KR101818303B1 - A method for analyzing composition ratio of fatty acid tetraester with pentaerythritol in polymer resin - Google Patents
A method for analyzing composition ratio of fatty acid tetraester with pentaerythritol in polymer resin Download PDFInfo
- Publication number
- KR101818303B1 KR101818303B1 KR1020150131859A KR20150131859A KR101818303B1 KR 101818303 B1 KR101818303 B1 KR 101818303B1 KR 1020150131859 A KR1020150131859 A KR 1020150131859A KR 20150131859 A KR20150131859 A KR 20150131859A KR 101818303 B1 KR101818303 B1 KR 101818303B1
- Authority
- KR
- South Korea
- Prior art keywords
- pentaerythritol
- ftpe
- fatty acid
- polymer resin
- acid tetraester
- Prior art date
Links
- 235000014113 dietary fatty acids Nutrition 0.000 title claims abstract description 66
- 229930195729 fatty acid Natural products 0.000 title claims abstract description 66
- 239000000194 fatty acid Substances 0.000 title claims abstract description 66
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 150000004665 fatty acids Chemical class 0.000 title claims abstract description 59
- 239000002952 polymeric resin Substances 0.000 title claims abstract description 43
- 229920003002 synthetic resin Polymers 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000000203 mixture Substances 0.000 title description 8
- -1 pentaerythritol fatty acid Chemical class 0.000 claims abstract description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000004458 analytical method Methods 0.000 claims description 11
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 238000002347 injection Methods 0.000 claims description 9
- 239000007924 injection Substances 0.000 claims description 9
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 9
- 229920000515 polycarbonate Polymers 0.000 claims description 9
- 239000004417 polycarbonate Substances 0.000 claims description 9
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 6
- 238000005470 impregnation Methods 0.000 claims description 6
- 239000000314 lubricant Substances 0.000 claims description 5
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical compound C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 claims description 4
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- 229920005992 thermoplastic resin Polymers 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 238000000944 Soxhlet extraction Methods 0.000 claims description 2
- 229920006351 engineering plastic Polymers 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 238000001212 derivatisation Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000003908 quality control method Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 11
- 239000007789 gas Substances 0.000 description 10
- IPCSVZSSVZVIGE-UHFFFAOYSA-N n-hexadecanoic acid Natural products CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 9
- HPEUJPJOZXNMSJ-UHFFFAOYSA-N Methyl stearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC HPEUJPJOZXNMSJ-UHFFFAOYSA-N 0.000 description 6
- 235000021314 Palmitic acid Nutrition 0.000 description 5
- 235000021355 Stearic acid Nutrition 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical class CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Chemical class CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 5
- 239000008117 stearic acid Chemical class 0.000 description 5
- FLIACVVOZYBSBS-UHFFFAOYSA-N Methyl palmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC FLIACVVOZYBSBS-UHFFFAOYSA-N 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000012491 analyte Substances 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 3
- 230000005526 G1 to G0 transition Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 235000019387 fatty acid methyl ester Nutrition 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 239000013543 active substance Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000000769 gas chromatography-flame ionisation detection Methods 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000002535 lyotropic effect Effects 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000011987 methylation Effects 0.000 description 1
- 238000007069 methylation reaction Methods 0.000 description 1
- 150000002942 palmitic acid derivatives Chemical class 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000001226 reprecipitation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/44—Resins; Plastics; Rubber; Leather
- G01N33/442—Resins; Plastics
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Immunology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The present invention relates to a method for analyzing the component ratio of fatty acid tetraester (FTPE) of pentaerythritol contained in a polymer resin. According to the present invention, when analyzed without derivatization, the component ratio of pentaerythritol fatty acid tetraester (FTPE) And it is advantageous that the quality control can be facilitated in the synthesis and application of the polymer resin.
Description
The present invention relates to a method for analyzing the component ratio of fatty acid tetraester (FTPE) of pentaerythritol contained in a polymer resin.
When the thermoplastic resin is heat-molded, the lubricant is added as an additive in order to improve its flowability and increase the workability and to easily remove the molded article from the mold. Fatty acid tetraester with pentaerythritol (FTPE), a kind of lyotropic agent, is known as PPPP (C [(CH 2) 2 ), which is classified by the degree of substitution of palmitic acid and stearic acid O) COOC 15 H 31] 4 ), PPPS ([H 31 C 13 OOC (CH 2 O)] 3 C (CH 2 O) COOC 17 H 35), PPSS ([H 31 C 13 OOC (CH 2 O) ] 2 C [(CH 2 O) COOC 17 H 35 ] 2 ), PSSS (H 31 C 13 OOC (CH 2 O) C [(CH 2 O) COOC 17 H 35 ] 3 ) and SSSS 2 O) COOC 17 H 35 ] 4 ), and the components are contained in different ratios depending on the manufacturer and grade. Since the ratio of the fatty acid tetraester (FTPE) of pentaerythritol greatly affects the properties of the process and the polymer resin, it is necessary to develop an analysis method capable of obtaining information on the composition ratio accurately and promptly.
Since the molecular weight of the fatty acid tetraester (FTPE) of pentaerythritol is too high to be detected by a general gas chromatographic analysis method, methylation of the fatty acid tetraester (FTPE) of pentaerythritol is converted into a fatty acid methyl ester, To measure the ratio of palmitic acid and stearic acid.
However, in the conventional method, since the fatty acid tetraester (FTPE) of pentaerythritol was methylated to obtain the total ratio of palmitic acid and stearic acid contained in the fatty acid tetraester (FTPE) of pentaerythritol, the PPPP (C [(CH 2 O ) COOC 15 H 31] 4), PPPS ([H 31 C 13 OOC (CH 2 O)] 3 C (CH 2 O) 5 of components contained in the ester (FTPE) COOC 17 H 35), PPSS ([ H 31 C 13 OOC (CH 2 O)] 2 C [(CH 2 O) COOC 17 H 35] 2), PSSS (H 31 C 13 OOC (CH 2 O) C [( CH 2 O) COOC 17 H 35 ] 3 ) and SSSS (C [(CH 2 O) COOC 17 H 35 ] 4 ).
SUMMARY OF THE INVENTION An object of the present invention is to solve the above-
Analysis of Component Ratio of Pentaerythritol Fatty Acid Tetraester (FTPE) Contained in Polymer Resins, which can analyze the exact component ratio of the substance contained in the fatty acid tetraester (FTPE) of pentaerythritol used as a lubricant in the production of polymer resin in a short time and with high resolution Method.
In order to solve the above problems,
a) extracting a fatty acid tetraester (FTPE) of pentaerythritol represented by the following
b) analyzing the fatty acid tetraester (FTPE) of the extracted pentaerythritol by using a high temperature gas phase chromatograph (HT-GC) to analyze the component ratio of the tetraester of fatty acid tetraester (FTPE) of pentaerythritol
(FTPE) of the pentaerythritol fatty acid contained in the polymer resin.
[Chemical Formula 1]
According to the present invention, it is possible to measure the component ratio of fatty acid tetraester (FTPE) of pentaerythritol with high resolution in a short period of time by analyzing without derivatization.
FIG. 1 is a chromatogram showing the results of analysis of component proportions of five components of fatty acid tetraester (FTPE) of pentaerythritol contained in a polymer resin according to Example 1. FIG. Among the peaks, 1 is palmitoic acid methyl ester and 2 is a peak of stearic acid methyl ester.
FIG. 2 is a chromatogram showing the results of analyzing the ratio of palmitic acid and stearic acid in the fatty acid tetraester (FTPE) of pentaerythritol contained in the polymer resin according to Comparative Example 1. FIG. Among the peaks, 1 is PPPP, 2 is PPPS, 3 is PPSS, 4 is PSSS, and 5 is the peak of SSSS.
According to the present invention,
a) extracting a fatty acid tetraester (FTPE) of pentaerythritol represented by the following
b) analyzing the fatty acid tetraester (FTPE) of the extracted pentaerythritol by using a high temperature gas phase chromatograph (HT-GC) to analyze the component ratio of the tetraester of fatty acid tetraester (FTPE) of pentaerythritol
(FTPE) of the pentaerythritol contained in the polymer resin.
[Chemical Formula 1]
The above-mentioned " fatty acid tetraester (FTPE) of pentaerythritol "means fatty acid tetraester with pentaerythritol bonded to pentaerythritol,
In the present specification, PPPP (C [(CH 2 O) COOC 15 H 31 ] 4 ), PPPS ([H 31 C 13 OOC (CH 2 O)] 3 C CH 2 O) COOC 17 H 35 ), PPSS ([H 31 C 13 OOC (CH 2 O)] 2 C [(CH 2 O) COOC 17 H 35] 2), PSSS (H 31 C 13 OOC (CH 2 O) C [(CH 2 O) COOC 17 H 35 ] 3 ) and SSSS (C [(CH 2 O) COOC 17 H 35 ] 4 ).
In one embodiment of the present invention,
The composition ratio of the above-mentioned FTPE is determined by PPPP (C [(CH 2 O) COOC 15 H 31 ] 4 ), PPPS ([H 31 C 13 OOC (CH 2 O)] 3 C (CH 2 O) COOC 17 H 35), PPSS ([H 31 C 13 OOC (CH 2 O)] 2 C [(CH 2 O) COOC 17 H 35] 2), PSSS (H 31 C 13 OOC (CH 2 O) C [(CH 2 O) COOC 17 H 35 ] 3 ) and SSSS (C [(CH 2 O) COOC 17 H 35 ] 4 ).
In another embodiment of the present invention,
The fatty acid tetraester (FTPE) of pentaerythritol may be used as a lubricant in the production of the polymer resin, but is not limited thereto.
Each step will be described in detail below.
First, in order to analyze the component ratio of the fatty acid tetraester (FTPE) of pentaerythritol contained in the polymer resin, a) a step of extracting tetraester of fatty acid (FTPE) of pentaerythritol represented by the following
In one embodiment of the present invention,
The extraction can be carried out using re-precipitation or soxlet extraction, but is not limited thereto.
The re-impregnation method is a method of dissolving a polymer resin in a solvent and then introducing the polymer resin solution into an excessive amount of a poor solvent to remove the solid polymer resin and extracting it. As the solvent, chloroform, dichloromethane, tetrahydrofuran, And xylene. It is preferable to use chloroform, but the present invention is not limited thereto.
Also, as a poor solvent, at least one selected from the group consisting of methanol, ethanol and acetonitrile can be used, and methanol is preferably used, but not limited thereto,
The type of the solvent and the poor solvent that can achieve the object of the present invention are not limited, but the use of chloroform as the solvent and methanol as the poor solvent are most preferable because of the solubility of the fatty acid tetraester (FTPE) of pentaerythritol.
In the case of extraction by the Soxhlet extraction method, at least one selected from the group consisting of chloroform, dichloromethane, tetrahydrofuran and toluene can be used as the solvent, and chloroform is used as the solvent for the extraction of fatty acid tetraester (FTPE) of pentaerythritol But the present invention is not limited thereto, and the range of the solvent is not limited as long as the solvent can achieve the object of the present invention.
Next, b) the fatty acid tetraester (FTPE) of the extracted pentaerythritol is analyzed using a high temperature gas phase chromatograph (HT-GC) to analyze the component ratio of pentaerythritol fatty acid tetraester (FTPE) .
The high temperature gaseous phase chromatograph used in the present invention is characterized in that the fatty acid tetraester (FTPE) of pentaerythritol, which is the analyte of the present invention, has a high molecular weight and a high melting point. Therefore, the pentaerythritol fatty acid It is preferable because vaporization of tetraester (FTPE) can be facilitated.
In one embodiment of the present invention,
In the analysis step, the fatty acid tetraester (FTPE) of pentaerythritol may be injected into the hot gas-phase chromatographic analyzer through a cool-on-column injection method.
The cool-on-column injection is an injection method used for analyzing a sample in which thermal decomposition or thermal denaturation may occur on a heated metal surface of a sample injection part during a high-temperature gas phase chromatographic analysis. The pentaerythritol In the case of fatty acid tetraester (FTPE), there is a possibility that thermal decomposition occurs at high temperature and the sample is damaged. Simultaneously with temperature and pressure programming, analysis time is shortened and good peaks can be obtained. It is preferable to inject a sample containing a fatty acid tetraester (FTPE) of pentaerythritol, which is an analyte of the present invention, into a high-temperature gas-phase chromatographic analyzer.
In the cool-on-column injection, the injector in the separation tube has a short length and has no vaporization chamber, and the needle of the syringe is directly inserted into the separation pipe made of glass. In order to precisely control the temperature of the injection port, air is injected into the injection head without diaphragm, and compressed air is blown to cool the injection port.
In another embodiment of the present invention,
The step of analyzing the ratio of the fatty acid tetraester (FTPE) of pentaerythritol to b) is preferably, but not limited to, using a flame ionization detector (FID) as a detector.
In another embodiment of the present invention,
The polymer resin may be at least one selected from the group consisting of a thermoplastic resin and an engineering plastic. More specifically, the polymer resin may be at least one selected from the group consisting of polycarbonate (PC), acrylonitrile butadiene styrene (ABS), polycarbonate / acrylonitrile butadiene styrene / ABS), polybutylene terephthalate (PBT), and polycarbonate / polybutylene terephthalate (PC / PBT).
Hereinafter, the present invention will be described in more detail by way of non-limiting examples. The embodiments of the present invention described below are by way of example only and the scope of the present invention is not limited to these embodiments. The scope of the present invention is indicated in the claims, and moreover, includes all changes within the meaning and range of equivalency of the claims. In the following Examples and Comparative Examples, "%" and "part" representing the content are on a mass basis unless otherwise specified.
Example
Example 1. Included in the polymer resin Pentaerythritol fatty acid Tetraester (FTPE) Method of composition ratio analysis
a) extracting the fatty acid tetraester (FTPE) of the active agent pentaerythritol from the polymer resin
Fatty acid tetraester (FTPE) of pentaerythritol in the polymer resin was extracted with a Soxhlet extractor for 24 hours, and chloroform was used as a solvent.
b) The fatty acid tetraester (FTPE) of the extracted pentaerythritol was analyzed with a high temperature gas phase chromatograph (column: Phenomenex, Zebron ZB-5HT inferno column, GC / FID: Agilent, 6890) 1).
In the step of analyzing with the high-temperature gas-phase chromatographic analyzer, the analyte can be preferably separated by using a capillary separation tube in the high-temperature gas-phase chromatographic analysis method.
At this time, a separation tube having a length of 15 m, a diameter of 0.53 mm, a stationary phase thickness of 0.15 μm and a stationary phase composition of 5% phenyl and 95% methyl-polysiloxane was used . High purity helium gas was used as the mobile phase gas in the gas phase chromatograph.
c) Peak intensities of PPPP, PPPS, PPSS, PSSS, and SSSS were quantified to calculate composition ratios.
Comparative Example 1. Included in the polymer resin Pentaerythritol fatty acid Tetraester (FTPE) Method of composition ratio analysis
a) Fatty acid tetraester of pentaerythritol (FTPE) in polymer resin was dissolved in toluene, and tetramethylammonium hydroxide was added thereto for reaction. After distilled water was added, the reaction solution was shaken and the supernatant was collected and derivatized with a methyl group.
b) Analysis of fatty acid methyl esters (palmitic acid methyl ester and stearic acid methyl ester) produced by derivatization with a methyl group in step a) with a gas chromatograph analyzer to determine the ratio of palmitic acid methyl ester and stearic acid methyl ester And expressed as a chromatogram (FIG. 2).
As can be seen from the above Example 1 and Comparative Example 1, in the case of the analysis method of Example 1, the composition ratios of the five components PPPP, PPPS, PPSS, PSSS and SSSS contained in the fatty acid tetraester (FTPE) of pentaerythritol were However, in the case of the analysis method of Comparative Example 1, only the ratio of palmitic acid and stearic acid contained in the fatty acid tetraester (FTPE) of pentaerythritol was known, and the exact component ratio was unknown.
Claims (13)
b) analyzing the fatty acid tetraester (FTPE) of the extracted pentaerythritol by using a high temperature gas phase chromatograph (HT-GC) to analyze the component ratio of the tetraester of fatty acid tetraester (FTPE) of pentaerythritol
(FTPE) of the pentaerythritol contained in the polymer resin, comprising the steps of:
[Chemical Formula 1]
The ratio of the fatty acid tetraester (FTPE) of pentaerythritol is PPPP (C [(CH 2 O) COOC 15 H 31 ] 4 ) contained in the fatty acid tetraester (FTPE) of pentaerythritol, PPPS ([H 31 C 13 OOC (CH 2 O)] 3 C (CH 2 O) COOC 17 H 35 ), PPSS ([H 31 C 13 OOC (CH 2 O)] 2 C [(CH 2 O) COOC 17 H 35 ] 2 ) (H 31 C 13 OOC (CH 2 O) C [(CH 2 O) COOC 17 H 35 ] 3 ) and SSSS (C [(CH 2 O) COOC 17 H 35 ] 4 ) , A method of analyzing the component ratio of the tetraester of fatty acid (FTPE) of pentaerythritol contained in the polymer resin.
Wherein the fatty acid tetraester (FTPE) of pentaerythritol is used as a lubricant in the production of the polymer resin, wherein the fatty acid tetraester (FTPE) of pentaerythritol is used as a lubricant in the production of the polymer resin.
Wherein the extraction is carried out using a re-impregnation method or a soxlet extraction method. 2. The method according to claim 1, wherein the pentaerythritol fatty acid tetraester (FTPE) is contained in the polymer resin.
The re-impregnation may be carried out by using at least one selected from the group consisting of chloroform, dichloromethane, tetrahydrofuran, toluene and xylene as the solvent. The fatty acid tetraester (FTPE) of pentaerythritol contained in the polymer resin, Lt; / RTI >
Wherein the re-impregnation method comprises using chloroform as a solvent, wherein the content ratio of fatty acid tetraester (FTPE) of pentaerythritol contained in the polymer resin is analyzed.
Wherein the re-impregnation method comprises using at least one member selected from the group consisting of methanol, ethanol and acetonitrile as a poor solvent, and analyzing the component ratio of pentaerythritol fatty acid tetraester (FTPE) contained in the polymer resin.
Wherein the re-impregnation method uses methanol as a poor solvent, wherein the content ratio of the fatty acid tetraester (FTPE) of pentaerythritol contained in the polymer resin is analyzed.
A method for analyzing the component ratio of fatty acid tetraester (FTPE) of pentaerythritol contained in a polymer resin, wherein the Soxhlet extraction method uses chloroform as a solvent.
Characterized in that the fatty acid tetraester (FTPE) of pentaerythritol is injected into the hot gas-phase chromatographic analyzer through a cool-on-column injection method in the step of analyzing. Method for analyzing component ratio of fatty acid tetraester (FTPE) of pentaerythritol.
Wherein the step of analyzing the component ratio of the fatty acid tetraester (FTPE) of pentaerythritol is carried out by using a flame ionization detector (FID) as a detector, and a step of contacting the fatty acid tetraester (FTPE) of pentaerythritol contained in the polymer resin Method of component ratio analysis.
Wherein the polymer resin is at least one member selected from the group consisting of a thermoplastic resin and an engineering plastic, and the component ratio of the fatty acid tetraester (FTPE) of pentaerythritol contained in the polymer resin.
The polymer resin may be selected from the group consisting of polycarbonate (PC), acrylonitrile butadiene styrene (ABS), polycarbonate / acrylonitrile butadiene styrene (PC / ABS), polybutylene terephthalate (PBT) and polycarbonate / polybutylene terephthalate (PCE / PBT), wherein the content ratio of the fatty acid tetraester (FTPE) of pentaerythritol contained in the polymer resin is at least one selected from the group consisting of PC / PBT.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020150131859A KR101818303B1 (en) | 2015-09-17 | 2015-09-17 | A method for analyzing composition ratio of fatty acid tetraester with pentaerythritol in polymer resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020150131859A KR101818303B1 (en) | 2015-09-17 | 2015-09-17 | A method for analyzing composition ratio of fatty acid tetraester with pentaerythritol in polymer resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| KR20170033721A KR20170033721A (en) | 2017-03-27 |
| KR101818303B1 true KR101818303B1 (en) | 2018-01-12 |
Family
ID=58496898
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| KR1020150131859A KR101818303B1 (en) | 2015-09-17 | 2015-09-17 | A method for analyzing composition ratio of fatty acid tetraester with pentaerythritol in polymer resin |
Country Status (1)
| Country | Link |
|---|---|
| KR (1) | KR101818303B1 (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002148254A (en) | 2000-11-08 | 2002-05-22 | Sumitomo Chem Co Ltd | Polyimide resin analyzing method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102325760B (en) | 2009-02-03 | 2014-11-05 | 图兰恩教育基金管理人 | Tuned synthetic dendrimer calibrants for mass spectrometry |
-
2015
- 2015-09-17 KR KR1020150131859A patent/KR101818303B1/en active IP Right Grant
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002148254A (en) | 2000-11-08 | 2002-05-22 | Sumitomo Chem Co Ltd | Polyimide resin analyzing method |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20170033721A (en) | 2017-03-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Kaal et al. | Extending the molecular application range of gas chromatography | |
| CN103217497B (en) | Method for detecting phenolic antibacterial agents in textiles through in-situ derivatization and dispersive liquid phase microextraction | |
| Tsujikawa et al. | Chemical profiling of seized methamphetamine putatively synthesized from phenylacetic acid derivatives | |
| BR112012012226A2 (en) | PROCESS | |
| KR101818303B1 (en) | A method for analyzing composition ratio of fatty acid tetraester with pentaerythritol in polymer resin | |
| La Nasa et al. | Alkyd paints in art: characterization using integrated mass spectrometry | |
| Sun et al. | Study of chiral ionic liquid as stationary phases for GC | |
| Toske et al. | Isolation and characterization of a newly identified impurity in methamphetamine synthesized via reductive amination of 1‐phenyl‐2‐propanone (P2P) made from phenylacetic acid/lead (II) acetate | |
| CN105974039B (en) | A kind of method for being enriched with and detecting phthalic acid ester in food packaging plastic products | |
| Jansson et al. | Determination of polymer additives using analytical pyrolysis | |
| Schwemer et al. | Characterization of a heroin manufacturing process based on acidic extracts by combining complementary information from two-dimensional gas chromatography and high resolution mass spectrometry | |
| Cousin et al. | Synthesis, NMR spectroscopic characterization and polysiloxane‐based immobilization of the three regioisomeric monooctenylpermethyl‐β‐cyclodextrins and their application in enantioselective GC | |
| Silva et al. | Characterization of additives of PVAc and acrylic waterborne dispersions and paints by analytical pyrolysis–GC–MS and pyrolysis–silylation–GC–MS | |
| Chiavari et al. | Effect of pigments on the analysis of fatty acids in siccative oils by pyrolysis methylation and silylation | |
| CN108535395B (en) | method for simultaneously and rapidly measuring 32 free fatty acids in health-care wine | |
| CN106290663A (en) | A kind of pre-treating method of tobacco aromatics using analysis of volatile components | |
| Barbosa et al. | Synthesis and characterization of acrylic fatty acid derivative and use as reactive coalescing agent | |
| CN102004131A (en) | Method for detecting glyceroltriacetate in cigarette filter rods | |
| Riedo et al. | Pyrolysis–GC/MS for the identification of macromolecular components in historical recipes | |
| CN114456119B (en) | Hydrogenated cardanol-heterocyclic Schiff base compound, preparation method and application thereof, polylactic acid composite material and preparation method | |
| Ohra-aho et al. | Thermochemolysis using TMAAc and TMAH reagents as means to differentiate between free acids and esters | |
| CN108195946A (en) | A kind of method of gas chromatography mass spectrometry method identification rubber precipitate | |
| JP2019196948A (en) | Method for analyzing triglyceride, sorting methods of fats and oils, and method for producing triglyceride | |
| Lankhorst et al. | A simple 13C NMR method for the discrimination of complex mixtures of stereoisomers: all eight stereoisomers of α‐tocopherol resolved | |
| Xu et al. | Phosphite-catalyzed alkoxycarbonylation of aryl diazonium salts |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A201 | Request for examination | ||
| E701 | Decision to grant or registration of patent right | ||
| GRNT | Written decision to grant |