KR950002611B1 - Method of producing low-viscosity polyester - Google Patents
Method of producing low-viscosity polyester Download PDFInfo
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- KR950002611B1 KR950002611B1 KR1019910014390A KR910014390A KR950002611B1 KR 950002611 B1 KR950002611 B1 KR 950002611B1 KR 1019910014390 A KR1019910014390 A KR 1019910014390A KR 910014390 A KR910014390 A KR 910014390A KR 950002611 B1 KR950002611 B1 KR 950002611B1
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- polyester
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- low viscosity
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/88—Post-polymerisation treatment
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
Description
본 발명은 저점도의 폴리에스테르를 제조하는 방법에 관한 것으로서, 더욱 상세하게는 기존의 폴리에스테르 용융물에 디메틸테레프탈레이트(이하, DMT라 함)를 투입하므로써 저점도 폴리에스테르를 연속적으로 얻을 수 있는 제조방법에 관한것이다.The present invention relates to a method for producing a low-viscosity polyester, and more particularly, to prepare a low-viscosity polyester continuously by injecting dimethyl terephthalate (hereinafter referred to as DMT) into an existing polyester melt. It's about how.
일반적으로 저점도 폴리에스테르는 양모와 같은 혼방 방적사에 이용되는 항필링(Antipilling)사 제조에 널리 이용되고 있다.In general, low-viscosity polyester is widely used in the production of anti-pilling (anti-pilling) company used for blended yarns such as wool.
종래 저점도 폴리에스테르를 제조할시 중합단계에서 중합도 조절이나 단량체의 구조변화를 통해서 저점도 폴리에스테르를 합성 제조 사용하여 왔다.Conventionally, when preparing low viscosity polyester, low viscosity polyester has been synthesized and used through polymerization degree control or monomer structure change in the polymerization step.
그러나, 이러한 종래의 방법들은 일반 폴리에스테르 제조후 저점도 폴리에스테르를 생산할때 중합 반응기의 세척 등으로 인하여 연속작업이 곤란한 문제점이 있어서, 대규모로 연속생산하는 공정에 이용하기에는 불가능 하였다.However, these conventional methods have a problem that the continuous operation is difficult due to the washing of the polymerization reactor, etc. when producing a low-viscosity polyester after the general polyester production, it is impossible to use in a continuous production process on a large scale.
이러한 문제점을 해결하기 위하여 비스(2-하이드록시에틸) 테레프탈레이트(이하, BHET라 함)를 이용하여 폴리에스테르의 가글리콜 분해반응을 이용한 저점도 폴리에스테르를 제조하는 방법도 제안되고 있으나, 이는 BHET의 제조 공정상 어려움으로 인하여 비용이 많이 드는 단점이 있을 뿐만아니라 특히 BHET의 강한 흡습성으로 인한 보관상의 어려움과 이로 인한 제조칩의 물성이 저하되는 문제가 있었다.In order to solve this problem, a method of preparing a low-viscosity polyester using a glycol glycol decomposition reaction of a polyester using bis (2-hydroxyethyl) terephthalate (hereinafter referred to as BHET) has been proposed, but this method has been proposed. Due to the difficulty of the manufacturing process, not only has a costly disadvantage, but also has a problem of storage difficulties due to the strong hygroscopicity of the BHET and the physical properties of the resulting manufacturing chip.
따라서, 본 발명은 이러한 종래의 문제점을 개선하기 위해 중합공정과 방사 공정 사이의 일반 폴리에스테르 용융물에 기존의 도징 머신(Dosing machine)을 이용하여 DMT를 투입하여 혼합기(Extruder)를 거치는 동안의 용융 혼합시 폴리에스테르의 에스테르 교환반응을 이용하여 저점도 폴리에스테르를 연속적으로 얻을 수 있는 제조방법을 제공하는데 그 목적이 있다.Therefore, the present invention is to melt melt during the extruder by injecting DMT using a conventional dosing machine to the general polyester melt between the polymerization process and spinning process to improve this conventional problem It is an object of the present invention to provide a method for continuously obtaining low-viscosity polyester using transesterification of raw polyester.
이하, 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.
본 발명은 점도가 낮은 폴리에스테르를 제조함에 있어서, 통상의 폴리에스테르 용융물에다 이에 대해 0.05∼10중량%의 디메틸테레프탈레이트(DMT)를 투입하여 폴리에스테르의 점도를 강하시켜서 저점도의 폴리에스테르를 연속적으로 제조하는 것을 그 특징으로 한다.In the present invention, in the production of low viscosity polyester, 0.05 to 10% by weight of dimethyl terephthalate (DMT) is added to a conventional polyester melt, and the viscosity of the polyester is lowered to continuously produce low viscosity polyester. It is characterized by manufacturing as.
이와 같은 본 발명을 더욱 상세히 설명하면 다음과 같다.Referring to the present invention in more detail as follows.
본 발명은 점도 강하시에 폴리에스테르의 물성에 미치는 영향을 최소화하고자하여 폴리에스테르의 구조와 유사하고 투입상태가 분말인 DMT를 폴리에스테르 용융물의 중합공정후 방사공정 전에 투입하여 다음 반응식(I)과 같은 에스테르 교환반응을 이용하여 짧은시간(1∼10분)내에 다양한 저점도 폴리에스테르를 연속적으로 제조하는 방법에 관한 것이다.The present invention is to minimize the effect on the physical properties of the polyester when the viscosity is strong, the DMT, which is similar to the structure of the polyester and the powdered state is added before the spinning process after the polymerization process of the melt of the polyester and the following reaction formula (I) and It relates to a method for continuously producing various low viscosity polyesters in a short time (1 to 10 minutes) using the same transesterification reaction.
〈반응식 I 〉<Scheme I>
CH3OOCC6H4COOCH3+ -OOCC6H4COOCH2CH2OOC- ↔ -COOCH3+CH3OOCC6H4COO-CH 3 OOCC 6 H 4 COOCH 3 + -OOCC 6 H 4 COOCH 2 CH 2 OOC- ↔ -COOCH 3 + CH 3 OOCC 6 H 4 COO-
상기 반응식(I)에서 DMT의 에스테르가 폴리에스테르의 에스테르 결합을 공격하여 폴리에스테르 사슬을 절단하여 저점도의 폴리에스테르가 형성되는 것이다.In Scheme (I), the ester of DMT attacks the ester bond of the polyester, thereby cutting the polyester chain to form a low viscosity polyester.
이때 DMT는 폴리에스테르 용융물에 대해 0.05∼10중량%를 투입하는바, 그 투입량이 0.05중량% 미만이면 바라는 점도의 점도 강하 효과를 얻을 수 없고, 10중량%를 초과하면 고유점도가 약 0.63에서 약 0.35로 크게 강하되기는 하지만 DMT 자체가 열분해를 수반함으로써 폴리에스테르 용융물에 연쇄적인 열분해를 일으켜 분자량 분포가 약 3.2에서 6.2정도로 증가하고, 산가가 약 30에서 약 80정도로 증가하여, 방사후 연신시에 사절의 직접적인 원인이 되어 작업성이 떨어지게 된다.At this time, DMT is added in the amount of 0.05 to 10% by weight based on the polyester melt, if the amount is less than 0.05% by weight can not obtain the viscosity drop effect of the desired viscosity, if it exceeds 10% by weight intrinsic viscosity is about 0.63 Although drastically lowered to 0.35, DMT itself is accompanied by pyrolysis, causing chain pyrolysis of the polyester melt, increasing the molecular weight distribution from about 3.2 to about 6.2, and increasing the acid value from about 30 to about 80, It is a direct cause of deterioration of workability.
예를 들면, 고유점도가 0.63인 일반폴리에스테르 용융물에 DMT를 0.5중량% 투입하면 용융 혼합기(Extruder)를 거치는 동안 약 1.0정도의 점도 하락이 발생하게 되는데,이 정도의 칩은 항필링(Antipilling)사의 특성과 유사하지만 10중량%를 초고하여 투입시는 점도의 하락 정도와 분자량 분포 및 산가의 변화가 커서 실을 형성 할 수가 없다.For example, if 0.5% by weight of DMT is added to a general polyester melt with an intrinsic viscosity of 0.63, a viscosity drop of about 1.0 occurs during the melt extruder, and this chip is anti-pilling. It is similar to the characteristics of the yarn, but when it is added at an ultra high 10% by weight, the degree of viscosity drop, molecular weight distribution, and acid value change are large, and thus a yarn cannot be formed.
이와 같은 본 발명에 의하면 저렴한 제조비용으로 다양한 저점도의 폴리에스테르를 연속적으로 제조할 수 있기 때문에 산업적 적용이 가능하여 대량 생산할 수 있는 장점이 있다.According to the present invention as described above it is possible to manufacture a variety of low-viscosity polyester at a low manufacturing cost, there is an advantage that can be industrially applied to mass production.
이하, 본 발명을 실시예에 의해 더욱 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in more detail with reference to Examples.
실시예 1Example 1
산가 28.5, 고유점도 0.63, 분자량 분포 3.25인 폴리에스테르 1kg, DMT 5g을 도징머신을 통해 투입하여 방사 교반기를 거친후 칩상태로 얻어 물성을 분석 하였다.The acid value 28.5, intrinsic viscosity 0.63, 1kg polyester with a molecular weight distribution of 3.25, DMT 5g was added through a dosing machine and passed through a spinning stirrer to obtain a chip state and analyzed physical properties.
실시예 2∼3, 비교예 1∼2Examples 2-3 and Comparative Examples 1-2
DMT의 투입량을 다음 표1과 같이 하고 상기 실시예1과 동일하게 실시하였다.Dosing amount of DMT was as shown in Table 1 and was performed in the same manner as in Example 1.
* 상기표에서 산가는 칩을 KOH 적정법으로 얻었으며 분자량분포는 GPC(Gel Permeation Chromato-graphy)에 의해 얻었다.* The acid value in the table was obtained by KOH titration method and the molecular weight distribution was obtained by GPC (Gel Permeation Chromato-graphy).
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019910014390A KR950002611B1 (en) | 1991-08-21 | 1991-08-21 | Method of producing low-viscosity polyester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019910014390A KR950002611B1 (en) | 1991-08-21 | 1991-08-21 | Method of producing low-viscosity polyester |
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| Publication Number | Publication Date |
|---|---|
| KR930004352A KR930004352A (en) | 1993-03-22 |
| KR950002611B1 true KR950002611B1 (en) | 1995-03-23 |
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| Application Number | Title | Priority Date | Filing Date |
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| KR1019910014390A KR950002611B1 (en) | 1991-08-21 | 1991-08-21 | Method of producing low-viscosity polyester |
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| KR (1) | KR950002611B1 (en) |
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- 1991-08-21 KR KR1019910014390A patent/KR950002611B1/en not_active IP Right Cessation
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| KR930004352A (en) | 1993-03-22 |
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