10 percent.
As the preferred technical scheme of the invention, the silicate is made of talcum powder.
The invention also provides a preparation method of the halogen-free flame-retardant nylon master batch, which comprises the following steps:
step one, material preparation: preparing five raw materials of polyamide, flame retardant, antioxidant, glass beads and silicate in advance according to a specified proportion;
step two, preliminary mixing: putting the five raw materials obtained in the first step into a high-speed stirrer for fully mixing to obtain a pasty fluid substance;
step three, secondary mixing: putting the pasty fluid substance obtained by mixing in the step two into a high-speed stirrer, and taking out after all the materials in the stirrer are uniformly mixed;
step four, granulation: putting the mixed materials into a double-screw extruder to extrude into strips, stretching the strips by a screw, a die head and a water tank, cooling the strips by the water tank, and preparing the strips into cylindrical granules or round granules by a granulator;
step five, packaging: and (3) putting the master batch which is made into cylindrical granules or round granules into a packaging bag, pumping air in the packaging bag to a vacuum state through an air pump, and then finishing the sealing of the packaging bag through a sealing machine to finally finish the product packaging.
As the preferable technical scheme of the invention, in the process of preliminary mixing of the materials in the step two, the stirring temperature is 30-60 ℃, the stirring speed is 6000-10000rpm, the stirring pressure is normal pressure, and the stirring time is controlled to be 3-10 min.
As the preferable technical scheme of the invention, the stirring temperature in the secondary mixing process of the materials in the step three is 0-20 ℃, the stirring speed is 6000-10000rpm, the stirring air pressure is normal pressure, and the stirring time is controlled to be 3-10 min.
As a preferable technical scheme of the invention, in the granulation process in the fourth step, the temperature of the feeding section of the double-screw extruder is controlled to be 220 ℃ C, the temperature of the melting section of the double-screw extruder is controlled to be 250 ℃ C, the temperature of the extrusion section of the double-screw extruder is controlled to be 240 ℃ C, and the air pressure in the three stages is normal pressure.
Compared with the prior art, the invention has the beneficial effects that:
compared with the traditional product, the invention can reach UL 94V-0 flame retardant level by higher addition ratio, the product addition ratio is lower, the deterioration of the mechanical property of the product is not obvious, and the product can also be used for sheet materials, plates and the like and has stronger practical application value.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and simplicity of description, and do not indicate or imply that the equipment or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the present invention.
The technical scheme provided by the invention is as follows:
example 1
The invention provides a nylon halogen-free flame-retardant master batch which comprises the following components: the flame retardant comprises polyamide, a flame retardant, an antioxidant, glass beads and silicate, wherein the content of the five components is as follows:
polyamide: 30 percent;
flame retardant: 67%;
antioxidant: 1 percent;
glass beads: 1 percent;
silicate salt: 1 percent.
In this example, polyamide-6 was used as the polyamide.
In this embodiment, the flame retardant is made of powdery melamine cyanurate.
In this example, zinc dialkyldithiophosphate was used as the antioxidant.
In this embodiment, the magnetic particles in the glass beads are not more than 0.1% of the total weight of the glass beads, and the content of bubbles in the glass beads is less than 10%.
In this embodiment, the silicate is talc.
The invention also provides a preparation method of the halogen-free flame-retardant nylon master batch, which comprises the following steps:
step one, material preparation: preparing five raw materials of polyamide, flame retardant, antioxidant, glass beads and silicate in advance according to a specified proportion;
step two, preliminary mixing: putting the five raw materials obtained in the first step into a high-speed stirrer for fully mixing to obtain a pasty fluid substance;
step three, secondary mixing: putting the pasty fluid substance obtained by mixing in the step two into a high-speed stirrer, and taking out after all the materials in the stirrer are uniformly mixed;
step four, granulation: putting the mixed materials into a double-screw extruder to extrude into strips, stretching the strips by a screw, a die head and a water tank, cooling the strips by the water tank, and preparing the strips into cylindrical granules or round granules by a granulator;
step five, packaging: and (3) putting the master batch which is made into cylindrical granules or round granules into a packaging bag, pumping air in the packaging bag to a vacuum state through an air pump, and then finishing the sealing of the packaging bag through a sealing machine to finally finish the product packaging.
In the embodiment, in the process of preliminary mixing of the materials in the second step, the stirring temperature is 30 ℃, the stirring speed is 6000rpm, the stirring pressure is normal pressure, and the stirring time is controlled to be 3 min.
In the embodiment, the stirring temperature in the secondary mixing process of the materials in the third step is 5 ℃, the stirring speed is 6000rpm, the stirring pressure is normal pressure, and the stirring time is controlled to be 3 min.
In the embodiment, in the granulation process in the fourth step, the temperature of the feeding section of the twin-screw extruder is controlled at 160 ℃, the temperature of the melting section of the twin-screw extruder is controlled at 220 ℃, the temperature of the extrusion section of the twin-screw extruder is controlled at 200 ℃, and the air pressure in the three stages is normal pressure.
Example 2
The invention provides a nylon halogen-free flame-retardant master batch which comprises the following components: the flame retardant comprises polyamide, a flame retardant, an antioxidant, glass beads and silicate, wherein the content of the five components is as follows:
polyamide: 35 percent;
flame retardant: 50 percent;
antioxidant: 5 percent;
glass beads: 5 percent;
silicate salt: 5 percent.
In this example, polyamide-66 was used as the polyamide.
In this embodiment, the flame retardant is made of powdery melamine cyanurate.
In this example, zinc dialkyldithiocarbamate was used as the antioxidant.
In this embodiment, the magnetic particles in the glass beads are not more than 0.1% of the total weight of the glass beads, and the content of bubbles in the glass beads is less than 10%.
In this embodiment, the silicate is talc.
The invention also provides a preparation method of the halogen-free flame-retardant nylon master batch, which comprises the following steps:
step one, material preparation: preparing five raw materials of polyamide, flame retardant, antioxidant, glass beads and silicate in advance according to a specified proportion;
step two, preliminary mixing: putting the five raw materials obtained in the first step into a high-speed stirrer for fully mixing to obtain a pasty fluid substance;
step three, secondary mixing: putting the pasty fluid substance obtained by mixing in the step two into a high-speed stirrer, and taking out after all the materials in the stirrer are uniformly mixed;
step four, granulation: putting the mixed materials into a double-screw extruder to extrude into strips, stretching the strips by a screw, a die head and a water tank, cooling the strips by the water tank, and preparing the strips into cylindrical granules or round granules by a granulator;
step five, packaging: and (3) putting the master batch which is made into cylindrical granules or round granules into a packaging bag, pumping air in the packaging bag to a vacuum state through an air pump, and then finishing the sealing of the packaging bag through a sealing machine to finally finish the product packaging.
In this embodiment, in the process of preliminary mixing of the materials in the second step, the stirring temperature is 45 ℃, the stirring speed is 8000rpm, the stirring pressure is normal pressure, and the stirring time is controlled to be 7 min.
In the embodiment, the stirring temperature in the secondary mixing process of the materials in the third step is 12 ℃, the stirring speed is 8000rpm, the stirring pressure is normal pressure, and the stirring time is controlled to be 7 min.
In the embodiment, in the granulation process in the fourth step, the temperature of the feeding section of the twin-screw extruder is controlled to be 190 ℃, the temperature of the melting section of the twin-screw extruder is controlled to be 235 ℃, the temperature of the extrusion section of the twin-screw extruder is controlled to be 220 ℃, and the air pressure in the three stages is normal pressure.
Example 3
The invention provides a nylon halogen-free flame-retardant master batch which comprises the following components: the flame retardant comprises polyamide, a flame retardant, an antioxidant, glass beads and silicate, wherein the content of the five components is as follows:
polyamide: 40 percent;
flame retardant: 30 percent;
antioxidant: 10 percent;
glass beads: 10 percent;
silicate salt: 10 percent.
In this example, polyamide-610 was used as the polyamide.
In this embodiment, the flame retardant is made of powdery melamine cyanurate.
In this example, the antioxidant was N-phenyl-alpha-naphthylamine.
In this embodiment, the magnetic particles in the glass beads are not more than 0.1% of the total weight of the glass beads, and the content of bubbles in the glass beads is less than 10%.
In this embodiment, the silicate is talc.
The invention also provides a preparation method of the halogen-free flame-retardant nylon master batch, which comprises the following steps:
step one, material preparation: preparing five raw materials of polyamide, flame retardant, antioxidant, glass beads and silicate in advance according to a specified proportion;
step two, preliminary mixing: putting the five raw materials obtained in the first step into a high-speed stirrer for fully mixing to obtain a pasty fluid substance;
step three, secondary mixing: putting the pasty fluid substance obtained by mixing in the step two into a high-speed stirrer, and taking out after all the materials in the stirrer are uniformly mixed;
step four, granulation: putting the mixed materials into a double-screw extruder to extrude into strips, stretching the strips by a screw, a die head and a water tank, cooling the strips by the water tank, and preparing the strips into cylindrical granules or round granules by a granulator;
step five, packaging: and (3) putting the master batch which is made into cylindrical granules or round granules into a packaging bag, pumping air in the packaging bag to a vacuum state through an air pump, and then finishing the sealing of the packaging bag through a sealing machine to finally finish the product packaging.
In this embodiment, in the process of preliminary mixing of the materials in the second step, the stirring temperature is 60 ℃, the stirring speed is 10000rpm, the stirring pressure is normal pressure, and the stirring time is controlled to be 10 min.
In this embodiment, the stirring temperature in the secondary mixing process of the materials in the third step is 20 ℃, the stirring speed is 10000rpm, the stirring pressure is normal pressure, and the stirring time is controlled to be 10 min.
In the embodiment, in the granulation process in the fourth step, the temperature of the feeding section of the twin-screw extruder is controlled at 220 ℃, the temperature of the melting section of the twin-screw extruder is controlled at 250 ℃, the temperature of the extrusion section of the twin-screw extruder is controlled at 240 ℃, and the air pressure in the three stages is normal pressure.
The nylon halogen-free flame-retardant master batch obtained in the 3 groups of embodiments and master batch terminal products prepared by the traditional process are subjected to comparative experiments on the relevant performances of the added terminal products, and the obtained comparative data are as follows:
| [0094] | [0095]conventional masterbatch 1 | [0096]Conventional masterbatch 2 | [0097]Nylon halogen-free flame-retardant master batch |
| [0098]Tensile yield strength/ISO 527-2-201250 mm/min | [0099] 65 Mpa | [00100] 45 Mpa | [00101] 58 Mpa |
| [00102]Unnotched impact strength/ISO 179-1-2010 | [00103]Continuously, continuously | [00104] 10 Mpa | [00105]Continuously, continuously |
| [00106]Notched impact strength/ISO 179-1-20104J/23 deg.C | [00107] 7.5 Mpa | [00108] 3.5 Mpa | [00109] 6.8 Mpa |
| [00110]Notched impact strength/ISO 179-1-20104J/-30 DEG C | [00111] 0.5 Mpa | [00112] 0 Mpa | [00113] 2.3 Mpa |
| [00114]Heat Distortion Temperature (HDT)/0.45 MPa | [00115] 180 ℃ | [00116] 185 ℃ | [00117] 210 ℃ |
| [00118] UL94 （0.4mm） | [00119] N/A | [00120] V-0 | [00121] V-0 |
The comparison of the experimental data can show that compared with the terminal product added with the traditional masterbatch, the terminal product added with the nylon halogen-free flame-retardant masterbatch provided by the invention has better performance indexes than the terminal product added with the traditional masterbatch, so the experimental data can prove that the nylon halogen-free flame-retardant masterbatch has excellent flame retardance, tensile resistance, impact resistance and other performances, and has stronger application value.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. The halogen-free flame-retardant nylon master batch is characterized in that: the paint consists of the following components: the flame retardant comprises polyamide, a flame retardant, an antioxidant, glass beads and silicate, wherein the content of the five components is as follows:
polyamide: 30% -40%;
flame retardant: 67% -30%;
antioxidant: 1% -10%;
glass beads: 1% -10%;
silicate salt: 1% -10%.
2. The halogen-free flame-retardant nylon masterbatch according to claim 1, wherein: the polyamide is selected from one of polyamide-6, polyamide-66 or polyamide-610.
3. The halogen-free flame-retardant nylon masterbatch according to claim 1, wherein: the flame retardant is made of powdery melamine cyanurate.
4. The halogen-free flame-retardant nylon masterbatch according to claim 1, wherein: the antioxidant is selected from zinc dialkyl dithiophosphate, zinc dialkyl dithiocarbamate, N-phenyl-alpha-naphthylamine and one of alkyl phenothiazine, benzotriazole derivatives or mercaptobenzothiazole derivatives.
5. The halogen-free flame-retardant nylon masterbatch according to claim 1, wherein: the magnetic particles in the glass beads are not more than 0.1 percent of the total weight of the glass beads, and the content of bubbles in the glass beads is less than 10 percent.
6. The halogen-free flame-retardant nylon masterbatch according to claim 1, wherein: the silicate is made of talcum powder.
7. A preparation method of a nylon halogen-free flame-retardant master batch is characterized by comprising the following steps: the method comprises the following steps:
step one, material preparation: preparing five raw materials of polyamide, flame retardant, antioxidant, glass beads and silicate in advance according to a specified proportion;
step two, preliminary mixing: putting the five raw materials obtained in the first step into a high-speed stirrer for fully mixing to obtain a pasty fluid substance;
step three, secondary mixing: putting the pasty fluid substance obtained by mixing in the step two into a high-speed stirrer, and taking out after all the materials in the stirrer are uniformly mixed;
step four, granulation: putting the mixed materials into a double-screw extruder to extrude into strips, stretching the strips by a screw, a die head and a water tank, cooling the strips by the water tank, and preparing the strips into cylindrical granules or round granules by a granulator;
step five, packaging: and (3) putting the master batch which is made into cylindrical granules or round granules into a packaging bag, pumping air in the packaging bag to a vacuum state through an air pump, and then finishing the sealing of the packaging bag through a sealing machine to finally finish the product packaging.
8. The preparation method of the halogen-free flame-retardant nylon master batch according to claim 7, which is characterized in that: in the step two, the stirring temperature is 30-60 ℃, the stirring speed is 6000-10000rpm, the stirring pressure is normal pressure, and the stirring time is controlled to be 3-10min in the primary mixing process of the materials.
9. The preparation method of the halogen-free flame-retardant nylon master batch according to claim 7, which is characterized in that: in the secondary mixing process of the materials in the third step, the stirring temperature is 0-20 ℃, the stirring speed is 6000-10000rpm, the stirring air pressure is normal pressure, and the stirring time is controlled to be 3-10 min.
10. The preparation method of the halogen-free flame-retardant nylon master batch according to claim 7, which is characterized in that: in the granulating process in the fourth step, the temperature of the feeding section of the double-screw extruder is controlled to be in the range of 160-220 ℃, the temperature of the melting section of the double-screw extruder is controlled to be in the range of 220-250 ℃, the temperature of the extruding section of the double-screw extruder is in the range of 200-240 ℃, and the air pressure in the three stages is normal pressure.
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| WO2023008359A1 (en) * | 2021-07-29 | 2023-02-02 | 富士フイルム株式会社 | Magnetorheological fluid and magnetorheological fluid device |
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