Modified PBT material and preparation method thereof

By combining a composite toughening system with flame retardants, the toughening effect and flame retardant properties of PBT materials are improved, the impact strength and low-temperature resistance are enhanced, and the cost is reduced.

CN120607803APending Publication Date: 2025-09-09SHENYANG SIWEI POLYMER PLASTIC
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Patent Information

Application Number
CN202410262341.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-03-07
Publication Date
2025-09-09

AI Technical Summary

Technical Problem

The flame retardant reinforcement and toughening effects of existing PBT materials are poor, and the toughening cost is high.

Method used

A composite toughening system is adopted, using GMA grafted POE or EPDM as toughening agent A, and SEBS grafted with maleic anhydride as toughening agent B, combined with brominated epoxy as flame retardant and antimony trioxide as synergist, and the modified PBT material is prepared by high-speed mixing and twin-screw extruder processing.

Benefits of technology

The impact strength and fluidity of PBT materials are improved, the low temperature resistance is enhanced, and the toughening cost is reduced.

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Abstract

The invention discloses a modified PBT (polybutylene terephthalate) material and a preparation method thereof.The preparation method comprises the steps that weighed polybutylene terephthalate, a flexibilizer A, a flexibilizer B, a flame retardant, a synergist, an antioxidant 1010, an antioxidant 168, barium stearate and barium sulfate are added into a high-speed mixer in proportion, the rotating speed is 1000 revolutions, the mixing time is 3 minutes, the materials are fully and evenly stirred, and a mixture is obtained; and extruding by using a twin-screw extruder, granulating and drying to obtain the modified PBT. The invention relates to the technical field of chemical substances. According to the modified PBT material and the preparation method thereof, a composite toughening system is selected for toughening, GMA provides a better compatible toughening effect, and the SEBS graft is compounded, so that the product has good fluidity and better low-temperature resistance.
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Description

Technical Field

[0001] The present invention relates to the technical field of chemical substances, in particular to a modified PBT material and a preparation method thereof. Background Art

[0002] PBT polybutylene terephthalate, also known as polytetramethylene terephthalate, belongs to the polyester series and is one of the toughest engineering thermoplastic materials. It is made by the polycondensation of 1.4-PBT butanediol (1.4-Butylene glycol) and terephthalic acid (PTA) or dimethyl terephthalate (DMT). It has excellent chemical stability, mechanical strength, electrical insulation properties and thermal stability. It is widely used in household appliances, electrical components and the automotive industry. At the same time, PBT also has important applications in fibers, films and other fields.

[0003] At present, the impact strength of flame-retardant reinforced PBT is generally low. PBT is a resin that is difficult to toughen. The toughening effect of simple maleic anhydride grafting is average, and the cost of using GMA grafting is greatly increased. Summary of the Invention

[0004] (1) Technical problems solved

[0005] In view of the shortcomings of the existing technology, the present invention provides a modified PBT material and a preparation method thereof, which solves the problems of generally low impact strength, general toughening effect and high grafting cost of the current flame retardant reinforced PBT.

[0006] (2) Technical solution

[0007] To achieve the above objectives, the present invention is implemented through the following technical solutions: a modified PBT material, the PBT material comprises the following components by weight:

[0008] 50-150 parts of polybutylene terephthalate, 1-5 parts of toughening agent A, 1-5 parts of toughening agent B, 10-25 parts of flame retardant, 1-6 parts of synergist, 0.1-0.6 parts of antioxidant 1010, 0.1-0.6 parts of antioxidant 168, 0.1-0.3 parts of barium stearate and 0.1-0.3 parts of barium sulfate.

[0009] Preferably, the polybutylene terephthalate comprises 50 parts, 1 part of toughener A, 1 part of toughener B, 10 parts of flame retardant, 1 part of synergist, 0.1 parts of antioxidant 1010, 0.1 parts of antioxidant 168, 0.1 parts of barium stearate and 0.1 parts of barium sulfate.

[0010] Preferably, the polybutylene terephthalate comprises 100 parts, 3 parts of toughener A, 3 parts of toughener B, 17 parts of flame retardant, 3.5 parts of synergist, 0.3 parts of antioxidant 1010, 0.3 parts of antioxidant 168, 0.2 parts of barium stearate and 0.2 parts of barium sulfate.

[0011] Preferably, the polybutylene terephthalate comprises 150 parts, toughener A 5 parts, toughener B 5 parts, flame retardant 25 parts, synergist 6 parts, antioxidant 10100.6 parts, antioxidant 1680.6 parts, barium stearate 00.3 parts and barium sulfate 0.3 parts.

[0012] Preferably, the toughening agent A is one of GMA grafted POE or EPDM.

[0013] Preferably, the toughening agent B is maleic anhydride grafted SEBS.

[0014] Preferably, the flame retardant is brominated epoxy, and the synergist is antimony trioxide.

[0015] A method for preparing a modified PBT material, specifically comprising the following steps:

[0016] The weighed polybutylene terephthalate, toughener A, toughener B, flame retardant, synergist, antioxidant 1010, antioxidant 168, barium stearate and barium sulfate were added into a high-speed mixer in proportion at a speed of 1000 rpm for 3 min. The mixture was fully stirred and extruded through a twin-screw extruder, pelletized and dried to obtain modified PBT.

[0017] The twin-screw extruder is divided into six zones, with zone one at 165°C, zone two at 245°C, zone three at 240°C, zone four at 240°C, zone five at 235°C, zone six at 235°C and zone seven at 230°C. The head temperature is 245°C and the vacuum degree of the twin-screw extruder is 0.6Mpa. The speed of the twin-screw main engine is 390 rpm, the feeding speed is 21.5 rpm, and the cutter speed is 800 rpm.

[0018] (3) Beneficial effects

[0019] The present invention provides a modified PBT material and a preparation method thereof. Compared with the prior art, the present invention has the following advantages:

[0020] (1) The modified PBT material and its preparation method are flame-retardant reinforced PBT. The notched impact strength is low due to the addition of inorganic fillers and flame retardants. This product uses a composite toughening system for toughening. GMA provides better compatibility and toughening effect. The compound SEBS grafted material makes the product have good fluidity and better low-temperature resistance. DETAILED DESCRIPTION

[0021] The technical solutions in the embodiments of the present invention are clearly and completely described. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. All other embodiments derived by persons of ordinary skill in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0022] The present invention provides a technical solution: a modified PBT material, which includes the following components by weight: 50 parts of polybutylene terephthalate, 1 part of toughening agent A, 1 part of toughening agent B, 10 parts of flame retardant, 1 part of synergist, 10100.1 parts of antioxidant, 1680.1 parts of antioxidant, 0.1 part of barium stearate and 0.1 part of barium sulfate.

[0023] A method for preparing a modified PBT material, specifically comprising the following steps:

[0024] The weighed polybutylene terephthalate, toughener A, toughener B, flame retardant, synergist, antioxidant 1010, antioxidant 168, barium stearate and barium sulfate were added into a high-speed mixer in proportion at a speed of 1000 rpm for 3 min. The mixture was fully stirred and extruded through a twin-screw extruder, pelletized and dried to obtain modified PBT.

[0025] Example 2

[0026] The present invention provides a technical solution: a modified PBT material, the PBT material including the following components by weight: 100 parts of polybutylene terephthalate, 3 parts of toughening agent A, 3 parts of toughening agent B, 17 parts of flame retardant, 3.5 parts of synergist, 0.3 parts of antioxidant 1010, 0.3 parts of antioxidant 168, 0.2 parts of barium stearate and 0.2 parts of barium sulfate.

[0027] A method for preparing a modified PBT material, specifically comprising the following steps:

[0028] The weighed polybutylene terephthalate, toughener A, toughener B, flame retardant, synergist, antioxidant 1010, antioxidant 168, barium stearate and barium sulfate were added into a high-speed mixer in proportion at a speed of 1000 rpm for 3 min. The mixture was fully stirred and extruded through a twin-screw extruder, pelletized and dried to obtain modified PBT.

[0029] Example 3

[0030] The present invention provides a technical solution: a modified PBT material, the PBT material comprising the following components by weight: 150 parts of polybutylene terephthalate, 5 parts of toughener A, 5 parts of toughener B, 25 parts of flame retardant, 6 parts of synergist, 10100.6 parts of antioxidant, 1680.6 parts of antioxidant, 00.3 parts of barium stearate and 0.3 parts of barium sulfate.

[0031] A method for preparing a modified PBT material, specifically comprising the following steps:

[0032] The weighed polybutylene terephthalate, toughener A, toughener B, flame retardant, synergist, antioxidant 1010, antioxidant 168, barium stearate and barium sulfate were added into a high-speed mixer in proportion at a speed of 1000 rpm for 3 min. The mixture was fully stirred and extruded through a twin-screw extruder, pelletized and dried to obtain modified PBT.

[0033] Among the above three embodiments, the toughening agent A is one of GMA grafted POE or EPDM, wherein GMA is glycidyl methacrylate, and the grafted POE is epoxy-grafted ethylene propylene rubber particles, which has a high grafting rate and stable quality, and avoids the sensitivity of maleic anhydride grafted materials to moisture. Since partial vulcanization is used for the grafted POE, the impact strength is greatly improved and a significant decrease in rigidity is avoided. The grafted EPDM is prepared by grafting maleic anhydride on EPDM elastomer through reaction extrusion, and only one of them can be used.

[0034] Toughener B is maleic anhydride grafted SEBS, wherein SEBS is a linear triblock copolymer with polystyrene as the terminal segment and ethylene-butylene copolymer obtained by hydrogenating polybutadiene as the middle elastic block. MAH, or maleic anhydride grafted, is a polymer obtained by grafting maleic anhydride as a monomer with other materials under appropriate temperature conditions. Generally, the grafting methods mainly include solution method, melt method, radiation method and solid phase method. Maleic anhydride grafted SEBS refers to a triblock copolymer grafted with MAH through solution method, melt method, radiation method and solid phase method.

[0035] Furthermore, the flame retardant is brominated epoxy and the synergist is antimony trioxide.

[0036] A further antioxidant, 1010, also known as pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate, is a white crystalline powder.

[0037] Further antioxidant 168, also known as tris(2,4-di-tert-butylphenyl) phosphite antioxidant 168, is a low-volatile organic synthetic antioxidant inhibitor.

[0038] The following table is a comparison of the data of the embodiment;

[0039]

[0040] According to the data comparison, it can be seen that the composite toughening system is used for toughening. The GMA type provides better compatible toughening effect, and the compound SEBS grafted material makes the product have good fluidity and better low temperature resistance.

[0041] Meanwhile, the contents not described in detail in this specification belong to the prior art known to those skilled in the art.

[0042] It should be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the terms "comprises," "comprising," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that includes a list of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such process, method, article, or apparatus.

[0043] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

Claims

1. A modified PBT material, characterized in that: The PBT material comprises the following components in parts by weight: 50-150 parts of polybutylene terephthalate, 1-5 parts of toughening agent A, 1-5 parts of toughening agent B, 10-25 parts of flame retardant, 1-6 parts of synergist, 0.1-0.6 parts of antioxidant 1010, 0.1-0.6 parts of antioxidant 168, 0.1-0.3 parts of barium stearate and 0.1-0.3 parts of barium sulfate.

2. A modified PBT material according to claim 1, characterized in that: The polybutylene terephthalate is 50 parts, the toughening agent A is 1 part, the toughening agent B is 1 part, the flame retardant is 10 parts, the synergist is 1 part, the antioxidant 10100.1 parts, the antioxidant 1680.1 parts, the barium stearate is 0.1 parts and the barium sulfate is 0.1 parts.

3. The modified PBT material according to claim 1, characterized in that: The polybutylene terephthalate is 100 parts, the toughening agent A is 3 parts, the toughening agent B is 3 parts, the flame retardant is 17 parts, the synergist is 3.5 parts, the antioxidant 10100.3 parts, the antioxidant 1680.3 parts, the barium stearate is 0.2 parts and the barium sulfate is 0.2 parts.

4. The modified PBT material according to claim 1, characterized in that: The polybutylene terephthalate is 150 parts, the toughening agent A is 5 parts, the toughening agent B is 5 parts, the flame retardant is 25 parts, the synergist is 6 parts, the antioxidant 10100.6 parts, the antioxidant 1680.6 parts, the barium stearate is 00.3 parts and the barium sulfate is 0.3 parts.

5. The modified PBT material according to claim 1, characterized in that: The toughening agent A is one of GMA grafted POE or EPDM, and the toughening agent B is maleic anhydride grafted SEBS.

6. The modified PBT material according to claim 1, characterized in that: The flame retardant is epoxy bromide, and the synergist is antimony trioxide.

7. The method for preparing a modified PBT material according to any one of claims 1 to 6, characterized in that: Specifically include the following steps: The weighed polybutylene terephthalate, toughener A, toughener B, flame retardant, synergist, antioxidant 1010, antioxidant 168, barium stearate and barium sulfate were added into a high-speed mixer in proportion at a speed of 1000 rpm for 3 min. The mixture was fully stirred and extruded through a twin-screw extruder, pelletized and dried to obtain modified PBT.