KR20200046622A - Analysis method for polymer end-group - Google Patents
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- 229920000642 polymer Polymers 0.000 title claims abstract description 40
- 238000004458 analytical method Methods 0.000 title claims description 14
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000000605 extraction Methods 0.000 claims description 11
- 238000001226 reprecipitation Methods 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 6
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 claims description 4
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 claims description 4
- 239000012634 fragment Substances 0.000 claims description 3
- 238000000197 pyrolysis Methods 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims 2
- 238000004090 dissolution Methods 0.000 abstract description 3
- 239000004734 Polyphenylene sulfide Substances 0.000 description 10
- 229920000069 polyphenylene sulfide Polymers 0.000 description 10
- 238000005481 NMR spectroscopy Methods 0.000 description 7
- 239000004417 polycarbonate Substances 0.000 description 5
- 229920000515 polycarbonate Polymers 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000010306 acid treatment Methods 0.000 description 3
- 238000004949 mass spectrometry Methods 0.000 description 3
- CJWNFAKWHDOUKL-UHFFFAOYSA-N 2-(2-phenylpropan-2-yl)phenol Chemical compound C=1C=CC=C(O)C=1C(C)(C)C1=CC=CC=C1 CJWNFAKWHDOUKL-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- QHPQWRBYOIRBIT-UHFFFAOYSA-N 4-tert-butylphenol Chemical compound CC(C)(C)C1=CC=C(O)C=C1 QHPQWRBYOIRBIT-UHFFFAOYSA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical group 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000001840 matrix-assisted laser desorption--ionisation time-of-flight mass spectrometry Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000000045 pyrolysis gas chromatography Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
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- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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Abstract
Description
본 발명은 고분자 말단기 성분을 분석하는 방법에 관한 것이다.The present invention relates to a method of analyzing polymer end group components.
고분자 말단기 성분을 분석하는 방법으로는 일반적으로 핵자기공명 분석법(nuclear magnetic resonance, NMR), 말디토프 질량 분석법(Matrix-assisted laser desorption/ionization-time-of-flight mass spectrometry, MALDI-TOF MS) 등을 사용한다.As a method of analyzing the polymer end group components, nuclear magnetic resonance (NMR) and malditope mass spectrometry (MALDI-TOF MS) are generally used. Etc. are used.
NMR 분석의 경우 정성분석과 함께 정량분석을 할 수 있다는 장점을 가지지만, 고분자가 용매에 반드시 녹아야 한다는 제한점이 있으므로 분자량이 크거나 난용 특성을 가지는 수지와 같은 물질은 분석이 어렵다는 큰 단점이 있다.In the case of NMR analysis, it has the advantage of being capable of quantitative analysis together with qualitative analysis, but has a limitation in that polymers must be dissolved in a solvent. .
또한, 말디토프 질량 분석법은 고분자가 용매에 녹지 않아도 분석이 가능하다는 장점이 있으나, 이온화가 어렵다는 단점이 있다.In addition, malditop mass spectrometry has an advantage in that it can be analyzed even if the polymer is not dissolved in a solvent, but has a disadvantage that ionization is difficult.
그러므로, 상기와 같은 단점을 극복하고 간단한 방법으로 말단기 성분을 확인할 수 있는 방법이 요구된다.Therefore, there is a need for a method that overcomes the above drawbacks and can identify the end group components in a simple way.
본 발명의 목적은 고분자의 말단기 성분을 분석할 수 있는 방법을 제공하는 것이다.An object of the present invention is to provide a method for analyzing the end group component of the polymer.
상기 과제를 해결하기 위하여, 본 발명은In order to solve the above problems, the present invention
고분자로부터 올리고머 성분을 추출하는 추출 단계;An extraction step of extracting the oligomer component from the polymer;
상기 올리고머 성분을 분석하는 분석 단계; 및An analysis step of analyzing the oligomer component; And
상기 분석 결과로부터 단편(fragments)들을 해석하여 말단기 구조를 확인하는 단계를 포함하는, 고분자 말단기 분석 방법을 제공한다.It provides a method for analyzing a polymer end group, comprising the steps of analyzing the fragments from the analysis results to confirm the end group structure.
일구현예에 따르면, 상기 추출 단계는 저온분쇄, 초음파, 마이크로파, 쉐이킹 및 재침전으로 이루어지는 군으로부터 선택되는 하나 이상의 방법을 포함할 수 있다. 예를 들면, 상기 추출 단계는 가용성 고분자로부터 재침전법으로 올리고머 성분을 추출하는 단계를 포함할 수 있다. 또 다른 예를 들면, 상기 추출 단계는 난용성 고분자를 저온 분쇄한 후, 초음파 또는 마이크로파를 가하여 올리고머 성분을 추출하는 단계를 포함할 수 있다.According to one embodiment, the extraction step may include one or more methods selected from the group consisting of low temperature pulverization, ultrasound, microwave, shaking and reprecipitation. For example, the extraction step may include the step of extracting the oligomer component from the soluble polymer by reprecipitation. For another example, the extraction step may include the step of pulverizing the poorly soluble polymer at a low temperature, and then extracting an oligomer component by adding ultrasonic waves or microwaves.
일구현예에 따르면, 상기 분석 단계는 GC-MS, 열분해 GC-MS, LC-MS, FT-IR 또는 이들의 조합을 실시하는 단계를 포함할 수 있다.According to one embodiment, the analyzing step may include performing GC-MS, pyrolysis GC-MS, LC-MS, FT-IR, or a combination thereof.
본 발명의 다른 구현예에 따르면, 상기와 같은 방법에 따른 방법을 적용한 시스템을 제공할 수 있다.According to another embodiment of the present invention, it is possible to provide a system to which a method according to the above method is applied.
기타 본 발명의 구현예들의 구체적인 사항은 이하의 상세한 설명에 포함되어 있다.Other specific details of the embodiments of the present invention are included in the following detailed description.
본 발명은 고분자에 대하여 용해 특성 및 이온화 여부에 관계없이 고분자의 말단기 성분을 확인할 수 있다. 그러므로 시료의 분자량을 간단하게 측정할 수 있고, 고분자의 말단기를 전환하는 경우 상대 분자량을 예측할 수 있으며, 타 공정을 확인하는 데 유용하게 적용할 수 있다.The present invention can confirm the end group component of the polymer regardless of the dissolution characteristics and ionization of the polymer. Therefore, it is possible to simply measure the molecular weight of the sample, predict the relative molecular weight when converting the end groups of the polymer, and can be usefully applied to confirm other processes.
도 1은 실시예 1에 따른 GC/MS 결과를 나타내는 그래프이다.
도 2 및 3은 실시예 2에 따른 GC/MS 결과를 나타내는 그래프이다.
도 4는 비교예 1에 따른 NMR 결과를 나타내는 그래프이다.1 is a graph showing GC / MS results according to Example 1.
2 and 3 are graphs showing GC / MS results according to Example 2.
4 is a graph showing NMR results according to Comparative Example 1.
본 발명은 다양한 변환을 가할 수 있고 여러 가지 실시예를 가질 수 있는 바, 특정 실시예를 도면에 예시하고 상세한 설명에 상세하게 설명하고자 한다. 그러나, 이는 본 발명을 특정한 실시 형태에 대해 한정하려는 것이 아니며, 본 발명의 사상 및 기술 범위에 포함되는 모든 변환, 균등물 내지 대체물을 포함하는 것으로 이해되어야 한다. 본 발명을 설명함에 있어서 관련된 공지 기술에 대한 구체적인 설명이 본 발명의 요지를 흐릴 수 있다고 판단되는 경우 그 상세한 설명을 생략한다.The present invention can be applied to various conversions and can have various embodiments, and specific embodiments will be illustrated in the drawings and described in detail in the detailed description. However, this is not intended to limit the present invention to specific embodiments, and should be understood to include all conversions, equivalents, and substitutes included in the spirit and scope of the present invention. In the description of the present invention, when it is determined that a detailed description of known technologies related to the present invention may obscure the subject matter of the present invention, the detailed description will be omitted.
이하, 본 발명의 구현예에 따른 고분자 말단기 분석 방법에 대하여 보다 상세하게 설명한다.Hereinafter, a method for analyzing a polymer end group according to an embodiment of the present invention will be described in more detail.
본 발명은, 고분자로부터 올리고머 성분을 추출하는 추출 단계;The present invention, the extraction step of extracting the oligomer component from the polymer;
상기 올리고머(oligomer) 성분을 분석하는 분석 단계; 및An analysis step of analyzing the oligomer component; And
상기 분석 결과로부터 단편(fragments)들을 해석하여 말단기 구조를 확인하는 단계를 포함하는, 고분자 말단기 분석 방법을 제공한다.It provides a method for analyzing a polymer end group, comprising the steps of analyzing the fragments from the analysis results to confirm the end group structure.
일구현예에 따르면, 상기 추출 단계는 저온 분쇄(freeze milling), 초음파(sonication), 마이크로파(micro wave), 쉐이킹(shaking) 및 재침전(reprecipitaion)으로 이루어지는 군으로부터 선택되는 하나 이상의 방법을 포함할 수 있다. 구체적으로 예를 들면, 가용성 고분자로부터 재침전법으로 올리고머 성분을 추출할 수 있다. 또한, 예를 들면, 난용성 고분자를 저온 분쇄한 후, 초음파 또는 마이크로파를 가하여 올리고머 성분을 추출하는 단계를 포함할 수 있다. 저온 분쇄법은 액체질소 등 불활성 가스 냉매를 이용하여 시료를 동결시킨 상태에서 물리적인 힘을 가하여 분쇄하는 방법이다. 초음파 또는 마이크로파 처리는 20kHz 이상 또는 300MHz 이상의 전자파로 고분자를 절단하는 방법이다. 쉐이킹법은 용매를 첨가하고 쉐이킹하여 고분자를 분해하는 방법이다. 재침전법은 용액 중의 침전물을 적당한 용매에 용해시킨 후 다시 침전시키는 방법이다.According to one embodiment, the extraction step may include one or more methods selected from the group consisting of freeze milling, sonication, microwave, shaking and reprecipitaion. You can. Specifically, for example, the oligomer component can be extracted from the soluble polymer by reprecipitation. In addition, for example, after low-temperature pulverization of the poorly soluble polymer, it may include the step of extracting the oligomer component by adding ultrasonic waves or microwaves. The low temperature grinding method is a method in which a sample is frozen using an inert gas refrigerant such as liquid nitrogen and then crushed by applying physical force. Ultrasonic or microwave treatment is a method of cutting a polymer with electromagnetic waves of 20 kHz or higher or 300 MHz or higher. The shaking method is a method of decomposing a polymer by adding a solvent and shaking. The reprecipitation method is a method in which a precipitate in a solution is dissolved in a suitable solvent and then precipitated again.
일구현예에 따르면, 상기 분석 단계는 GC-MS(gas chromatograph-mass spectrometry), 열분해 GC-MS(pyrolysis-GC/MS), LC-MS(Liquid chromatography-mass spectrometry), 푸리에 변환 적외분광법(fourier transform infrared spectroscopy, FT-IR) 또는 이들을 조합한 방법을 실시하는 단계를 포함할 수 있다.According to one embodiment, the analysis step is GC-MS (gas chromatograph-mass spectrometry), pyrolysis GC-MS (pyrolysis-GC / MS), LC-MS (Liquid chromatography-mass spectrometry), Fourier transform infrared spectroscopy (fourier) transform infrared spectroscopy (FT-IR) or a combination thereof.
일구현예에 따르면, 시료로서 사용할 수 있는 고분자의 예로 폴리카보네이트(PC) 수지, 폴리페닐렌 설파이드(polyphenylene sulfide, PPS) 수지 등을 포함할 수 있으나, 분석 가능한 고분자의 종류는 특별히 제한되지 않는다.According to one embodiment, examples of a polymer that can be used as a sample may include polycarbonate (PC) resin, polyphenylene sulfide (PPS) resin, and the like, but the type of polymer that can be analyzed is not particularly limited.
본 발명의 다른 구현예에 따르면, 상기한 바와 같은 방법을 적용한 시스템을 제공함으로써 고분자의 용해 특성 및 이온화 여부 등에 관계없이 용이하게 말단기를 분석할 수 있다.According to another embodiment of the present invention, by providing a system to which the method as described above is applied, end groups can be easily analyzed regardless of polymer dissolution characteristics and ionization.
이하, 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자가 용이하게 실시할 수 있도록 본 발명의 실시예에 대하여 상세히 설명한다. 그러나 본 발명은 여러 가지 상이한 형태로 구현될 수 있으며 여기에서 설명하는 실시예에 한정되지 않는다.Hereinafter, embodiments of the present invention will be described in detail so that those skilled in the art to which the present invention pertains can easily practice. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein.
실시예 1Example 1
가용성 고분자로서 각각 PTBP 말단 폴리카보네이트(A사) 및 큐밀 페놀(cumyl phenol) 말단 폴리카보네이트(B사)를 사용하여 재침전법으로 올리고머 성분을 추출하였다. 추출한 올리고머 성분을 GC/MS(Agilent 7890A/5975C)로 측정하여 그 결과를 도 1에 나타내었다.As a soluble polymer, oligomer components were extracted by reprecipitation using PTBP terminal polycarbonate (Company A) and cumyl phenol terminal polycarbonate (Company B), respectively. The extracted oligomer component was measured by GC / MS (Agilent 7890A / 5975C) and the results are shown in FIG. 1.
실시예 2Example 2
난용성 고분자로서 폴리페닐렌 설파이드(PPS)를 사용하였다. PPS는 일반적으로 Cl 말단을 가지므로 추출 후 GC/MS 측정 시 -Cl말단을 쉽게 확인할 수 있다.Polyphenylene sulfide (PPS) was used as a poorly soluble polymer. Since PPS generally has a Cl terminal, the -Cl terminal can be easily confirmed when GC / MS is measured after extraction.
한편, PPS 합성 시 수지를 변형(modify)시켜 산(acid) 말단을 합성하기 위하여 산으로서 초산(acetic acid)로 세척할 수 있으며, 산 처리 시 카복실산(carboxyl acid)이 치환된 PPS가 생성될 수 있다.On the other hand, when synthesizing PPS, the resin can be washed with acetic acid as acid to synthesize acid ends by modifying the resin, and when acid treatment, PPS substituted with carboxylic acid can be generated. have.
PPS 고분자를 SPEX SAMPLE Prep 6850 Freezer Mill로 저온 분쇄한 후, Branson 5510 초음파 세척기로 초음파 처리하여 올리고머 성분을 추출하였다. 추출한 올리고머 성분을 GC/MS(Agilent 7890A/5975C)로 측정하였으며, 산을 처리한 PPS 분석 결과는 도 2에, 산을 처리하지 않은 PPS 분석 결과는 도 3에 나타내었다.After pulverizing the PPS polymer with a SPEX SAMPLE Prep 6850 Freezer Mill, the oligomer component was extracted by ultrasonic treatment with a Branson 5510 ultrasonic cleaner. The extracted oligomer components were measured by GC / MS (Agilent 7890A / 5975C), and the result of PPS analysis with acid treatment was shown in FIG. 2 and the result of PPS analysis without acid treatment was shown in FIG. 3.
비교예 1Comparative Example 1
가용성 고분자로서 폴리카보네이트를 사용하였다. 폴리카보네이트 고분자를 NMR 용매(Chloroform d, Euriso-Top)에 직접 녹여 NMR(Agilent 600MHz NMR)로 측정하였다. 도 4에 그 결과를 나타내었으며, 큐밀 페놀 (Cumyl phenol)과 페놀(phenol) 구조의 구분이 명확하게 나타나지 않음을 확인하였다.Polycarbonate was used as a soluble polymer. The polycarbonate polymer was directly dissolved in an NMR solvent (Chloroform d, Euriso-Top) and measured by NMR (Agilent 600 MHz NMR). The results are shown in FIG. 4, and it was confirmed that the distinction between the structure of cumyl phenol and phenol was not clearly seen.
상기한 바와 같이, 본 발명에 따른 방법의 의하면 고분자의 특성에 관계 없이 용이하게 고분자의 말단기를 분석할 수 있고, 정확도를 향상시킬 수 있다.As described above, according to the method according to the present invention, the end groups of the polymer can be easily analyzed regardless of the properties of the polymer, and accuracy can be improved.
이상으로 본 발명 내용의 특정한 부분을 상세히 기술한 바, 당 업계의 통상의 지식을 가진 자에게 있어서, 이러한 구체적 기술은 단지 바람직한 실시 양태일 뿐이며, 이에 의해 본 발명의 범위가 제한되는 것이 아닌 점은 명백할 것이다. 따라서 본 발명의 실질적인 범위는 첨부된 청구항들과 그것들의 등가물에 의하여 정의된다고 할 것이다.As described above in detail the specific parts of the present invention, for those skilled in the art, this specific technique is only a preferred embodiment, and it is obvious that the scope of the present invention is not limited thereby. something to do. Therefore, the substantial scope of the present invention will be defined by the appended claims and their equivalents.
Claims (6)
상기 올리고머 성분을 분석하는 분석 단계; 및
상기 분석 결과로부터 단편(fragments)들을 해석하여 말단기 구조를 확인하는 단계를 포함하는, 고분자 말단기 분석 방법.An extraction step of extracting the oligomer component from the polymer;
An analysis step of analyzing the oligomer component; And
And analyzing fragments from the analysis results to confirm the end group structure.
상기 추출 단계가 저온분쇄, 초음파, 마이크로파, 쉐이킹 및 재침전으로 이루어지는 군으로부터 선택되는 하나 이상의 방법을 포함하는 것인, 고분자 말단기 분석 방법.According to claim 1,
The extraction step comprises one or more methods selected from the group consisting of low temperature pulverization, ultrasound, microwave, shaking and reprecipitation, polymer end group analysis method.
상기 추출 단계가 가용성 고분자로부터 재침전법으로 올리고머 성분을 추출하는 단계를 포함하는 것인, 고분자 말단기 분석 방법.According to claim 1,
The extraction step comprises the step of extracting the oligomer component by reprecipitation from the soluble polymer, polymer end group analysis method.
상기 추출 단계가 난용성 고분자를 저온 분쇄한 후, 초음파 또는 마이크로파를 가하여 올리고머 성분을 추출하는 단계를 포함하는 것인, 고분자 말단기 분석 방법.According to claim 1,
The extraction step comprises a step of pulverizing the poorly soluble polymer at a low temperature, and then extracting an oligomer component by adding ultrasonic waves or microwaves.
상기 분석 단계가 GC-MS, 열분해 GC-MS, LC-MS, FT-IR 또는 이들의 조합을 실시하는 단계를 포함하는 것인, 고분자 말단기 분석 방법.According to claim 1,
The analysis step comprises a step of performing GC-MS, pyrolysis GC-MS, LC-MS, FT-IR, or a combination thereof, polymer end group analysis method.
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| KR20240057868A (en) | 2022-10-25 | 2024-05-03 | 에스케이케미칼 주식회사 | Method and system for automated analysis of polymer end-group |
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