CN108329662B - Flame-retardant reinforced PBT composition and preparation method thereof - Google Patents
Flame-retardant reinforced PBT composition and preparation method thereof Download PDFInfo
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- CN108329662B CN108329662B CN201711430596.9A CN201711430596A CN108329662B CN 108329662 B CN108329662 B CN 108329662B CN 201711430596 A CN201711430596 A CN 201711430596A CN 108329662 B CN108329662 B CN 108329662B
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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
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a flame-retardant reinforced PBT composition which comprises the following components in parts by weight: 40-55 parts of PBT resin; 20-35 parts of glass fiber; 7-17 parts of a flame retardant; 1-3 parts of flame-retardant synergist; 2-5 parts of polyethylene wax. According to the invention, the polyethylene wax with a specific content is added into the formula of the flame-retardant reinforced PBT composition, so that the toughness of the PBT material can be obviously improved, the flowability can be improved, and the heat distortion temperature can be improved.
Description
Technical Field
The invention relates to a PBT composition, in particular to a flame-retardant reinforced PBT composition and a preparation method thereof.
Background
Polybutylene terephthalate (PBT) is a semi-crystalline engineering plastic, has good mechanical properties, electrical properties, heat resistance, chemical resistance and the like, and is widely used in the industries of automobiles, electronics, electric appliances and the like.
However, in some specific cases, the flame retardant reinforced PBT material has poor toughness, and the toughening is generally carried out by adding a toughening agent, but the addition of the toughening agent causes reduction of fluidity. The toughening agent added to PBT is a reactive toughening agent containing glycidyl ester or maleic anhydride, such as AX-8900, PTW, maleic anhydride graft, etc., and the problem is that the flowability is reduced.
So far, no report has been made about the addition of a specific content of polyethylene wax to a flame retardant reinforced PBT composition for improving the toughness of the PBT material and also improving the flowability and the heat distortion temperature.
Disclosure of Invention
In order to overcome the disadvantages and shortcomings of the prior art, the invention provides a flame-retardant reinforced PBT composition with obviously improved toughness and obviously improved fluidity and heat distortion temperature
Another object of the invention is to provide a process for preparing the flame retardant reinforced PBT composition.
The above purpose of the invention is realized by the following technical scheme:
the flame-retardant reinforced PBT composition comprises the following components in parts by weight:
40-55 parts of PBT resin;
20-35 parts of glass fiber;
7-17 parts of a flame retardant;
1-3 parts of flame-retardant synergist;
2-5 parts of polyethylene wax.
When the polyethylene wax is added in an amount of less than 2 parts by weight, based on the total weight of the flame retardant reinforced PBT composition, the toughening effect of the flame retardant reinforced PBT composition is poor; and when the amount of the polyethylene wax added exceeds 5 parts by weight, the flame-retardant reinforced PBT composition is subjected to injection molding with precipitates.
Wherein the softening point of the polyethylene wax is 100-110 ℃, preferably 106-108 ℃. The appearance is separated out due to the excessively low softening point; the softening point is too high, and the fluidity, the toughness and the heat distortion temperature are low.
The method for testing the softening point comprises the following steps: freezing the flame-retardant reinforced PBT composition by using liquid nitrogen, grinding the composition into powder by using a grinder, extracting the powder for 24 hours by using methanol, evaporating the methanol in the extract to dryness to obtain polyethylene wax, and testing the softening point of the extracted polyethylene wax according to GB 12007.6-1989.
Wherein the diameter of the glass fiber is 5-15 μm.
The flame retardant is a brominated flame retardant, preferably one or more of brominated epoxy resin, decabromodiphenylethane, brominated triazine and brominated polystyrene.
Wherein the flame retardant synergist is selected from one or more of antimony trioxide and sodium antimonate.
A preparation method of the flame-retardant reinforced PBT composition comprises the following steps:
mixing the PBT resin, the flame retardant, the flame-retardant synergist and the polyethylene wax in a high-speed mixer for 1-2 minutes according to the proportion to obtain a premix, performing melt extrusion on the premix at 220-240 ℃ by a double-screw extruder, performing side feeding on glass fibers, cooling and granulating to obtain the flame-retardant reinforced PBT composition.
Wherein, the temperature of each screw cylinder from the charging opening to the machine head of the double-screw extruder is respectively as follows: 150-170 ℃, 210-230 ℃, 220-240 ℃, 230-250 ℃, 210-230 ℃, the screw rotating speed of 280-320 revolutions per minute, and the feeding amount of 50-70 kg/h.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the polyethylene wax with a specific content is added into the formula of the flame-retardant reinforced PBT composition, so that the toughness of the PBT material can be obviously improved, the flowability can be improved, and the heat distortion temperature can be improved.
Detailed Description
The present invention is further illustrated by the following specific examples, which are, however, not intended to limit the scope of the invention.
The test method of each performance index comprises the following steps:
tensile strength: test standard ISO 527/2-93;
notched impact strength: test standard ISO 180-2000;
heat distortion temperature: test standard ISO 75-2;
melt flow rate: 250 ℃ and 2.16 kg;
and (3) injection molding and precipitation: a100-mold square plate was continuously injection-molded, and the presence or absence of precipitates in the mold and the square plate was visually observed.
The examples of the present invention employ, but are not limited to, the following raw materials:
PBT resin, model PBT-2100-211M, Taiwan Changchun;
glass fiber: a boulder group with a diameter of 10 μm, ER-13;
flame retardant: brominated epoxy resin, type powder f-2100, Israel chemical;
flame retardant synergist: antimony trioxide, manufacturer yang-benefiting flash star antimony industry ltd;
polyethylene wax: polyethylene wax-1, softening point 95 ℃, model BN-100, manufacturer: qingdao Bangni chemical industry;
polyethylene wax-2, softening point 100 ℃, model BN-108, manufacturer: qingdao Bangni chemical industry;
polyethylene wax-3, softening point 108 ℃, type CERALENE 2T, manufacturer: EUROCES corporation;
polyethylene wax-4, softening point 124 ℃, type CERALENE 128, manufacturer EUROCES;
a toughening agent: ethylene-butyl acrylate-glycidyl methacrylate, model PTW, manufacturer: dupont company.
Examples 1-8 and comparative examples 1-4: preparation of flame-retardant reinforced PBT composition
Mixing the PBT resin, the flame retardant, the flame-retardant synergist and the polyethylene wax in a high-speed mixer according to the proportion in the table 1 for 1-2 minutes to obtain a premix, and performing melt extrusion, cooling and granulation on the premix at 220-240 ℃ by using a double-screw extruder to obtain the flame-retardant reinforced PBT composition; wherein the temperature of each screw cylinder of the double-screw extruder (from a charging port to a machine head) is respectively as follows: 160 ℃, 220 ℃, 230 ℃, 240 ℃, 220 ℃, the screw rotating speed is 300 r/min, and the feeding amount is 60 kg/h. The measured performance indexes of the flame-retardant reinforced PBT composition, such as tensile strength, notch impact strength, heat distortion temperature, melt flow rate, injection molding precipitation and the like, are shown in Table 1.
TABLE 1 ingredient ratios (parts by weight) and results of performance tests for examples 1 to 8 and comparative examples 1 to 4
TABLE 1
As can be seen from the comparison between examples 1-8 and comparative examples 1-4 in Table 1, the addition of polyethylene wax in a specific amount to the formulation of the flame retardant reinforced PBT composition can significantly improve the toughness, the flowability and the heat distortion temperature of the PBT material.
Claims (6)
1. The flame-retardant reinforced PBT composition comprises the following components in parts by weight:
40-55 parts of PBT resin;
20-35 parts of glass fiber;
7-17 parts of a flame retardant;
1-3 parts of flame-retardant synergist;
2-5 parts of polyethylene wax;
the softening point of the polyethylene wax is 108 ℃.
2. The flame retardant reinforced PBT composition of claim 1, wherein the glass fiber has a diameter of from 5 μm to 15 μm.
3. The flame retardant reinforced PBT composition of claim 1, wherein the flame retardant is a brominated flame retardant selected from one or more of brominated epoxy resins, decabromodiphenylethane, bromotriazine, and brominated polystyrene.
4. The flame retardant reinforced PBT composition of claim 1, wherein the flame retardant synergist is selected from one or more of antimony trioxide and sodium antimonate.
5. A process for preparing the flame retardant reinforced PBT composition of any of claims 1-4, wherein: the method comprises the following steps:
mixing the PBT resin, the flame retardant, the flame-retardant synergist and the polyethylene wax in a high-speed mixer for 1-2 minutes according to the proportion to obtain a premix, performing melt extrusion on the premix at 220-240 ℃ by a double-screw extruder, performing side feeding on glass fibers, cooling and granulating to obtain the flame-retardant reinforced PBT composition.
6. The method for preparing the flame retardant reinforced PBT composition according to claim 5, wherein the temperatures of each barrel of the twin-screw extruder from the feeding port to the head are respectively as follows: 150-170 ℃, 210-230 ℃, 220-240 ℃, 230-250 ℃, 210-230 ℃, the screw rotating speed of 280-320 revolutions per minute, and the feeding amount of 50-70 kg/h.
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| CN201711430596.9A CN108329662B (en) | 2017-12-26 | 2017-12-26 | Flame-retardant reinforced PBT composition and preparation method thereof |
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| CN108329662B true CN108329662B (en) | 2021-05-04 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717559A (en) * | 2009-11-09 | 2010-06-02 | 江阴济化新材料有限公司 | Tin-soldering resistant polybutylece terephthalate (PBT) engineering plastic and method for preparing same |
| CN103525020A (en) * | 2012-07-02 | 2014-01-22 | 青岛欣展塑胶有限公司 | Glass fiber-reinforced halogen flame-retardant high-temperature-resistant PBT (Polybutylene Terephthalate) and preparation method thereof |
| CN107189371A (en) * | 2017-06-26 | 2017-09-22 | 东莞市东翔塑胶有限公司 | A kind of low Tvoc anti-flaming PBT composites and preparation method thereof |
-
2017
- 2017-12-26 CN CN201711430596.9A patent/CN108329662B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717559A (en) * | 2009-11-09 | 2010-06-02 | 江阴济化新材料有限公司 | Tin-soldering resistant polybutylece terephthalate (PBT) engineering plastic and method for preparing same |
| CN103525020A (en) * | 2012-07-02 | 2014-01-22 | 青岛欣展塑胶有限公司 | Glass fiber-reinforced halogen flame-retardant high-temperature-resistant PBT (Polybutylene Terephthalate) and preparation method thereof |
| CN107189371A (en) * | 2017-06-26 | 2017-09-22 | 东莞市东翔塑胶有限公司 | A kind of low Tvoc anti-flaming PBT composites and preparation method thereof |
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