CN104236994A - Extraction method of phthalate compound in toy - Google Patents
Extraction method of phthalate compound in toy Download PDFInfo
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- CN104236994A CN104236994A CN201410503439.6A CN201410503439A CN104236994A CN 104236994 A CN104236994 A CN 104236994A CN 201410503439 A CN201410503439 A CN 201410503439A CN 104236994 A CN104236994 A CN 104236994A
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Abstract
The invention relates to an extraction method of a phthalate compound in a toy, in particular to an extraction method and a detection method of a phthalate compound in a toy taking textiles, polyvinyl chloride, rubber and coatings as raw materials. The method comprises the following steps: by taking ethyl acetate as a solvent, performing microwave extraction at 100-120 DEG C for 6-8 hours. The method is mainly applied to extraction of the phthalate compound in the toy materials such as the textiles, polyvinyl chloride, the rubber or the coatings. The method has the benefits that the extraction solvent is relatively low in toxicity and environmental disruption, convenient in extraction mode, practical and relatively high in phthalate extraction efficiency.
Description
Technical field
The present invention relates to the detection method of objectionable impurities in a kind of toy material, particularly relate to the extracting process of phthalate compound in textile, Polyvinylchloride, rubber and the coating toy that is material.
Background technology
The rubber often used in toy material, plastic products, surface paint, often can use phthalic ester in leather and textile.Such as in plastic toy, many enterprises, in order to cost-saving, use waste material, feed back add phthalate plasticizers and increase pliability and glossiness, so the use face of phthalic ester in toy material widely.Because phthalic ester can badly influence human reproductive systems, immune system and nervous system, and threaten the existence of the mankind, particularly have infringement to the organ such as liver,spleen,kidney of the child being in the growth stage, therefore a lot of countries and regions all limit the content of phthalic ester in toy in the world
Because toy material coverage is wide, existing examination criteria cannot cover the detection of phthalate compound in all material.Plastic products in such as toy material, leather, textile, surface paint, all phthalic ester may be contained in rubber, for textile in GB, and the detection of phthalic ester in PVC material in plastic products has all had detailed detection method, but all also still belongs to blank for the detection of the phthalic ester in other toy materials.
In addition in existing detection method, the reagent of some uses is unfriendly to environment, or the toxicity of reagent own is too large, as " mensuration of GB/T22931-2008 leather and fur chemical experiment plastifier " and " mensuration of GB/T20388-2006 textile phthalic ester ", use methenyl choloride as solvent extraction, but methenyl choloride is larger to environmental disruption." EN14372-2004 children use and nursing materials knife and fork and nursing instrument safety requirements " uses absolute ether extraction solvent, the test routine of phthalic ester " CPSC-CH-C1001-09.1 test " uses tetrahydrofuran as extraction solvent, and absolute ether and these two kinds of reagent relative toxicities of tetrahydrofuran larger.
All do not have in prior art and carry out for the extracting process of phthalate compound in the toy being material with textile, Polyvinylchloride, rubber and coating the report studied specially.，
Summary of the invention
Object of the present invention solves the problems of the prior art exactly, the extracting process of phthalate compound in a kind of toy is proposed, especially with the toy that textile, Polyvinylchloride, rubber and coating are material, the method extraction solvent toxicity is relatively little, less to environmental disruption, extraction mode is convenient, practical, higher again to the extraction efficiency of phthalic ester.
Technical scheme of the present invention is as follows:
An extracting process for phthalate compound in toy, especially with the toy that textile, Polyvinylchloride, rubber and coating are material, adopts ethyl acetate as solvent, uses microwave abstracting.
Preferably, the temperature of microwave abstracting is at 100-120 DEG C, and extraction time is in 6-8 hour.
The present invention also protects above-mentioned extracting process in textile, Polyvinylchloride, rubber or coating toy, extract the application of phthalic acid ester type compound.
The present invention also protects the method adopting above-mentioned extracting process to detect phthalate compound in toy material.
Beneficial effect of the present invention: extraction solvent toxicity is relatively little, less to environmental disruption, extraction mode is convenient, practical, higher again to the extraction efficiency of phthalic ester.
The present invention is directed to and study with the extracting process of phthalate compound in textile, Polyvinylchloride, rubber and the coating toy that is material, innovation is mainly in the selection of extraction solvent, extracting process and extraction process parameter, above-mentioned every be all that applicant draws after great many of experiments, these extraction process and parameter can make the phthalate compound in leather toy material obtain extraction efficiency to reach maximum.Embodiment part lists part demonstration test, and these tests are only representational.Do not represent the present invention to be drawn by following test.
Embodiment
Use the mode of microwave abstracting, contrast normal hexane, isooctane, methenyl choloride, methylene chloride, ethyl acetate, acetonitrile, ether, acetone, ethanol, tetrahydrofuran, normal hexane: acetone (1:1), methylene chloride: these 12 kinds of solvents of methyl alcohol (1:1) are that in the toy of material, phthalate compound extracts respectively to textile, Polyvinylchloride, rubber and coating, and result is as follows:
The content (mg/kg) of DEHP in sample in the different extraction solvent of table 1
Can find out, for the extraction of phthalate compound in the toy being material with textile, Polyvinylchloride, rubber and coating, with ethyl acetate as solvent, extraction efficiency is far above other solvents.
Embodiment 2
Use ethyl acetate as solvent, relatively microwave abstracting, ultrasonic extraction, surname extraction, ASE Accelerate solvent extraction four kinds of extraction modes are the extraction efficiency of phthalate compound in the toy of material to textile, Polyvinylchloride, rubber and coating, visible, for the extraction of phthalate compound in the toy being material with textile, Polyvinylchloride, rubber and coating, use the mode of microwave abstracting, extraction efficiency is far above other modes.
Table 2 uses ethyl acetate for solvent, the content (mg/kg) of DEHP in the sample under different extraction mode
Embodiment 3
Employing ethyl acetate is solvent, and adopt microwave abstracting (800W, 30min) to extract at different temperatures, visible, extraction temperature effect when 100-120 DEG C is best.
Table 3 uses ethyl acetate for solvent, in the mode of microwave abstracting (800W, 30min), and the content (mg/kg) of the DEHP of sample under extraction temperature
Above embodiment display and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and instructions just illustrates principle of the present invention; instead of limit the scope of the invention by any way; without departing from the scope of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in claimed scope.
Claims (4)
1. the extracting process of phthalate compound in toy, especially with the toy that textile, Polyvinylchloride, rubber and coating are material, is characterized in that, adopts ethyl acetate as solvent, uses microwave abstracting.
2. extracting process as claimed in claim 1, it is characterized in that, the temperature of microwave abstracting is at 100-120 DEG C, and extraction time is in 6-8 hour.
3. extracting process according to claim 2 extracts the application of phthalic acid ester type compound in textile, Polyvinylchloride, rubber or coating toy material.
4. the detection method of phthalate compound in toy, especially with the toy that textile, Polyvinylchloride, rubber and coating are material, is characterized in that, adopts extracting process according to claim 2 to detect.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410503439.6A CN104236994A (en) | 2014-09-26 | 2014-09-26 | Extraction method of phthalate compound in toy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410503439.6A CN104236994A (en) | 2014-09-26 | 2014-09-26 | Extraction method of phthalate compound in toy |
Publications (1)
| Publication Number | Publication Date |
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| CN104236994A true CN104236994A (en) | 2014-12-24 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410503439.6A Pending CN104236994A (en) | 2014-09-26 | 2014-09-26 | Extraction method of phthalate compound in toy |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105606689A (en) * | 2016-01-14 | 2016-05-25 | 中国检验检疫科学研究院 | Quick detection method of di(2-ethylhexyl) phthalate in beverages |
| CN107982954A (en) * | 2016-10-26 | 2018-05-04 | 中国石油化工股份有限公司 | A kind of agent of tri compound microwave abstracting and its application |
| CN110068626A (en) * | 2019-05-08 | 2019-07-30 | 东莞市信准检测技术服务有限公司 | The measuring method of phthalic acid ester in toy for children |
| WO2022243043A1 (en) * | 2021-05-20 | 2022-11-24 | IFP Energies Nouvelles | Method for extraction and transformation by transesterification of phthalates contained in pvc plastics materials |
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| CN102095716A (en) * | 2010-12-09 | 2011-06-15 | 江南大学 | Method for detecting DEHP (Di 2-Ethyl Hexyl Phthalate) by using laser Raman spectrum |
| CN102419352A (en) * | 2011-08-30 | 2012-04-18 | 华南农业大学 | Determination method of amount of phthalic acid 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 |
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Patent Citations (3)
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| CN102095716A (en) * | 2010-12-09 | 2011-06-15 | 江南大学 | Method for detecting DEHP (Di 2-Ethyl Hexyl Phthalate) by using laser Raman spectrum |
| CN102419352A (en) * | 2011-08-30 | 2012-04-18 | 华南农业大学 | Determination method of amount of phthalic acid 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 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105606689A (en) * | 2016-01-14 | 2016-05-25 | 中国检验检疫科学研究院 | Quick detection method of di(2-ethylhexyl) phthalate in beverages |
| CN107982954A (en) * | 2016-10-26 | 2018-05-04 | 中国石油化工股份有限公司 | A kind of agent of tri compound microwave abstracting and its application |
| CN110068626A (en) * | 2019-05-08 | 2019-07-30 | 东莞市信准检测技术服务有限公司 | The measuring method of phthalic acid ester in toy for children |
| WO2022243043A1 (en) * | 2021-05-20 | 2022-11-24 | IFP Energies Nouvelles | Method for extraction and transformation by transesterification of phthalates contained in pvc plastics materials |
| FR3123070A1 (en) * | 2021-05-20 | 2022-11-25 | IFP Energies Nouvelles | METHOD FOR THE EXTRACTION AND TRANSFORMATION BY TRANSESTERIFICATION OF PHTHALATES CONTAINED IN PVC PLASTICS |
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Application publication date: 20141224 |