JP2006199973A5

JP2006199973A5 -

Info

Publication number: JP2006199973A5
Application number: JP2006125107A
Authority: JP
Filing date: 2006-04-28
Publication date: 2007-11-08

Description

本発明者等は、前記現状に鑑みて鋭意検討した結果、溶融重縮合樹脂を固相重縮合反応に供したとき、化学反応速度論におけるアレニウスの式、ｋ＝Ａ exp（−ΔＥ／ＲＴ）〔ここで、ｋは速度定数、Ａは頻度因子、ΔＥは活性化エネルギー、Ｒは気体定数、Ｔは絶対温度である。〕の活性化エネルギーΔＥと頻度因子Ａとが特定の関係を有する溶融重縮合樹脂を固相重縮合反応させることによりその速度定数ｋを大きくし、前記目的を達成できることを見出し本発明に到達したもので、即ち、本発明は、テレフタル酸を主成分とするジカルボン酸成分とエチレングリコールを主成分とするジオール成分とを、エステル化反応させた後、重縮合触媒の存在下に溶融重縮合反応させ、引き続いて固相重縮合反応させてポリエステル樹脂を製造するにおいて、固有粘度が０．１〜０．７ｄｌ／ｇであって、固相重縮合反応に供したときの活性化エネルギーΔＥと頻度因子Ａとが下記式を満足する溶融重縮合樹脂を固相重縮合反応させ、固有粘度が０．５〜１．５ｄｌ／ｇで、色調がハンターの色差式における色座標ｂ値で−１０〜３の固相重縮合樹脂となすポリエステル樹脂の製造方法、を要旨とする。
ｌｎＡ／ΔＥ≧０．８０〔モル／（ｋｃａｌ・時間）〕 As a result of intensive studies in view of the above situation, the present inventors have found that when the melt polycondensation resin is subjected to a solid phase polycondensation reaction, the Arrhenius equation in chemical kinetics, k = A exp (−ΔE / RT) [Where k is the rate constant, A is the frequency factor, ΔE is the activation energy, R is the gas constant, and T is the absolute temperature. The rate constant k can be increased by subjecting the melt polycondensation resin having a specific relationship between the activation energy ΔE and the frequency factor A to a solid phase polycondensation reaction, and the above object can be achieved. That is, in the present invention, a dicarboxylic acid component mainly composed of terephthalic acid and a diol component mainly composed of ethylene glycol are esterified and then subjected to a melt polycondensation reaction in the presence of a polycondensation catalyst. In the production of a polyester resin by subsequent solid-phase polycondensation reaction, the intrinsic viscosity is 0.1 to 0.7 dl / g, and the activation energy ΔE and frequency when subjected to the solid-phase polycondensation reaction A melt polycondensation resin satisfying the following formula with factor A is subjected to solid phase polycondensation reaction, the intrinsic viscosity is 0.5 to 1.5 dl / g , and the color tone is -10 in the color coordinate b value in Hunter's color difference formula. The method of manufacturing a polyester resin formed by the ~ 3 solid phase polycondensation resins, and the gist.
lnA / ΔE ≧ 0.80 [mol / (kcal · time)]

又、色調が、ハンターの色差式における色座標ｂ値で、−１０〜３、好ましくは−５〜２、特に好ましくは−３〜２であり、又、アセトアルデヒド含有量が、好ましくは５ｐｐｍ以下、更に好ましくは３ｐｐｍ以下、特に好ましくは２ｐｐｍ以下であり、又、環状三量体含有量が、好ましくは０．５０重量％以下、更に好ましくは０．４０重量％以下、特に好ましくは０．３５重量％以下のものとなる。 Furthermore, color tone, color coordinate value b of the color difference formula Hunter, - 10-3, good Mashiku is -5～2, particularly preferably -3～2, also the acetaldehyde content, preferably 5ppm In the following, it is more preferably 3 ppm or less, particularly preferably 2 ppm or less, and the cyclic trimer content is preferably 0.50 wt% or less, more preferably 0.40 wt% or less, particularly preferably 0. 35% by weight or less.

Claims

An esterification reaction between a dicarboxylic acid component containing terephthalic acid as the main component and a diol component containing ethylene glycol as the main component is followed by a melt polycondensation reaction in the presence of a polycondensation catalyst, followed by a solid-phase polycondensation reaction. In the production of the polyester resin, the intrinsic viscosity is 0.1 to 0.7 dl / g, and the activation energy ΔE and the frequency factor A when subjected to the solid phase polycondensation reaction satisfy the following formula: The melt polycondensation resin is subjected to a solid phase polycondensation reaction to obtain a solid phase polycondensation resin having an intrinsic viscosity of 0.5 to 1.5 dl / g and a color tone of -10 to 3 in terms of color coordinate b value in Hunter's color difference formula. A method for producing a polyester resin.
lnA / ΔE ≧ 0.80 [mol / (kcal · time)]