CN107982954A - A kind of agent of tri compound microwave abstracting and its application - Google Patents

A kind of agent of tri compound microwave abstracting and its application Download PDF

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Publication number
CN107982954A
CN107982954A CN201610943542.1A CN201610943542A CN107982954A CN 107982954 A CN107982954 A CN 107982954A CN 201610943542 A CN201610943542 A CN 201610943542A CN 107982954 A CN107982954 A CN 107982954A
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microwave abstracting
extractant
dichloromethane
agent
extraction
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CN201610943542.1A
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Inventor
胡法
孙晋
华晔
武志军
熊志敏
魏若奇
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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Priority to CN201610943542.1A priority Critical patent/CN107982954A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • G01N2030/062Preparation extracting sample from raw material

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention relates to a kind of agent of tri compound microwave abstracting and its application of the field of polymers.The tri compound microwave abstracting agent, is made of dimethylbenzene, dichloromethane and n-hexane, and the volume ratio of the dimethylbenzene, dichloromethane and n-hexane is 100:(40‑60):(10‑20).With strong points, the plasticizer P AEs being exclusively used in extraction PVC of the tri compound microwave abstracting agent, and extraction yield is high;The boiling point of tri compound microwave abstracting agent of the present invention at the same time is relatively low, its requirement to temperature and pressure is relatively low, it is not necessary to which maximum extraction can be achieved in very high microwave abstracting temperature and pressure, reduces quick-fried tank equivalent risk.

Description

A kind of agent of tri compound microwave abstracting and its application
Technical field
The invention belongs to the field of polymers, and in particular to a kind of agent of tri compound microwave abstracting and its application.
Background technology
Polyvinyl chloride (Polyvinyl chloride, abbreviation PVC) is polymerized by vinyl chloride under initiator effect Thermoplastic resin, is one of five big general-purpose plastics.
Plasticizer is added in high molecular material the plasticity that can improve material, strengthens the flexibility of high molecular material, in day Using extremely extensive, such as packaging bag, mat applying, wallpaper, toy in regular supplies.When some liquid in body or production and living When being contacted with the high molecular material containing plasticizer, micro plasticizer can be extracted from high molecular material, if plasticizer contains Measure excessive, Long Term Contact can then cause body necessarily to injure.
Phthalic acid ester (PAEs), also known as phthalate ester, are the general designations that phthalic acid forms ester.Have in plastics industry It is widely used, is often added in plastics and is used as plasticizer.When being used as plastic plasticizer, generally referred to as adjacent benzene The ester that dioctyl phthalate is formed with the alcohol containing 4-15 carbon.Since PAEs and polymer body only pass through hydrogen bond or Van der Waals force knot Close, therefore can constantly discharge and be transferred in surrounding environment in use, become be widely present in air, water body, Organic pollution in soil, so as to be prevalent in the environment of human lives.PAEs is typical environmental estrogens pollution Thing, by plant absorption enter plant in, it may occur that biological concentration, Long Term Contact can influence human endocrine, cause deformity, Canceration and mutagenesis, thus extensive concern both domestic and external was caused in recent years.
The phthalic acid ester that polyvinyl chloride raw material and product manufacturing most generally use at present has:Phthalic acid two Methyl esters (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP), diisobutyl phthalate (DIBP), phthalic acid two (2- methoxyl groups) ethyl ester (DMEP), phthalic acid two (4- methyl -2- amyl groups) ester (BMPP), Phthalic acid two (2- ethyoxyls) ethyl ester (DEEP), diamyl phthalate (DPP), dihexyl phthalate (DHXP), Butyl benzyl phthalate (BBP), phthalic acid two (2- butoxy) ethyl ester (DBEP), dicyclohexyl phthalate (DCHP), the own ester (DEHP) of phthalic acid two (2- ethyls), diphenyl phthalate (DPhP), phthalic acid two are just pungent Ester (DNOP), dinonyl phthalate (DNP) etc..
The method of plasticizer mainly has soxhlet extraction, ultrasonic extraction and microwave abstracting etc. in extraction PVC at present, wherein micro- Ripple extraction has the advantages that speed is fast, saves solvent, pollution is small, and application is more and more.But different types of sample carry out it is micro- When ripple extracts, the factor such as species and polarity of extractant can influence extraction yield and instrument safety.Single solvent is used as extraction PVC It is difficult to meet the conditions such as solubility, polarity, instrument applicability and high-recovery at the same time during middle plasticizer.
Therefore, a kind of new, with strong points microwave abstracting agent of necessary invention, to reach quick, accurately extract PVC The purpose of middle plasticizer.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of tri compound microwave abstracting in view of the deficiencies of the prior art Agent, the extractant it is with strong points, be exclusively used in plasticizer P AEs in extraction PVC, and the extractant wants temperature, pressure Ask relatively low, it is not necessary to which maximum extraction can be achieved in very high microwave abstracting temperature and pressure, and extraction yield is high and reduces quick-fried tank etc. Risk.
Present invention also offers a kind of side that phthalic acid ester in pvc material is extracted using the extract Method, this method is easy to operate, of low cost.
The qualitative, quantitative that the extract and extracting process are applied to follow-up gas chromatography-mass spectrography measures, can be with The species and content of the phthalate compound contained by pvc material are accurately determined, it is easy to operate, quick.
For this reason, one aspect of the present invention provides a kind of tri compound microwave abstracting agent, it is by dimethylbenzene, dichloromethane and just Hexane forms.
In some embodiments of the invention, the volume ratio of the dimethylbenzene, dichloromethane and n-hexane is 100:(40- 60):(10-20)。
In other embodiments of the present invention, the volume ratio of the dimethylbenzene, dichloromethane and n-hexane is 100: (50-60):(10-20)。
Another aspect of the present invention provides a kind of using phthalic acid in the extractant extraction pvc material The method of ester.
In some embodiments of the invention, the temperature of the extraction is 60-120 DEG C.
In other embodiments of the present invention, the mass volume ratio of the pvc material and extractant is 1:(30- 70)。
Third aspect present invention provides a kind of method for measuring phthalic acid ester content in pvc material, it is wrapped Include:
(1) using the extractant or using the phthalic acid in the extraction process pvc material Ester;With
(2) using the content of the phthalic acid ester in gas phase-Mass Spectrometry measure pvc material.
Beneficial effects of the present invention are:
(1) extractant of the present invention is with strong points, the plasticizer P AEs being exclusively used in extraction PVC, and extraction yield is high.
(2) since the boiling point of extractant of the present invention is relatively low, thus its requirement to temperature and pressure is relatively low, no Need very high microwave abstracting temperature and pressure that maximum extraction can be achieved, reduce quick-fried tank equivalent risk.
Embodiment
To be readily appreciated that the present invention, the present invention is described more detail below.
As it was previously stated, the extractant that plasticizer P AEs is taken in extraction PVC at present is mainly single formula, and it is single molten When agent is used as plasticizer in extraction PVC, it is difficult to while meet the conditions such as solubility, polarity, instrument applicability and high-recovery.
The present inventor is had found by studying, and the solvent (dimethylbenzene, dichloromethane and n-hexane) of three kinds of opposed polarities is pressed According to the extractant obtained after certain ratio mixing, under the synergistic effect of three components so that the compound extract is for polychlorostyrene The extraction of phthalic acid ester in ethene has good effect.Compared with single solvent extract in the prior art, this hair The specific aim of bright compound extract is stronger, and actual use temperature is lower than single solvent, improves the safety in utilization of instrument. The present invention is based on what the above method was made.
For this reason, one aspect of the present invention provides a kind of tri compound microwave abstracting agent, it is by dimethylbenzene, dichloromethane and just Hexane forms.
In some embodiments of the invention, the volume ratio of the dimethylbenzene, dichloromethane and n-hexane is 100:(40- 60):(10-20)。
In other embodiments of the present invention, the volume ratio of the dimethylbenzene, dichloromethane and n-hexane is 100: (50-60):(10-20)。
Another aspect of the present invention provides a kind of using phthalic acid in the extractant extraction pvc material The method of ester.
In some embodiments of the invention, the temperature of the extraction is 60-120 DEG C.
In other embodiments of the present invention, the mass volume ratio of the pvc material and extractant is 1:(30- 70), for example, in some embodiments, the mass volume ratio of the pvc material and extractant is 1:50.
Third aspect present invention provides a kind of method for measuring phthalic acid ester content in pvc material, it is wrapped Include:
(1) using the extractant or using the phthalic acid in the extraction process pvc material Ester;
(2) standard curve of each phthalate compound is drawn using gas phase-Mass Spectrometry;
(3) gas phase-Mass Spectrometry is used, according to the O-phthalic in the standard curve determination pvc material of drafting The content of acid esters.
Term " mass volume ratio of pvc material and extractant " of the present invention is the " quality of pvc material The ratio between with the volume of extractant ".
Embodiment
To make the present invention easier to understand, the present invention is further described below in conjunction with embodiment, these realities Apply example only serve it is illustrative, it is not limited to application range of the invention.If raw material or component nothing used in the present invention Specified otherwise can be made by commercial sources or conventional method.
Embodiment 1
(1) extractant is prepared:100mL dimethylbenzene, 50mL dichloromethane, 15mL n-hexanes is pipetted respectively with pipette to be placed in In 250mL conical flask with cover, uniformly mixed, i.e., required tri compound microwave abstracting agent is rocked;
(2) microwave abstracting:By containing plasticizer sample (sample 1 and sample 2) rub, weigh 0.2000g (± 0.0010g) sample, is placed in microwave abstracting pressurized tank, then adds the prepared extractants of 10mL, screws protective case, put Enter and microwave abstracting is carried out in microwave extracting apparatus, the temperature-time program of microwave abstracting is shown in Table 1, is extracted after extraction Liquid;
(3) nitrogen blows constant volume:Extract is transferred in nitrogen evaporator test tube, after nitrogen is blown to 0.1mL, adds a small amount of dichloromethane Alkane, after ultrasonic vibration, moves in 10mL volumetric flasks, is sample prepare liquid using dichloromethane constant volume;
(4) drafting of standard curve:The standard solution of the plasticizer P AEs of various concentrations is prepared using extractant as solvent, is used Gas phase-Mass Spectrometry, draws out the standard curve of each phthalate compound;
(5) gas phase-mass spectrometry:Using gas phase-Mass Spectrometry, according in the standard curve determination sample of drafting Phthalic acid ester content, gas-chromatography heating schedule is shown in Table 2;The content of plasticizer P AEs is shown in the PVC being calculated Table 3.
Embodiment 2
(1) extractant is prepared:100mL dimethylbenzene, 55mL dichloromethane, 10mL n-hexanes is pipetted respectively with pipette to be placed in In 250mL conical flask with cover, uniformly mixed, i.e., required tri compound microwave abstracting agent is rocked;
(2) microwave abstracting:By containing plasticizer sample (sample 1 and sample 2) rub, weigh 0.2000g (± 0.0010g) sample, is placed in microwave abstracting pressurized tank, then adds the prepared extractants of 10mL, screws protective case, put Enter and microwave abstracting is carried out in microwave extracting apparatus, the temperature-time program of microwave abstracting is shown in Table 1, is extracted after extraction Liquid;
(3) nitrogen blows constant volume:Extract is transferred in nitrogen evaporator test tube, after nitrogen is blown to 0.1mL, adds a small amount of dichloromethane Alkane, after ultrasonic vibration, moves in 10mL volumetric flasks, is sample prepare liquid using dichloromethane constant volume;
(4) drafting of standard curve:The standard solution of the plasticizer P AEs of various concentrations is prepared using extractant as solvent, is used Gas phase-Mass Spectrometry, draws out the standard curve of each phthalate compound;
(5) gas phase-mass spectrometry:Using gas phase-Mass Spectrometry, according in the standard curve determination sample of drafting Phthalic acid ester content, gas-chromatography heating schedule is shown in Table 2;The content of plasticizer P AEs is shown in the PVC being calculated Table 3.
Embodiment 3
(1) extractant is prepared:100mL dimethylbenzene, 60mL dichloromethane, 20mL n-hexanes is pipetted respectively with pipette to be placed in In 250mL conical flask with cover, uniformly mixed, i.e., required tri compound microwave abstracting agent is rocked;
(2) microwave abstracting:By containing plasticizer sample (sample 1 and sample 2) rub, weigh 0.2000g (± 0.0010g) sample, is placed in microwave abstracting pressurized tank, then adds the prepared extractants of 10mL, screws protective case, put Enter and microwave abstracting is carried out in microwave extracting apparatus, the temperature-time program of microwave abstracting is shown in Table 1, is extracted after extraction Liquid;
(3) nitrogen blows constant volume:Extract is transferred in nitrogen evaporator test tube, after nitrogen is blown to 0.1mL, adds a small amount of dichloromethane Alkane, after ultrasonic vibration, moves in 10mL volumetric flasks, is sample prepare liquid using dichloromethane constant volume;
(4) drafting of standard curve:The standard solution of the plasticizer P AEs of various concentrations is prepared using extractant as solvent, is used Gas phase-Mass Spectrometry, draws out the standard curve of each phthalate compound;
(5) gas phase-mass spectrometry:Using gas phase-Mass Spectrometry, according in the standard curve determination sample of drafting Phthalic acid ester content, gas-chromatography heating schedule is shown in Table 2;The content of plasticizer P AEs is shown in the PVC being calculated Table 3.
Embodiment 4
(1) extractant is prepared:100mL dimethylbenzene, 40mL dichloromethane, 10mL n-hexanes is pipetted respectively with pipette to be placed in In 250mL conical flask with cover, uniformly mixed, i.e., required tri compound microwave abstracting agent is rocked;
(2) microwave abstracting:By containing plasticizer sample (sample 1 and sample 2) rub, weigh 0.2000g (± 0.0010g) sample, is placed in microwave abstracting pressurized tank, then adds the prepared extractants of 10mL, screws protective case, put Enter and microwave abstracting is carried out in microwave extracting apparatus, the temperature-time program of microwave abstracting is shown in Table 1, is extracted after extraction Liquid;
(3) nitrogen blows constant volume:Extract is transferred in nitrogen evaporator test tube, after nitrogen is blown to 0.1mL, adds a small amount of dichloromethane Alkane, after ultrasonic vibration, moves in 10mL volumetric flasks, is sample prepare liquid using dichloromethane constant volume;
(4) drafting of standard curve:The standard solution of the plasticizer P AEs of various concentrations is prepared using extractant as solvent, is used Gas phase-Mass Spectrometry, draws out the standard curve of each phthalate compound;
(5) gas phase-mass spectrometry:Using gas phase-Mass Spectrometry, according in the standard curve determination sample of drafting Phthalic acid ester content, gas-chromatography heating schedule is shown in Table 2;The content of plasticizer P AEs is shown in the PVC being calculated Table 3.
Comparative example 1
(1) microwave abstracting:By containing plasticizer sample (sample 1 and sample 2) rub, weigh 0.2000g (± 0.0010g) sample, is placed in microwave abstracting pressurized tank, then adds 10mL dichloromethane extractants, screws protective case, put Enter and microwave abstracting is carried out in microwave extracting apparatus, the temperature-time program of microwave abstracting is shown in Table 1, is extracted after extraction Liquid;
(2) nitrogen blows constant volume:Extract is transferred in nitrogen evaporator test tube, after nitrogen is blown to 0.1mL, adds a small amount of dichloromethane Alkane, after ultrasonic vibration, moves in 10mL volumetric flasks, is sample prepare liquid using dichloromethane constant volume;
(3) drafting of standard curve:The standard solution of the plasticizer P AEs of various concentrations is prepared using extractant as solvent, is used Gas phase-Mass Spectrometry, draws out the standard curve of each phthalate compound;
(4) gas phase-mass spectrometry:Using gas phase-Mass Spectrometry, according in the standard curve determination sample of drafting Phthalic acid ester content, gas-chromatography heating schedule is shown in Table 2;The content of plasticizer P AEs is shown in the PVC being calculated Table 3.
Comparative example 2
(1) microwave abstracting:By containing plasticizer sample (sample 1 and sample 2) rub, weigh 0.2000g (± 0.0010g) sample, is placed in microwave abstracting pressurized tank, then adds 10mL acetate extractants, screws protective case, put Enter and microwave abstracting is carried out in microwave extracting apparatus, the temperature-time program of microwave abstracting is shown in Table 1, is extracted after extraction Liquid;
(2) nitrogen blows constant volume:Extract is transferred in nitrogen evaporator test tube, after nitrogen is blown to 0.1mL, adds a small amount of dichloromethane Alkane, after ultrasonic vibration, moves in 10mL volumetric flasks, is sample prepare liquid using dichloromethane constant volume;
(3) drafting of standard curve:The standard solution of the plasticizer P AEs of various concentrations is prepared using extractant as solvent, is used Gas phase-Mass Spectrometry, draws out the standard curve of each phthalate compound;
(4) gas phase-mass spectrometry:Using gas phase-Mass Spectrometry, according in the standard curve determination sample of drafting Phthalic acid ester content, gas-chromatography heating schedule is shown in Table 2;The content of plasticizer P AEs is shown in the PVC being calculated Table 3.
The temperature-time program table of microwave abstracting in table 1 embodiment 1-4 and comparative example 1-2
Gas-chromatography heating schedule table in table 2 embodiment 1-4 and comparative example 1-2
The extraction quantity of plasticizer P AEs in the PVC measured in table 3 embodiment 1-4 and comparative example 1-2
As can be known from the results of Table 3, under identical extraction conditions, tri compound microwave abstracting agent pair of the present invention The effect of extracting of plasticizer P AEs in PVC, is above single extractant, illustrates tri compound microwave abstracting agent of the present invention With good effect of extracting and with higher specificity.
Embodiment 5:Stability of the antioxidant 1010 in tri compound microwave abstracting agent
(1) extractant is prepared:100mL dimethylbenzene, 50mL dichloromethane, 15mL n-hexanes is pipetted respectively with pipette to be placed in In 250mL conical flask with cover, uniformly mixed, i.e., required tri compound microwave abstracting agent is rocked;
(2) a certain amount of antioxidant 1010 is dissolved in prepared extractant, respectively 0h, 8h, 24h, 72h, The content of antioxidant 1010 in extractant is measured by sampling in 216h, 648h, and measurement result is shown in Table 4.
4 antioxidant 1010 of table content in tri compound microwave abstracting agent
As known from Table 4, antioxidant 1010 is smaller in the changes of contents of tri compound microwave abstracting agent after 27 days, illustrates antioxygen Agent 1010 has good stability in the tri compound microwave abstracting agent of the present invention.
It should be noted that embodiment described above is only used for explaining the present invention, do not form to any of the present invention Limitation.By referring to exemplary embodiments, invention has been described, it should be appreciated that word wherein used is descriptive With explanatory vocabulary, rather than limited vocabulary.The present invention can be made within the scope of the claims by regulation Modification, and the present invention is revised in without departing substantially from scope and spirit of the present invention.Although the present invention described in it relates to And specific method, material and embodiment, it is not intended that the present invention is limited to wherein disclosed particular case, on the contrary, this hair It is bright to can be extended to other all methods and applications with identical function.

Claims (7)

1. a kind of tri compound microwave abstracting agent, it is made of dimethylbenzene, dichloromethane and n-hexane.
2. extractant according to claim 1, it is characterised in that the volume of the dimethylbenzene, dichloromethane and n-hexane Than for 100:(40-60):(10-20).
3. extractant according to claim 2, it is characterised in that the volume of the dimethylbenzene, dichloromethane and n-hexane Than for 100:(50-60):(10-20).
A kind of 4. side that phthalic acid ester in pvc material is extracted using claim 1-3 any one of them extractant Method.
5. according to the method described in claim 4, it is characterized in that, the temperature of the extraction is 60-120 DEG C.
6. according to claim 4-5 any one of them methods, it is characterised in that the matter of the pvc material and extractant It is 1 to measure volume ratio:(30-70).
7. a kind of method for measuring phthalic acid ester content in pvc material, it includes:
(1) extractant any one of claim 1-3 or the method any one of using claim 4-6 are used Extract the phthalic acid ester in pvc material;With
(2) using the content of the phthalic acid ester in gas phase-Mass Spectrometry measure pvc material.
CN201610943542.1A 2016-10-26 2016-10-26 A kind of agent of tri compound microwave abstracting and its application Pending CN107982954A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112300087A (en) * 2019-07-26 2021-02-02 中国石油化工股份有限公司 Ternary extractant of benzotriazole light stabilizer in polyolefin material and application thereof

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5655437A (en) * 1979-10-15 1981-05-16 Shimada Kankyo Kagaku Kenkyusho:Kk Reclamation of waste polyvinyl chloride film for agriculture, forestry or fishery use
CN101363782A (en) * 2008-09-17 2009-02-11 重庆市计量质量检测研究院 Extractive agent for detecting plasticiser in PVC products
CN101498701A (en) * 2009-03-09 2009-08-05 南京大学 Detection method for phthalate ester residue
TW201400799A (en) * 2012-06-26 2014-01-01 Univ Kaohsiung Medical Method for analyzing phthalate esters and agent for analyzing phthalate esters
CN103787884A (en) * 2012-10-29 2014-05-14 中国石油化工股份有限公司 Ternary extractant and its application, and method for extracting antioxidant 1010 from polyolefin material
CN103792307A (en) * 2012-10-26 2014-05-14 中国石油化工股份有限公司 Extraction liquid for testing of phthalic acid ester content in polyvinyl chloride (PVC) product and its applications
CN104236994A (en) * 2014-09-26 2014-12-24 中华人民共和国台州出入境检验检疫局 Extraction method of phthalate compound in toy
CN104548653A (en) * 2013-10-22 2015-04-29 中国石油化工股份有限公司 Quaternary extractant, application thereof, and method for extracting antioxidant from polyolefin

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5655437A (en) * 1979-10-15 1981-05-16 Shimada Kankyo Kagaku Kenkyusho:Kk Reclamation of waste polyvinyl chloride film for agriculture, forestry or fishery use
CN101363782A (en) * 2008-09-17 2009-02-11 重庆市计量质量检测研究院 Extractive agent for detecting plasticiser in PVC products
CN101498701A (en) * 2009-03-09 2009-08-05 南京大学 Detection method for phthalate ester residue
TW201400799A (en) * 2012-06-26 2014-01-01 Univ Kaohsiung Medical Method for analyzing phthalate esters and agent for analyzing phthalate esters
CN103792307A (en) * 2012-10-26 2014-05-14 中国石油化工股份有限公司 Extraction liquid for testing of phthalic acid ester content in polyvinyl chloride (PVC) product and its applications
CN103787884A (en) * 2012-10-29 2014-05-14 中国石油化工股份有限公司 Ternary extractant and its application, and method for extracting antioxidant 1010 from polyolefin material
CN104548653A (en) * 2013-10-22 2015-04-29 中国石油化工股份有限公司 Quaternary extractant, application thereof, and method for extracting antioxidant from polyolefin
CN104236994A (en) * 2014-09-26 2014-12-24 中华人民共和国台州出入境检验检疫局 Extraction method of phthalate compound in toy

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
刘萌 等: "HF-LPME-GC 测定PVC 输液管路中6 种邻苯二甲酸酯的迁移", 《药物分析杂志》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112300087A (en) * 2019-07-26 2021-02-02 中国石油化工股份有限公司 Ternary extractant of benzotriazole light stabilizer in polyolefin material and application thereof

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