PBT (polybutylene terephthalate) flexibilizer and preparation method thereof

Abstract

The preparation method comprises the following steps: adding an ethylene-octylene copolymer, ethylene propylene diene monomer and silicone into a high-speed mixer in proportion, and fully and uniformly stirring for later use; the preparation method comprises the following steps: adding weighed glycidyl methacrylate, styrene, gamma-methacryloxypropyltrimethoxysilane and an initiator into a liquid mixing device, fully and uniformly stirring for later use, adding the prepared grafted monomer mixture into a raw material mixture, and keeping the speed of a high-speed mixer at 900 revolutions in the process; the preparation method comprises the following steps: adding a direct monomer mixture within 1 minute, mixing and stirring for 3 minutes, extruding and pelletizing by using a double-screw extruder, and finally drying to obtain the flexibilizer. According to the PBT toughening agent and the preparation method thereof, the PBT toughening effect is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of toughening agents, in particular to a PBT toughening agent and a preparation method thereof. Background Art

[0002] Toughening agents are substances that increase the flexibility of adhesive films. Certain thermosetting resin adhesives, such as epoxy resins, phenolic resins, and unsaturated polyester resins, have low elongation and are brittle after curing. When the bonded area is subjected to external forces, cracks easily form and rapidly expand, causing the adhesive layer to crack. These cracks are fatigue-prone and cannot be used for structural bonding. Therefore, methods must be employed to reduce brittleness, increase toughness, and improve load-bearing strength. Toughening agents are substances that can reduce brittleness and increase toughness without affecting the other key properties of the adhesive. They can be categorized as rubber-based toughening agents and thermoplastic elastomer-based toughening agents.

[0003] Currently, the manufacturing of PBT toughening agents with reactive toughening agents (requiring polymerization equipment) is difficult and has high equipment requirements. Another type of toughening agent is maleic anhydride grafted products, which have a general toughening effect on PBT. The traditional method is single carrier grafting and single initiator system grafting. Summary of the Invention

[0004] (1) Technical problems solved

[0005] In view of the shortcomings of the prior art, the present invention provides a PBT toughening agent and a preparation method thereof, which solves the problem that the toughening effect of PBT is average.

[0006] (2) Technical solution

[0007] To achieve the above objectives, the present invention is implemented through the following technical solution: a PBT toughening agent, comprising the following raw materials in parts by weight: 50-80 parts of ethylene octene copolymer, 10-40 parts of EPDM rubber, 0.1-0.5 parts of silicone, 1-10 parts of glycidyl methacrylate, 0.1-1 parts of styrene, 0.1-0.5 parts of initiator and 0.5-2 parts of γ-methacryloxypropyltrimethoxysilane.

[0008] Preferably, the ethylene octene copolymer comprises 50 parts, 10 parts of EPDM rubber, 0.1 parts of silicone, 1 part of glycidyl methacrylate, 0.1 parts of styrene, 0.1 parts of initiator and 0.5 parts of γ-methacryloxypropyltrimethoxysilane.

[0009] Preferably, the ethylene octene copolymer comprises 75 parts, ethylene propylene diene monomer rubber 25 parts, silicone 0.1 parts, glycidyl methacrylate 5 parts, styrene 0.5 parts, initiator 0.2 parts and γ-methacryloxypropyltrimethoxysilane 1 part.

[0010] Preferably, the ethylene octene copolymer comprises 80 parts, 40 parts of EPDM rubber, 0.5 parts of silicone, 10 parts of glycidyl methacrylate, 1 part of styrene, 0.5 parts of initiator and 2 parts of γ-methacryloxypropyltrimethoxysilane.

[0011] Preferably, the initiator is 2,5-dimethyl-2,5-diperoxytert-butylhexane.

[0012] The present invention also discloses a method for preparing a PBT toughening agent, comprising the following steps:

[0013] S1, preparation of raw material mixture, adding ethylene octene copolymer, EPDM rubber and silicone in proportion into a high-speed mixer, and stirring them thoroughly for standby use;

[0014] S2. Preparation of a graft monomer mixture: adding weighed glycidyl methacrylate, styrene, γ-methacryloxypropyltrimethoxysilane and initiator to a liquid mixing device and stirring thoroughly for later use;

[0015] S3, preparation of PBT toughening agent, adding the prepared grafted monomer mixture to the raw material mixture, during this process the high-speed mixer is still at 900 rpm, the direct monomer mixture is added within 1 minute, mixed and stirred for 3 minutes, then extruded and pelletized by a twin-screw extruder, and finally dried to obtain the toughening agent.

[0016] Preferably, in step S1, the speed of the high-speed mixer is 900 rpm, and the mixing time is 1 min.

[0017] Preferably, in the step S3, the main engine speed of the twin-screw extruder is 350 rpm, the feeding speed is 35 rpm, the cutter speed is 400 rpm, and the vacuum degree is 0.6 MPa.

[0018] (3) Beneficial effects

[0019] The present invention provides a PBT toughening agent and a preparation method thereof. Compared with the prior art, it has the following beneficial effects:

[0020] (1) The PBT toughening agent and its preparation method, by selecting POE and EPDM in combination, not only maintain the excellent heat resistance and chemical resistance of POE, but also significantly improve the low temperature resistance of the toughening agent by adding EPDM.

[0021] (2) The PBT toughening agent and its preparation method greatly improve the grafting activity of GMA by introducing styrene monomer.

[0022] (3) The PBT toughening agent and its preparation method greatly improve the efficiency of the entire grafting reaction process by combining the peroxide initiator dipentadiene and the silane coupling agent KH570.

[0023] (4) The PBT toughening agent and its preparation method can improve the impact strength of the product by using the PBT toughening agent. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 This is a flow chart for preparing the PBT toughening agent of the present invention. DETAILED DESCRIPTION

[0025] 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.

[0026] See also Figure 1

[0027] Example 1. The present invention provides a technical solution: a PBT toughener, comprising the following raw materials in parts by weight: 50 parts of POE (ethylene octene copolymer), 10 parts of EPDM (ethylene propylene diene monomer), 0.1 parts of silicone, 1 part of GMA (glycidyl methacrylate), 0.1 parts of styrene, 0.1 parts of initiator (2,5-dimethyl-2,5-diperoxy tert-butylhexane) and 0.5 parts of KH570 (γ-methacryloxypropyltrimethoxysilane).

[0028] A method for preparing a PBT toughening agent comprises the following steps:

[0029] S1, preparation of raw material mixture, adding ethylene octene copolymer, EPDM rubber and silicone in proportion into a high-speed mixer, and stirring them thoroughly for standby use;

[0030] S2. Preparation of a graft monomer mixture: adding weighed glycidyl methacrylate, styrene, γ-methacryloxypropyltrimethoxysilane and initiator to a liquid mixing device and stirring thoroughly for later use;

[0031] S3, preparation of PBT toughening agent, adding the prepared grafted monomer mixture to the raw material mixture, during this process the high-speed mixer is still at 900 rpm, the direct monomer mixture is added within 1 minute, mixed and stirred for 3 minutes, then extruded and pelletized by a twin-screw extruder, and finally dried to obtain the toughening agent.

[0032] Furthermore, in step S1, the rotation speed of the high-speed mixer is 900 rpm, and the mixing time is 1 min.

[0033] Furthermore, in step S3, the main engine speed of the twin-screw extruder is 350 rpm, the feeding speed is 35 rpm, the cutting speed is 400 rpm, and the vacuum degree is 0.6 MPa.

[0034] Example 2. The present invention provides a technical solution: a PBT toughener, comprising the following raw materials in parts by weight: 75 parts of POE (ethylene octene copolymer), 25 parts of EPDM (ethylene propylene diene monomer), 0.1 parts of silicone, 5 parts of GMA (glycidyl methacrylate), 0.5 parts of styrene, 0.2 parts of initiator (2,5-dimethyl-2,5-diperoxy tert-butylhexane) and 1 part of KH570 (γ-methacryloxypropyltrimethoxysilane).

[0035] A method for preparing a PBT toughening agent comprises the following steps:

[0036] S1, preparation of raw material mixture, adding ethylene octene copolymer, EPDM rubber and silicone in proportion into a high-speed mixer, and stirring them thoroughly for standby use;

[0037] S2. Preparation of a graft monomer mixture: adding weighed glycidyl methacrylate, styrene, γ-methacryloxypropyltrimethoxysilane and initiator to a liquid mixing device and stirring thoroughly for later use;

[0038] S3, preparation of PBT toughening agent, adding the prepared grafted monomer mixture to the raw material mixture, during this process the high-speed mixer is still at 900 rpm, the direct monomer mixture is added within 1 minute, mixed and stirred for 3 minutes, then extruded and pelletized by a twin-screw extruder, and finally dried to obtain the toughening agent.

[0039] Furthermore, in step S1, the rotation speed of the high-speed mixer is 900 rpm, and the mixing time is 1 min.

[0040] Furthermore, in step S3, the main engine speed of the twin-screw extruder is 350 rpm, the feeding speed is 35 rpm, the cutting speed is 400 rpm, and the vacuum degree is 0.6 MPa.

[0041] Example 3. The present invention provides a technical solution: a PBT toughener, comprising the following raw materials in parts by weight: 80 parts of POE (ethylene octene copolymer), 40 parts of EPDM (ethylene propylene diene monomer), 0.5 parts of silicone, 10 parts of GMA (glycidyl methacrylate), 1 part of styrene, 0.5 parts of initiator (2,5-dimethyl-2,5-diperoxy tert-butylhexane) and 2 parts of KH570 (γ-methacryloxypropyltrimethoxysilane).

[0042] A method for preparing a PBT toughening agent comprises the following steps:

[0043] S1, preparation of raw material mixture, adding ethylene octene copolymer, EPDM rubber and silicone in proportion into a high-speed mixer, and stirring them thoroughly for standby use;

[0044] S2. Preparation of a graft monomer mixture: adding weighed glycidyl methacrylate, styrene, γ-methacryloxypropyltrimethoxysilane and initiator to a liquid mixing device and stirring thoroughly for later use;

[0045] S3, preparation of PBT toughening agent, adding the prepared grafted monomer mixture to the raw material mixture, during this process the high-speed mixer is still at 900 rpm, the direct monomer mixture is added within 1 minute, mixed and stirred for 3 minutes, then extruded and pelletized by a twin-screw extruder, and finally dried to obtain the toughening agent.

[0046] Furthermore, in step S1, the rotation speed of the high-speed mixer is 900 rpm, and the mixing time is 1 min.

[0047] Furthermore, in step S3, the main engine speed of the twin-screw extruder is 350 rpm, the feeding speed is 35 rpm, the cutting speed is 400 rpm, and the vacuum degree is 0.6 MPa.

[0048] The twin-screw extruders in the three embodiments are divided into six zones according to length during extrusion, wherein the temperature of zone 1 is 195°C, zone 2 is 205°C, zone 3 is 215°C, zone 4 is 210°C, zone 5 is 205°C and zone 6 is 200°C. In addition, the temperature of the die head is 195°C. The required temperature is used to ensure the quality of extrusion.

[0049] In addition, the experimental data in the above embodiment 2 are as follows:

[0050]

[0051] The toughening effect of the PBT toughening agent prepared by the formula in Example 2 is improved. The notched impact strength of the flame-retardant reinforced PBT is low due to the addition of inorganic fillers and flame retardants. The addition of this toughening agent can greatly improve the impact strength of this product.

[0052] At the same time, the contents not described in detail in this specification belong to the existing technology well known to those skilled in the art.

[0053] 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.

[0054] 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 PBT toughening agent, characterized in that: The invention comprises the following raw materials in parts by weight: 50-80 parts of ethylene octene copolymer, 10-40 parts of ethylene propylene diene monomer rubber, 0.1-0.5 parts of silicone, 1-10 parts of glycidyl methacrylate, 0.1-1 parts of styrene, 0.1-0.5 parts of initiator and 0.5-2 parts of gamma-methacryloyloxypropyltrimethoxysilane.

2. A PBT toughening agent according to claim 1, characterized in that: The ethylene octene copolymer is 50 parts, the ethylene propylene diene monomer rubber is 10 parts, the silicone is 0.1 parts, the glycidyl methacrylate is 1 part, the styrene is 0.1 parts, the initiator is 0.1 parts and the gamma-methacryloxypropyltrimethoxysilane is 0.5 parts.

3. A PBT toughening agent according to claim 1, characterized in that: The ethylene octene copolymer is 75 parts, the ethylene propylene diene monomer rubber is 25 parts, the silicone is 0.1 parts, the glycidyl methacrylate is 5 parts, the styrene is 0.5 parts, the initiator is 0.2 parts and the gamma-methacryloxypropyltrimethoxysilane is 1 part.

4. A PBT toughening agent according to claim 1, characterized in that: 80 parts of the ethylene octene copolymer, 40 parts of EPDM rubber, 0.5 parts of silicone, 10 parts of glycidyl methacrylate, 1 part of styrene, 0.5 parts of initiator and 2 parts of γ-methacryloxypropyltrimethoxysilane.

5. A PBT toughening agent according to claim 1, characterized in that: The initiator is 2,5-dimethyl-2,5-diperoxide tert-butylhexane.

6. The method for preparing any one of the PBT toughening agents according to claims 1-5, characterized in that: The following steps are involved: S1, preparation of raw material mixture, adding ethylene octene copolymer, EPDM rubber and silicone in proportion into a high-speed mixer, and stirring them thoroughly for standby use; S2. Preparation of a graft monomer mixture: adding weighed glycidyl methacrylate, styrene, γ-methacryloxypropyltrimethoxysilane and initiator to a liquid mixing device and stirring thoroughly for later use; S3, preparation of PBT toughening agent, adding the prepared grafted monomer mixture to the raw material mixture, during this process the high-speed mixer is still at 900 rpm, the direct monomer mixture is added within 1 minute, mixed and stirred for 3 minutes, then extruded and pelletized by a twin-screw extruder, and finally dried to obtain the toughening agent.

7. The method for preparing a PBT toughening agent according to claim 6, wherein: In step S1, the rotation speed of the high-speed mixer is 900 rpm, and the mixing time is 1 min.

8. The method for preparing a PBT toughening agent according to claim 6, wherein: In the step S3, the main engine speed of the twin-screw extruder is 350 rpm, the feeding speed is 35 rpm, the cutting speed is 400 rpm, and the vacuum degree is 0.6 MPa.

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