Synthetic resins or natural rubbers -- part of the class 520 ser – Synthetic resins – Mixing of two or more solid polymers; mixing of solid...
Reexamination Certificate
2001-04-24
2003-07-15
Sellers, Robert E. L. (Department: 1712)
Synthetic resins or natural rubbers -- part of the class 520 ser
Synthetic resins
Mixing of two or more solid polymers; mixing of solid...
C525S438000, C525S450000
Reexamination Certificate
active
06593434
ABSTRACT:
BACKGROUND OF THE INVENTION
The present invention No. I relates to an efficient method for the preparation of a polyester block copolymer which is excellent in heat resistance and hydrolysis resistance, in which lactones are addition-polymerized onto a crystalline aromatic polyester.
The present invention No. II relates to a method for the preparation of a polyester block copolymer which is excellent in heat resistance and hydrolysis resistance, and which has a higher molecular weight, in which the polyester block copolymer obtained in the present invention No. I is further allowed to react in a solid state.
The present invention No. III relates to a polyester block copolymer composition which is excellent in heat resistance and hydrolysis resistance, color hue, and melt viscosity stability, and a method for the preparation thereof.
The present invention No. IV relates to a polyester block copolymer composition which is excellent in heat resistance under a contact with a metal and a polyvinyl chloride (PVC), and relates to a heat-sensitive body for a heater cable in which polyester block copolymer-based resin is employed.
The present invention Nos. V and VI relate to a polyester block copolymer composition which is excellent in a blow-moldability and heat resistance.
The present invention No. VII relates to a polyester block copolymer composition composed of a crystalline aromatic polyester and lactones, and relates to a method for the preparation thereof, and which is excellent in a blow-moldability and heat resistance.
BACKGROUND TECHNOLOGY
Prior arts in relation to the present invention Nos. I and II are as follows.
Many polyester block copolymers possesses a mechanical property such as flexibility, and widely enlarge uses such as parts for cars and electric and electronic parts as a thermoplastic elastomer which is excellent in heat resistance and chemical resistance, which contains a crystalline aromatic polyester unit such as a polybutylene terephthalate unit as a hard segment, and in which crystallinity is lowered by combination of a long chain diol with an aromatic dicarboxylic acid in spite of an aliphatic polyether such as a poly(alkyleneoxide) glycol, and/or an aliphatic polyester such as a polylactone and/or a polyester, and an aromatic polyester.
Hitherto, as a technology for giving flexibility to a crystalline aromatic polyester, JP-B-73004116 Official Gazette states a method for obtaining a block copolymer having a elasticity by reaction of a crystalline aromatic polyester with lactones. The method stated herein is a first method which shows that a block copolymer can be obtained by an addition reaction of lactones, however, there is nothing described in relation to an importance of residual unreacted lactone monomers after the above-described reaction and a technical effect, and there is also nothing described in relation to a melting point in the block copolymer obtained.
On the other hand, JP-B-77049037 Official Gazette describes a method for polymerizing lactones under the presence of a crystalline aromatic polyester which is in a solid phase. By descriptions, it is shown that a method in which a reaction is conducted in a melting state has a problem of a remarkable decline in a melting point of the crystalline aromatic polyester, and it can be solved by conducting a reaction under a solid condition.
However, it includes a problem that since it is a reaction at a low temperature, there is required a long time of period in the reaction, and since productivity is worse, and it lacks practicability.
Further, JP-B-96009661, JP-B-93023289, JP-B-93023290, JP-B-95033434, JP-B-94033435, JP-A-05043666, and JP-A-05043667 Official Gazettes all describe a method for allowing to continuously react a crystalline aromatic polyester with lactones, and some of the Gazettes include descriptions including a step for removing unreacted lactones. Removal of the unreacted lactone described herein has an effect for reducing a monomer smell in the polyester block copolymer and, moreover, by conducting a continuous removal operation, it has an effect for further reducing concentration of the unreacted lactones in the polyester block copolymer.
Still further, some of the above-described prior arts describe that there is included a step for conducting a polycondensation reaction in a solid state, and the polycondensation reaction in a solid state has an effect for increasing a solution viscosity of a polyester block copolymer (P1).
However, all of the prior arts only describe that a thermal property such as a melting point of a resin obtained are decided by raw materials to be employed, reaction temperature, reaction time of period, and conditions for removing unreacted lactones, and all the prior arts do not describe a technical concept and a specific method for intentionally improving the thermal property by increasing the amount of the lactones to be introduced and by remaining the amount of the unreacted lactones.
In JP-A-02252729 and JP-A-04072325 Official Gazettes, there is described a method for elevating a melting point of a block copolymer obtained. The JP-A-02252729 Official Gazette describes a method in which there are dissolved a crystalline aromatic polyester and lactones at a lower temperature, and those have an effect for reducing decomposition reaction by heating, however, there is small an effect for preventing a decline of a melting point, further, occasionally, a reaction time of period unpreferably becomes long. Further, the JP-A-04072325 Official Gazette describes that the lactones is partially added in advance in a highly-polymerized state, and elevation of a melting point can be effectively actualized. However, in spite of an inherent low cost in the lactones, the method partially highly-polymerized in advance includes a problem of a fair adverse affection to total profitability.
JP-A-61287922 Official Gazette describes that in a method for the preparation of an elastic polyester by allowing to react a crystalline aromatic polyester with lactones, the method for the preparation of an elastic polyester characterized in that an addition polymerization is conducted by continuously feeding a melted crystalline polyester and lactones into a reaction vessel, and then, those are allowed to react with each other in a solid state.
However, even in the method, there are not shown a technical concept and a specific method, etc., that thermal properties are intentionally elevated by increasing the amount of the lactones and by remaining the amount of unreacted lactones.
As described hereinabove, those have been still insufficient as a method for the preparation of a polyester block copolymer having a high melting point and a high molecular weight.
Prior arts in relation to the present invention No. III are as follows.
However, in relation to the polyester block copolymer composed of a hard segment and a soft segment described in the prior arts for the present invention No. I, an industrially-produced polymer is not sufficient in heat resistance and hydrolysis resistance, and, in the case that it is applied to a melting molding method such as a blow molding and extrusion molding in which a high melt viscosity is required, there has been caused a problem that moldability is worse.
Accordingly, as a method for elevating a heat resistance and hydrolysis resistance in a polyester block copolymer, there have been proposed a variety of methods until now. Further, there are proposed methods simultaneously elevating a melt viscosity in the many proposes. For example, JP-B-77030999 and the above-described JP-B-77049037 Official Gazettes propose a method for increasing a melt viscosity by a solid phase polymerization. However, in the method for increasing a melt viscosity proposed herein, there is required a very long time of period for heating and, further, hydrolysis resistance is not improved at all.
JP-B-91077826 Official Gazette proposes a method for melt-mixing a monofunctional epoxy compound with a bifunctional epoxy compound. By the method, although heat resistance and hydrol
Daicel Chemical Industries Ltd.
Morgan & Finnegan L.L.P.
Sellers Robert E. L.
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