Process for preparing polyphenylene ether microspore dispersion

Patent metadata

Field	Value
Publication number	US-9920218-B2
Application number	US-201615148050-A
Country	US
Kind code	B2
Filing date	May 6, 2016
Priority date	May 18, 2015
Publication date	Mar 20, 2018
Grant date	Mar 20, 2018

Abstract

A process for preparing PPE microspore dispersion includes steps of: dissolving a high-molecular polyphenylene ether in a first solvent at 45-110° C. to form a dissolution liquid; adding processing aids and well mixing the dissolution liquid into a dispersed phase; cooling the dissolution liquid to 42-80° C., and adding a second solvent to generate PPE microspores via PPE to wrap around the processing aids; cooling the dissolution liquid to 0-40° C. to obtain PPE microspore dispersions for use in application for impregnation processes performed below 40° C., thereby high-temperature impregnation equipment are no longer needed, and copper clad laminates made of using the PPE microspore dispersion enjoy excellent physical properties including high Tg, low Dk, low Df and high copper foil's peel strength.

First claim

What is claimed is:

1. A process for preparing a polyphenylene ether microspore dispersion comprising the following steps:
(a) selecting a high-molecular polyphenylene ether (HM-PPE) that has a number-average molecular weight (Mn) ranging between 12,000 g/mole and 30,000 g/mole, and a low-molecular polyphenylene ether (LR-PPE) that has a number-average molecular weight (Mn) ranging between 800 g/mole and 6,000 g/mole, respectively;
(b) selecting a first solvent that dissolves the HM-PPE at 45-110° C., and selecting a second solvent that does not dissolve the HM-PPE;
wherein the first solvent is one or more selected from the group consisting of benzene, methylbenzene, dimethylbenzene, trimethylbenzene and any combinations thereof; and
wherein the second solvent is one or more selected from the group consisting of dimethyl ketone, methyl ethyl ketone, methyl isobutyl ketone, ethanol, propanol, butanol, pentanol, hexanol, dimethylformamide, methylacetamide, diethylamide and any combinations thereof;
(c) dissolving the HM-PPE of Step (a) in the first solvent at a temperature ranging between 45° C. and 110° C. to form a PPE-based dissolution liquid;
(d) adding the LR-PPE of Step (a) and processing aids being chosen as additives together into the PPE-based dissolution liquid of Step (c), and then performing adequate agitation until the LR-PPE and the processing aids are evenly dispersed throughout the dissolution liquid;
wherein, the processing aids are one or more selected from the group consisting of a polybutadiene resin, a flame retardant, a filler, a crosslinking agent, an initiator and any combinations thereof;
(e) cooling the PPE-based dissolution liquid of Step (d) to a temperature ranging between 42° C. and 80° C., and adding the second solvent of Step (b) into the cooled PPE-based dissolution liquid of Step (d) under a weight ratio of the first solvent to the second solvent ranging between 0.10 and 2.0, to cause the PPE to wrap around the processing aids to form as PPE microspores occurred constantly in the PPE-based dissolution liquid; and
(f) cooling the PPE-based dissolution liquid of Step (e) to a temperature ranging between 0° C. and 40° C., so as to obtain the PPE microspore dispersion that is suitable for impregnation processes performed below 40° C.

2. The process for preparing a polyphenylene ether microspore dispersion of claim 1 , wherein the weight ratio of the first solvent to the second solvent ranges between 0.15 and 1.5.

3. The process for preparing a polyphenylene ether microspore dispersion of claim 1 , wherein the weight ratio of the first solvent to the second solvent ranges between 0.20 and 1.2.

4. The process for preparing a polyphenylene ether microspore dispersion of claim 1 , wherein the flame retardant is selected from a bromine-containing flame retardant, a phosphorus-containing flame retardant, an ammonium polyphosphate-based flame retardant, a melamine polyphosphate-based flame retardant, a melamine cyanurate-based flame retardant, a phosphonitrile-based flame retardant or an inorganic flame retardant.

5. The process for preparing a polyphenylene ether microspore dispersion of claim 1 , wherein the filler is one or more selected from the group consisting of SiO2, Al(OH)3, Al2O3, TiO2, Mg(OH)2 and CaCO3.

6. The process for preparing a polyphenylene ether microspore dispersion of claim 1 , wherein the crosslinking agent is one or more selected from the group consisting of triallyl isocyanurate (TAIC), triallyl cyanurate (TAC), trimethallyl isocyanurate (TMAIC), trimethylolpropane trimethacrylate (TMPTMA), divinyl benzene, divinyl naphthalene, diallyl phthalate and diallyl isocyanurate.

7. The process for preparing a polyphenylene ether microspore dispersion of claim 1 , wherein the initiator is selected from benzoyl peroxide (BPO), cumyl hydroperoxide (CHP), dicumyl peroxide (DCP), tert-butyl cumyl peroxide, imidazole (IMZ), triphenylphosphine (TPP), 2-methylimidazole (2MI), 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane (DHBP), 2,5-di(tert-butylperoxy)-2,5-dimethyl-3-hexyne, or 1,1-di-(tert-butylperoxy)-3,3,5-trimethylcyclohexane (TMCH).

8. The process for preparing a polyphenylene ether microspore dispersion of claim 1 , wherein the PPE microspore dispersion has a viscosity ranging between 10 Cps and 400 Cps.

9. The process for preparing a polyphenylene ether microspore dispersion of claim 8 , wherein the PPE microspore dispersion contains a solid content composed of the PPE microspores and non-PPE microspores, and the solid content takes up 30-70% by weight of the overall dispersion.

10. The process for preparing a polyphenylene ether microspore dispersion of claim 9 , wherein the PPE microspore contains the HM-PPE taken up more than 80%, by weight of the PPE microspore.

11. The process for preparing a polyphenylene ether microspore dispersion of claim 9 , wherein said PPE microspore dispersion contains those PPE microspores having a diameter of 0.5˜20 μm are taken up more than 70% by weight of the total PPE microspores dispersed in said PPE microspore dispersion.

Assignees

• Nanya Plastics Corp

Inventors

• Liao Te-Chao
• Chuang Jung-Jen
• Chen hao-sheng
• Li Yi-Cheng
• Huang zhang-jian

Classifications

• C08G65/485

  Polyphenylene oxides · CPC title

• C08G65/46 Primary

  Post-polymerisation treatment, e.g. recovery, purification, drying · CPC title

• C08L71/12

  Polyphenylene oxides · CPC title

• C09D171/12 Primary

  Polyphenylene oxides · CPC title

• C08J2471/12

  Polyphenylene oxides · CPC title