CN115304895A - Reinforced flame-retardant PBT (polybutylene terephthalate) material and manufacturing method thereof - Google Patents
Reinforced flame-retardant PBT (polybutylene terephthalate) material and manufacturing method thereof Download PDFInfo
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
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- C08J2367/00—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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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K3/32—Phosphorus-containing compounds
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Abstract
The invention belongs to the technical field of resin processing, and particularly provides a reinforced flame-retardant PBT material which comprises the following raw materials in parts by weight: 25-35 parts of PBT;5-15 parts of PET;20-30 parts of glass fiber; 5-10 parts of a toughening agent; 15-25 parts of a composite flame retardant; 1-3 parts of assistant, wherein the composite flame retardant is prepared by blending phosphorus-nitrogen flame retardant and bromine-antimony flame retardant, the composite flame retardant for the enhanced flame-retardant PBT is a composite flame-retardant system prepared by blending phosphorus-nitrogen flame retardant and bromine-antimony flame retardant, the materials are fully fused under the action of a blending agent, and the PBT is blended and modified under the synergistic cooperation of a synergist and a toughening agent, so that the inherent advantages of PBT resin can be maintained, the performance of the PBT resin is improved, the cost of the material is reduced, the glow wire temperature is increased while the flame-retardant effect is achieved, the defect of instability of the enhanced flame-retardant PBT glow wire is overcome, the comprehensive performance is excellent, the glow wire reaches 750 ℃, the flame-retardant performance is good, and the flame retardance reaches UL94-5VA level.
Description
Technical Field
The invention relates to the technical field of resin processing, in particular to a reinforced flame-retardant PBT material and a manufacturing method thereof.
Background
PBT belongs to one of five engineering plastics, which is known as polybutylene terephthalate, is a polyester series and is prepared by polycondensation of 1, 4-butanediol and terephthalic acid or terephthalate through a mixing procedure to obtain a milky translucent to opaque crystalline thermoplastic polyester resin.
The PBT material is widely applied to the manufacturing industry of automobiles and electronic appliances due to excellent performance, however, the PBT resin also has the defects of poor heat resistance, low temperature resistance of glow wires, poor comprehensive performance, unstable flame retardance and the like, and basically, the inventor provides a novel reinforced flame-retardant PBT material to meet the diversified demands of the market.
Disclosure of Invention
The invention aims to provide a reinforced flame-retardant PBT material and a manufacturing method thereof, which are used for solving the technical problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the reinforced flame-retardant PBT material comprises the following raw materials in parts by weight:
25-35 parts of PBT;
5-15 parts of PET;
glass fiber: 20-30 parts of a solvent;
toughening agent: 5-10 parts;
composite flame retardant: 15-25 parts;
auxiliary agent: 1-3 parts;
wherein the composite flame retardant is prepared by blending a phosphorus-nitrogen flame retardant and a bromine-antimony flame retardant.
The further improvement lies in that: the proportion of the phosphorus-nitrogen flame retardant to the bromine-antimony flame retardant is (3-5): 1, preferably 3.5
The further improvement lies in that: the antimony bromide flame retardant is a mixture of octabromoether, antimony trioxide and magnesium hydroxide, and the proportion of the octabromoether, the antimony trioxide and the magnesium hydroxide is (2-3) to 1, (3.5-4), preferably 3
Wherein, the phosphorus-nitrogen flame retardant is prepared by mixing pentaerythritol (carbon source), ammonium polyphosphate (acid source) and melamine (foaming agent).
Wherein, the octabromoether is used as a main flame retardant, the antimonous oxide is used as a synergistic flame retardant, and the magnesium hydroxide is used as an inorganic flame retardant filler.
The further improvement is that: the toughening agent is one of ABS, SBS and MBS.
The further improvement lies in that: the auxiliary agent comprises a blending agent and a synergistic agent, and the ratio of the blending agent to the synergistic agent is 1: (1.2-1.8).
The further improvement is that: the blending agent is at least one of methyl silicone oil, ethyl silicone oil, phenyl silicone oil, methyl hydrogen-containing silicone oil and dimethyl silicone oil.
The synergist is at least one of aliphatic dibasic acid ester, fatty acid ester and polyol ester.
The invention also provides a manufacturing method of the reinforced flame-retardant PBT material, which comprises the following steps:
(1) Weighing the raw materials in parts by weight, sequentially adding PBT resin, PET resin, a toughening agent, an auxiliary agent and a composite flame retardant into a low-speed mixer, and mixing uniformly;
(2) And quickly adding the mixed materials into a double-screw extruder, introducing glass fibers after the materials are melted and before the materials are extruded, and finally extruding and granulating to obtain the reinforced flame-retardant PBT material.
The further improvement is that: the mixing temperature of the low-grade mixer is 40-60 ℃.
The further improvement lies in that: the temperature set by the twin-screw extruder is 220-250 ℃.
The process requires strict control of extrusion temperature and main machine rotation speed to prevent degradation of certain materials, grease exchange and excessive chopping of glass fibers, and the glass fiber content is inspected every hour, and the product performance is inspected every 8 hours.
The bromine-antimony flame retardant and the phosphorus-nitrogen flame retardant are cooperatively used, so that the flame retardant has good flame retardant effect on resin, the bromine-antimony flame retardant is less in addition amount, and the influence on the mechanical property of the resin is small, and the phosphorus-nitrogen flame retardant has the advantages of no halogen, low smoke and low toxicity.
Compared with the prior art, the invention has the beneficial effects that:
the technology overcomes the defect of instability of the enhanced flame-retardant PBT glowing filament, and the glowing filament has excellent comprehensive performance, reaches 750 ℃, has good flame-retardant performance and achieves the flame-retardant performance of UL94-5VA level.
The composite flame retardant for the enhanced flame-retardant PBT is a composite flame-retardant system in which a phosphorus-nitrogen flame retardant and a bromine-antimony flame retardant are matched, materials are fully fused under the action of a blending agent, and the PBT is subjected to blending modification under the synergistic matching of a synergist and a toughening agent, so that the inherent advantages of PBT resin can be maintained, the performance of the PBT resin is improved, the cost of the PBT resin is reduced, and the temperature of a glow wire is increased while the flame-retardant effect is achieved.
Drawings
FIG. 1 is a process flow diagram of the manufacturing method of the present invention.
Detailed Description
The technical solution of the present invention will be further described with reference to the following specific examples, but the present invention is not limited to these examples.
Example 1
(1) Adding 25 parts of PBT resin, 5 parts of PET resin, 5 parts of toughening agent, 1 part of auxiliary agent and 15 parts of composite flame retardant into a low-speed mixer in sequence, and mixing uniformly;
(2) The mixed material was quickly fed into a twin screw extruder, after the material was melted, and before extrusion, 20 parts of glass fiber was introduced, and finally extrusion granulation was performed to obtain example 1.
Wherein, the proportion of the phosphorus-nitrogen flame retardant to the bromine-antimony flame retardant is 3:1.
wherein, the bromine antimony flame retardant adopts a mixture of octabromoether, antimony trioxide and magnesium hydroxide, and the proportion of the octabromoether, the antimony trioxide and the magnesium hydroxide is 2.
Wherein the ratio of the methyl silicone oil to the fatty acid ester in the auxiliary agent is 1:1.2.
example 2
(1) Sequentially adding 35 parts of PBT resin, 15 parts of PET resin, 10 parts of toughening agent, 3 parts of auxiliary agent and 25 parts of composite flame retardant into a low-speed mixer, and mixing uniformly;
(2) The mixed material was quickly fed into a twin screw extruder, after the material was melted and before extrusion, 30 parts of glass fiber was introduced, and finally extruded and pelletized to obtain example 2.
Wherein the proportion of the phosphorus-nitrogen flame retardant to the antimony bromide flame retardant is 5:1.
wherein, the bromine antimony flame retardant adopts a mixture of octabromoether, antimony trioxide and magnesium hydroxide, and the proportion of the octabromoether, the antimony trioxide and the magnesium hydroxide is 3.
Wherein the proportion of ethyl silicone oil to fatty acid ester in the auxiliary agent is 1:1.8.
example 3
(1) Sequentially adding 30 parts of PBT resin, 10 parts of PET resin, 7 parts of toughening agent, 2 parts of auxiliary agent and 20 parts of composite flame retardant into a low-speed mixer, and mixing uniformly;
(2) The mixed material was rapidly fed into a twin screw extruder, after the material was melted, 25 parts of glass fiber was introduced before extrusion, and finally, extrusion granulation was performed to obtain example 3.
Wherein, the proportion of the phosphorus-nitrogen flame retardant to the bromine-antimony flame retardant is 3.5:1.
wherein, the bromine antimony flame retardant adopts a mixture of octabromoether, antimony trioxide and magnesium hydroxide, and the proportion of the octabromoether, the antimony trioxide and the magnesium hydroxide is 3.
Wherein the ratio of the methyl silicone oil to the fatty acid ester in the auxiliary agent is 1:1.5.
example 4
(1) Adding 28 parts of PBT resin, 12 parts of PET resin, 10 parts of toughening agent, 1 part of auxiliary agent and 19 parts of composite flame retardant into a low-speed mixer in sequence, and mixing uniformly;
(2) The mixed material was rapidly fed into a twin screw extruder, and after the material was melted and before the extrusion, 20 parts of glass fiber was introduced, and finally, extrusion granulation was performed to obtain example 4.
The proportion of the phosphorus-nitrogen flame retardant to the bromine-antimony flame retardant is 4:1.
the bromine antimony flame retardant is a mixture of octabromoether, antimony trioxide and magnesium hydroxide, and the proportion of the octabromoether, the antimony trioxide and the magnesium hydroxide is 2.5.
The proportion of the dimethyl silicone oil to the fatty acid ester in the auxiliary agent is 1:1.5.
comparative examples 1 to 7
Comparative example 1 differs from example 3 in that: comparative column 1 had no PET resin added.
Comparative example 2 differs from example 3 in that: comparative example 2 no composite flame retardant was added.
Comparative column 3 differs from example 3 in that: comparative example 3 the composite flame retardant was only a phosphorus-nitrogen based flame retardant.
Comparative column 4 differs from example 3 in that: comparative example 4 the composite flame retardant was only a bromoantimony-based flame retardant.
Comparative column 5 differs from example 3 in that: comparative example 5 no adjuvant was added.
Comparative column 6 differs from example 3 in that: comparative example 6 the adjuvant was only methyl silicone oil.
Comparative example 7 differs from example 3 in that: comparative example 7 the adjuvant was only a fatty acid ester.
The above prepared examples 1-4 and comparative examples 1-7 were subjected to performance tests under the same conditions as in table one:
the above table shows that the composite flame retardant for the reinforced flame-retardant PBT is a composite flame-retardant system in which a phosphorus-nitrogen flame retardant and a bromine-antimony flame retardant are matched, materials are fully fused under the action of a blending agent, and the PBT is subjected to blending modification under the synergistic matching of the synergist and a toughening agent, so that the inherent advantages of the PBT resin can be maintained, the performance of the PBT resin is improved, the cost of the PBT resin is reduced, the glowing filament temperature is increased while the flame-retardant effect is achieved, the defect of instability of the reinforced flame-retardant PBT glowing filament is overcome, the glowing filament reaches 750 ℃, the flame-retardant performance is good, and the flame retardance reaches UL94-5VA level.
While particular embodiments of the present invention have been illustrated and described, it would be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (10)
1. The reinforced flame-retardant PBT material is characterized by comprising the following raw materials in parts by weight:
25-35 parts of PBT;
5-15 parts of PET;
glass fiber: 20-30 parts;
a toughening agent: 5-10 parts;
composite flame retardant: 15-25 parts;
auxiliary agent: 1-3 parts;
wherein the composite flame retardant is prepared by blending a phosphorus-nitrogen flame retardant and a bromine-antimony flame retardant.
2. The reinforced flame-retardant PBT material according to claim 1, wherein the proportion of the phosphorus-nitrogen flame retardant to the antimony bromide flame retardant is (3-5): 1.
3. the reinforced flame-retardant PBT material according to claim 1 or 2, wherein the antimony bromide flame retardant is a mixture of octabromoether, antimony trioxide and magnesium hydroxide, and the ratio of the eight bromoether to the antimony trioxide to the magnesium hydroxide is (2-3) to 1 (3.5-4) in sequence.
4. The reinforced flame-retardant PBT material of claim 1, wherein the toughening agent is one of ABS, SBS and MBS.
5. The reinforced flame-retardant PBT material as recited in claim 1, wherein the auxiliary agent comprises a blending agent and a synergist, and the ratio of the blending agent to the synergist is 1: (1.2-1.8).
6. The reinforced flame-retardant PBT material of claim 5, wherein the blending agent is at least one of methyl silicone oil, ethyl silicone oil, phenyl silicone oil, methyl hydrogen-containing silicone oil and dimethyl silicone oil.
7. The reinforced flame-retardant PBT material of claim 5, wherein said synergist is at least one of aliphatic dibasic acid ester, aliphatic acid ester and polyol ester.
8. The manufacturing method of the reinforced flame-retardant PBT material of any one of claims 1 to 7, which comprises the following steps:
weighing the raw materials in parts by weight, sequentially adding PBT resin, PET resin, a toughening agent, an auxiliary agent and a composite flame retardant into a low-speed mixer, and mixing uniformly;
and quickly adding the mixed materials into a double-screw extruder, introducing glass fibers after the materials are melted and before the materials are extruded, and finally extruding and granulating to obtain the reinforced flame-retardant PBT material.
9. The manufacturing method of the reinforced flame-retardant PBT material as recited in claim 8, wherein the mixing temperature of the low-temperature mixer is 40-60 ℃.
10. The process for preparing the reinforced flame-retardant PBT material according to the claim 8, wherein the temperature of the twin-screw extruder is set to 220-250 ℃.
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- 2022-08-31 CN CN202211063266.1A patent/CN115304895A/en active Pending
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| CN101565536A (en) * | 2009-05-08 | 2009-10-28 | 南通中蓝工程塑胶有限公司 | Flame-retardant polybutylece terephthalate resin composition with high glow wire ignition temperature |
| CN103709609A (en) * | 2012-09-29 | 2014-04-09 | 青岛欣展塑胶有限公司 | Flame-retardant nanometer master batch for polyester plastic |
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