WO2012019341A1 - Method for extracting hexavalent chromium from plastic - Google Patents

Method for extracting hexavalent chromium from plastic Download PDF

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Publication number
WO2012019341A1
WO2012019341A1 PCT/CN2010/075879 CN2010075879W WO2012019341A1 WO 2012019341 A1 WO2012019341 A1 WO 2012019341A1 CN 2010075879 W CN2010075879 W CN 2010075879W WO 2012019341 A1 WO2012019341 A1 WO 2012019341A1
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WIPO (PCT)
Prior art keywords
plastic
hexavalent chromium
extract
mixture
alkaline solution
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PCT/CN2010/075879
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French (fr)
Chinese (zh)
Inventor
刘霁欣
肖融
秦德元
那星
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北京吉天仪器有限公司
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Priority to PCT/CN2010/075879 priority Critical patent/WO2012019341A1/en
Publication of WO2012019341A1 publication Critical patent/WO2012019341A1/en

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/02—Separating plastics from other materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/06—Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts
    • B29K2105/065—Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts containing impurities
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4055—Concentrating samples by solubility techniques
    • G01N2001/4061—Solvent extraction
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/62—Plastics recycling; Rubber recycling

Definitions

  • the invention relates to a method for extracting hexavalent chromium from plastics. Background technique
  • Chromium (Cr) is a metal element frequently encountered in daily life and is widely used in industrial fields such as electroplating, metallurgy, and dyes. Cr has two valence states, hexavalent and trivalent, which are represented by hexavalent chromium (Cr(VI)) and trivalent chromium (Cr(III)), among which Cr(VI) is a strong carcinogen and Cr(III) It is good for the human body, so to understand the hazard of Cr in plastics, it is meaningless to detect the total amount of Cr, and it is necessary to detect Cr(VI).
  • the method for extracting hexavalent chromium from the plastic of the invention comprises the following steps:
  • the mixture is continuously mixed at a temperature of 80 to 160 ° C for a certain period of time;
  • the inorganic phase is continuously recovered, and the inorganic phase is centrifugally layered to obtain an inorganic layer clear liquid containing hexavalent chromium;
  • the extract is a mixture of an organic solvent and an alkaline solution.
  • the organic solvent is any one or more of a benzene series, an ester and an aliphatic hydrocarbon
  • the solute of the alkaline solution is any one or any of lithium hydroxide, sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate.
  • a method for extracting hexavalent chromium from the plastic of the present invention wherein: each gram of the plastic and 0.01 1 L of the extract are mixed.
  • a method for extracting hexavalent chromium from a plastic of the present invention wherein: the volume ratio of the organic solvent to the alkaline solution is (1-10): (1-30).
  • a method for extracting hexavalent chromium from a plastic of the present invention wherein: the concentration of the solute in the alkaline solution is from 0.01 mol/L to 1 mol/L.
  • a method for extracting hexavalent chromium from a plastic of the present invention wherein: the plurality of times is at least 10 minutes.
  • the method for extracting hexavalent chromium from the plastic of the present invention, wherein: the method of continuously mixing is any one or any of stirring, microwave, ultrasonic, and mixing.
  • a method for extracting hexavalent chromium from a plastic of the present invention wherein: the organic solvent is benzene, decane, ethyl acetate, toluene or xylene.
  • the organic solvent is benzene, decane, ethyl acetate, toluene or xylene.
  • the total Cr addition recovery rate is between 90% and 110%; the Cr (VI) spike recovery rate is 90% ⁇ 110%.
  • the mixture of 0.1 g of polypropylene (PP) and 0.1 L of the extract was placed in a closed vessel with a heating and mixing device, sealed and heated, the temperature was maintained at 130 ° C, and stirred for 60 minutes to make the extract. And the mixture is prepared by mixing the mixture of decane and sodium hydroxide in a volume ratio of 1:30, wherein the concentration of the sodium hydroxide solution is O. Olmol/L; The inorganic phase is recovered, the inorganic phase is further centrifuged, and the inorganic layer is taken to determine the total Cr and Cr (VI) in the solution.
  • PP polypropylene
  • 0.1 L of the extract was placed in a closed vessel with a heating and mixing device, sealed and heated, the temperature was maintained at 130 ° C, and stirred for 60 minutes to make the extract.
  • the mixture is prepared by mixing the mixture of decane and sodium hydroxide in a volume ratio of 1:30, wherein the concentration of the sodium hydroxide solution is O. Olmol/L;
  • the total Cr addition recovery rate is between 90% and 110%; the Cr (VI) spike recovery rate is 90% ⁇ 110%.
  • the lg acrylonitrile-butadiene-styrene copolymer (ABS) and the 0.013L extract were mixed and placed in a closed container with a heating and coke ultrasonic extraction device, sealed and heated, and the temperature was maintained at 140°. C, stirring for 100 minutes, the extract and the acrylonitrile-butadiene-styrene copolymer (ABS) are thoroughly mixed and contacted, and the extract is prepared by mixing ethyl acetate and potassium hydroxide solution in a volume ratio of 10:1.
  • the concentration of the potassium hydroxide solution is 1 mol/L; after the end of the extraction, the inorganic phase is allowed to stand still, the inorganic phase is further centrifuged, and the inorganic layer is taken to determine the total Cr and Cr (VI) in the solution.
  • the total Cr addition recovery rate is between 90% and 110%; the Cr (VI) spike recovery rate is 90% ⁇ 110%.
  • ABS acrylonitrile-butadiene-styrene
  • the mixture of benzene and sodium carbonate solution is prepared according to a volume ratio of 1:5, wherein the concentration of the sodium carbonate solution is 0.5 mol/L; after the end of the extraction, the inorganic phase is continuously recovered, and the inorganic phase is further centrifuged to obtain an inorganic layer. The supernatant measures the total Cr and Cr (VI) in the solution.
  • the total Cr addition recovery rate is between 90% and 110%; the Cr (VI) spike recovery rate is 90% ⁇ 110%.
  • the total Cr addition recovery rate is between 90% and 110%; the Cr (VI) spike recovery rate is 90% ⁇ 110%.
  • the extract is prepared by mixing benzene with an alkaline solution in a volume ratio of 3:12, wherein the solute of the alkaline solution is a mixture of lithium hydroxide and sodium hydroxide, lithium hydroxide The concentration of the mixture is 0.08 mol / L, the concentration of sodium hydroxide is 0. 075mol / L ; after the end of the extraction, the inorganic phase is recovered, the inorganic phase is further centrifuged, and the inorganic layer is taken to determine the total Cr in the solution. Cr (VI).
  • the total Cr addition recovery rate is between 90% and 110%; the Cr (VI) spike recovery rate is 90% ⁇ 110%.
  • the extract is prepared by mixing xylene with an alkaline solution in a volume ratio of 1:5, wherein the solute of the alkaline solution is a mixture of potassium hydroxide and sodium carbonate, potassium hydroxide
  • concentration of the sodium carbonate is 0. 5 mol / L
  • concentration of sodium carbonate is 0. 2 mol / L
  • the inorganic phase is recovered, the inorganic phase is further centrifuged, and the inorganic layer is taken to determine the total Cr and Cr in the solution.
  • the total Cr addition recovery rate is between 90% and 110%; the Cr (VI) spike recovery rate is 90% ⁇ 110%.
  • the method for extracting hexavalent chromium from the plastic of the present invention has high recovery rate of total Cr and hexavalent chromium extracted from plastic, and can accurately detect Cr(VI) in plastic products.

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  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

Disclosed is a method for extracting hexavalent chromium from plastic, which comprises the following steps: mixing plastic and extracting solution to obtain a mixture, continuously blending at a temperature of 80~ 160°C in a sealed environment, recovering inorganic phase after static stratification, and obtaining clear solution of inorganic layer containing hexavalent chromium after centrifugal stratifying the inorganic phase. Said extracting solution is the mixture of organic solvent and alkaline solution. The method is of help to accurately inspect hexavalent chromium in plastic.

Description

从塑料中提取六价铬的方法 技术领域  Method for extracting hexavalent chromium from plastics
本发明涉及一种塑料中六价铬的提取方法。 背景技术  The invention relates to a method for extracting hexavalent chromium from plastics. Background technique
铬 （Cr) 是日常生活中经常接触到的金属元素， 在电镀、 冶金、 染料等工业领域得到 广泛的应用。 Cr存在六价和三价两种价态， 分别表示为六价铬 (Cr(VI))和三价铬 (Cr(III))， 其中 Cr(VI)是强致癌物， 而 Cr(III)则对人体有益， 所以要了解塑料中 Cr的危害， 检测 Cr 的总量毫无意义， 而必须检测其中的 Cr(VI)。 目前， 虽然在欧盟的 《电气、 电子设备中限 用有害物质指令》 （RoHS)中规定检测 Cr(VI)， 而且在执行过程中相关工作组也在标准中给 出了碱液提取的方法， 但由于塑料结构致密， 碱液难于进入其内部， 所以该方法并不能有 效提取塑料中的 Cr(VI)， 致使塑料制品中 Cr(VI)处在一个无从检测、 监管的尴尬境地。 发明公开  Chromium (Cr) is a metal element frequently encountered in daily life and is widely used in industrial fields such as electroplating, metallurgy, and dyes. Cr has two valence states, hexavalent and trivalent, which are represented by hexavalent chromium (Cr(VI)) and trivalent chromium (Cr(III)), among which Cr(VI) is a strong carcinogen and Cr(III) It is good for the human body, so to understand the hazard of Cr in plastics, it is meaningless to detect the total amount of Cr, and it is necessary to detect Cr(VI). At present, although the detection of Cr(VI) is specified in the European Union's Directive on the Restriction of Hazardous Substances in Electrical and Electronic Equipment (RoHS), and the relevant working group also gives the method of lye extraction in the standard during the implementation process. However, due to the dense structure of the plastic, it is difficult for the lye to enter the interior. Therefore, the method cannot effectively extract Cr(VI) in the plastic, and the Cr(VI) in the plastic product is in an embarrassing situation without detection and supervision. Invention disclosure
本发明的目的是提供一种回收率高的塑料中六价铬的提取方法。  It is an object of the present invention to provide a method for extracting hexavalent chromium from plastics having a high recovery rate.
本发明的塑料中六价铬的提取方法， 包括如下步骤：  The method for extracting hexavalent chromium from the plastic of the invention comprises the following steps:
将塑料和提取液混合， 得到混合物；  Mixing the plastic and the extract to obtain a mixture;
密闭环境中， 混合物在温度 80~160°C持续混匀若干时间；  In a closed environment, the mixture is continuously mixed at a temperature of 80 to 160 ° C for a certain period of time;
静置回收无机相， 无机相离心分层， 得到含有六价铬的无机层清液；  The inorganic phase is continuously recovered, and the inorganic phase is centrifugally layered to obtain an inorganic layer clear liquid containing hexavalent chromium;
所述提取液为有机溶剂与碱性溶液的混合物。  The extract is a mixture of an organic solvent and an alkaline solution.
本发明的塑料中六价铬的提取方法， 其中： 所述有机溶剂为苯系物， 酯和脂肪烃中的 任一种或任几种；  The method for extracting hexavalent chromium from the plastic of the present invention, wherein: the organic solvent is any one or more of a benzene series, an ester and an aliphatic hydrocarbon;
本发明的塑料中六价铬的提取方法， 其中： 所述碱性溶液的溶质为氢氧化锂、 氢氧化 钠、 氢氧化钾、 碳酸钠和碳酸钾中的任一种或任几种。  In the method for extracting hexavalent chromium from the plastic of the present invention, the solute of the alkaline solution is any one or any of lithium hydroxide, sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate.
本发明的塑料中六价铬的提取方法， 其中： 每克所述塑料和 0.01 1L所述提取液混 合。 本发明的塑料中六价铬的提取方法， 其中： 所述有机溶剂和所述碱性溶液的体积比为 ( 1-10) ： ( 1-30) 。  A method for extracting hexavalent chromium from the plastic of the present invention, wherein: each gram of the plastic and 0.01 1 L of the extract are mixed. A method for extracting hexavalent chromium from a plastic of the present invention, wherein: the volume ratio of the organic solvent to the alkaline solution is (1-10): (1-30).
本发明的塑料中六价铬的提取方法， 其中： 所述碱性溶液中溶质的浓度为 0.01mol/L~lmol/L。 本发明的塑料中六价铬的提取方法， 其中： 所述若干时间为至少 10min。 本发明的塑料中六价铬的提取方法， 其中： 所述持续混匀的方式为搅拌、 微波、 超 声、 混旋中的任一种或任几种。 A method for extracting hexavalent chromium from a plastic of the present invention, wherein: the concentration of the solute in the alkaline solution is from 0.01 mol/L to 1 mol/L. A method for extracting hexavalent chromium from a plastic of the present invention, wherein: the plurality of times is at least 10 minutes. The method for extracting hexavalent chromium from the plastic of the present invention, wherein: the method of continuously mixing is any one or any of stirring, microwave, ultrasonic, and mixing.
本发明的塑料中六价铬的提取方法， 其中： 所述有机溶剂为苯、 壬烷、 乙酸乙酯、 甲 苯或二甲苯。 实施发明的最佳方式  A method for extracting hexavalent chromium from a plastic of the present invention, wherein: the organic solvent is benzene, decane, ethyl acetate, toluene or xylene. The best way to implement the invention
实施例 1、  Example 1.
将 0. lg 聚碳酸酯 （PC) 和 0. 012L 提取液混合放到带有加热和搅拌装置的密闭容器 中， 密封后进行加热， 温度保持在 140 °C， 搅拌 30分钟， 使提取液和聚碳酸酯 （PC) 的充 分混合接触， 提取液为苯与氢氧化锂溶液按照体积比为 1 : 5 混合制成， 其中氢氧化锂溶 液的浓度为 0. 125mol/L; 提取结束后静置回收无机相， 无机相继续离心分层， 取无机层清 液测定溶液中的总 Cr和 Cr (VI)。  Mix 0. lg polycarbonate (PC) and 0. 012L extract into a closed container with heating and stirring device, heat it after sealing, keep the temperature at 140 °C, stir for 30 minutes, make the extract and摩尔摩尔后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后后即可The inorganic phase is recovered, the inorganic phase is further centrifuged, and the inorganic layer is taken to determine the total Cr and Cr (VI) in the solution.
总 Cr加标回收率在 90%〜 110 %之间； Cr (VI)加标回收率达到 90%〜 110 %。  The total Cr addition recovery rate is between 90% and 110%; the Cr (VI) spike recovery rate is 90%~110%.
实施例 2、  Example 2
将 0. 1 g聚丙烯 （PP) 和 0. 1L提取液混合放到带有加热和混旋装置的密闭容器中， 密封后进行加热， 温度保持在 130°C， 搅拌 60分钟， 使提取液和聚丙烯 （PP) 的充分混合 接触， 提取液为壬烷与氢氧化钠溶液按照体积比为 1 : 30 混合制成， 其中氢氧化钠溶液的 浓度为 O. Olmol/L; 提取结束后静置回收无机相， 无机相继续离心分层， 取无机层清液测 定溶液中的总 Cr和 Cr (VI)。  The mixture of 0.1 g of polypropylene (PP) and 0.1 L of the extract was placed in a closed vessel with a heating and mixing device, sealed and heated, the temperature was maintained at 130 ° C, and stirred for 60 minutes to make the extract. And the mixture is prepared by mixing the mixture of decane and sodium hydroxide in a volume ratio of 1:30, wherein the concentration of the sodium hydroxide solution is O. Olmol/L; The inorganic phase is recovered, the inorganic phase is further centrifuged, and the inorganic layer is taken to determine the total Cr and Cr (VI) in the solution.
总 Cr加标回收率在 90%〜 110 %之间； Cr (VI)加标回收率达到 90%〜 110 %。  The total Cr addition recovery rate is between 90% and 110%; the Cr (VI) spike recovery rate is 90%~110%.
实施例 3、  Example 3
将 0. lg丙烯腈-丁二烯-苯乙烯共聚物 （ABS) 和 0. 013L提取液混合放到带有加热和 焦超声提取装置的密闭容器中， 密封后进行加热， 温度保持在 140°C， 搅拌 100 分钟， 使 提取液和丙烯腈-丁二烯-苯乙烯共聚物 （ABS ) 的充分混合接触， 提取液为乙酸乙酯与氢 氧化钾溶液按照体积比为 10: 1混合制成， 其中氢氧化钾溶液的浓度为 lmol/L; 提取结束 后静置回收无机相， 无机相继续离心分层， 取无机层清液测定溶液中的总 Cr和 Cr (VI)。  The lg acrylonitrile-butadiene-styrene copolymer (ABS) and the 0.013L extract were mixed and placed in a closed container with a heating and coke ultrasonic extraction device, sealed and heated, and the temperature was maintained at 140°. C, stirring for 100 minutes, the extract and the acrylonitrile-butadiene-styrene copolymer (ABS) are thoroughly mixed and contacted, and the extract is prepared by mixing ethyl acetate and potassium hydroxide solution in a volume ratio of 10:1. The concentration of the potassium hydroxide solution is 1 mol/L; after the end of the extraction, the inorganic phase is allowed to stand still, the inorganic phase is further centrifuged, and the inorganic layer is taken to determine the total Cr and Cr (VI) in the solution.
总 Cr加标回收率在 90%〜 110 %之间； Cr (VI)加标回收率达到 90%〜 110 %。  The total Cr addition recovery rate is between 90% and 110%; the Cr (VI) spike recovery rate is 90%~110%.
实施例 4、  Example 4
将 0. lg丙烯腈-丁二烯-苯乙烯共聚物 （ABS) 和 0. 012L提取液混合放到带有加热和 焦超声提取装置的密闭容器中， 密封后进行加热， 温度保持在 160°C， 搅拌 100 分钟， 使 提取液和丙烯腈-丁二烯-苯乙烯共聚物 （ABS ) 的充分混合接触， 提取液为苯与碳酸钠溶 液按照体积比为 1 : 5混合制成， 其中碳酸钠溶液的浓度为 0. 5 mol/L; 提取结束后静置回 收无机相， 无机相继续离心分层， 取无机层清液测定溶液中的总 Cr和 Cr (VI)。 Mixing 0.1 g of acrylonitrile-butadiene-styrene (ABS) and 0.012 L of extract with heat and In a closed container of the ultrasonic ultrasonic extraction device, after sealing, heating is performed, the temperature is maintained at 160 ° C, and the mixture is stirred for 100 minutes, so that the extract and the acrylonitrile-butadiene-styrene copolymer (ABS) are thoroughly mixed and contacted, and the extract is extracted. The mixture of benzene and sodium carbonate solution is prepared according to a volume ratio of 1:5, wherein the concentration of the sodium carbonate solution is 0.5 mol/L; after the end of the extraction, the inorganic phase is continuously recovered, and the inorganic phase is further centrifuged to obtain an inorganic layer. The supernatant measures the total Cr and Cr (VI) in the solution.
总 Cr加标回收率在 90%〜 110 %之间； Cr (VI)加标回收率达到 90%〜 110 %。  The total Cr addition recovery rate is between 90% and 110%; the Cr (VI) spike recovery rate is 90%~110%.
实施例 5、  Example 5
将 0. 15g 聚丙烯 （PP ) 和 0. 02 L 提取液混合放到带有加热和混旋装置的密闭容器 中， 密封后进行加热， 温度保持在 80°C， 搅拌 10 分钟， 使提取液和聚丙烯 （PP) 的充分 混合接触， 提取液为甲苯与碳酸钾溶液按照体积比为 3: 1 混合制成， 其中碳酸钾溶液的 浓度为 0. 015mol/L; 提取结束后静置回收无机相， 无机相继续离心分层， 取无机层清液测 定溶液中的总 Cr和 Cr (VI)。  Mix 0. 15g of polypropylene (PP) and 0.02 L of extract into a closed container with heating and mixing device, seal and heat, keep the temperature at 80 ° C, stir for 10 minutes, make the extract And the mixture is prepared by mixing with a mixture of toluene and potassium carbonate in a volume ratio of 3:1, wherein the concentration of the potassium carbonate solution is 0.015 mol/L; The inorganic phase is further centrifuged and stratified, and the inorganic layer is taken to determine the total Cr and Cr (VI) in the solution.
总 Cr加标回收率在 90%〜 110 %之间； Cr (VI)加标回收率达到 90%〜 110 %。  The total Cr addition recovery rate is between 90% and 110%; the Cr (VI) spike recovery rate is 90%~110%.
实施例 6、  Example 6.
将 0. 12g聚碳酸酯 （PC) 和 0. 015L提取液混合放到带有加热和搅拌装置的密闭容器 中， 密封后进行加热， 温度保持在 135 °C， 搅拌 30分钟， 使提取液和聚碳酸酯 （PC) 的充 分混合接触， 提取液为苯与碱性溶液按照体积比为 3: 12 混合制成， 其中碱性溶液的溶质 为氢氧化锂和氢氧化钠的混合物， 氢氧化锂的浓度为 0. 08 mol/L , 氢氧化钠的浓度为 0. 075mol/L; 提取结束后静置回收无机相， 无机相继续离心分层， 取无机层清液测定溶液 中的总 Cr和 Cr (VI)。 Mix 0. 12g of polycarbonate (PC) and 0.015L of extract into a closed container with heating and stirring device, heat it after sealing, keep the temperature at 135 °C, stir for 30 minutes, make the extract and Fully mixed contact of polycarbonate (PC), the extract is prepared by mixing benzene with an alkaline solution in a volume ratio of 3:12, wherein the solute of the alkaline solution is a mixture of lithium hydroxide and sodium hydroxide, lithium hydroxide The concentration of the mixture is 0.08 mol / L, the concentration of sodium hydroxide is 0. 075mol / L ; after the end of the extraction, the inorganic phase is recovered, the inorganic phase is further centrifuged, and the inorganic layer is taken to determine the total Cr in the solution. Cr (VI).
总 Cr加标回收率在 90%〜 110 %之间； Cr (VI)加标回收率达到 90%〜 110 %。  The total Cr addition recovery rate is between 90% and 110%; the Cr (VI) spike recovery rate is 90%~110%.
实施例 7、  Example 7.
将 0. lg 聚碳酸酯 （PC) 和 0. 001L 提取液混合放到带有加热和搅拌装置的密闭容器 中， 密封后进行加热， 温度保持在 130 °C， 搅拌 50分钟， 使提取液和聚碳酸酯 （PC) 的充 分混合接触， 提取液为二甲苯与碱性溶液按照体积比为 1 : 5 混合制成， 其中碱性溶液的 溶质为氢氧化钾和碳酸钠的混合物， 氢氧化钾的浓度为 0. 5mol/L， 碳酸钠的浓度为 0. 2 mol/L; 提取结束后静置回收无机相， 无机相继续离心分层， 取无机层清液测定溶液中的 总 Cr和 Cr (VI)。  Mix 0. lg polycarbonate (PC) and 0.001L extract into a closed container with heating and stirring device, heat it after sealing, keep the temperature at 130 °C, stir for 50 minutes, make the extract and Intimate mixed contact of polycarbonate (PC), the extract is prepared by mixing xylene with an alkaline solution in a volume ratio of 1:5, wherein the solute of the alkaline solution is a mixture of potassium hydroxide and sodium carbonate, potassium hydroxide The concentration of the sodium carbonate is 0. 5 mol / L, the concentration of sodium carbonate is 0. 2 mol / L; after the end of the extraction, the inorganic phase is recovered, the inorganic phase is further centrifuged, and the inorganic layer is taken to determine the total Cr and Cr in the solution. (VI).
总 Cr加标回收率在 90%〜 110 %之间； Cr (VI)加标回收率达到 90%〜 110 %。 以上的实施例仅仅是对本发明的优选实施方式进行描述， 并非对本发明的范围进行限 定， 在不脱离本发明设计精神的前提下， 本领域普通工程技术人员对本发明的技术方案作 出的各种变形和改进， 均应落入本发明的权利要求书确定的保护范围内。 工业实用性 The total Cr addition recovery rate is between 90% and 110%; the Cr (VI) spike recovery rate is 90%~110%. The above embodiments are merely illustrative of the preferred embodiments of the present invention, and are not intended to limit the scope of the present invention. Various modifications of the technical solutions of the present invention will be made by those skilled in the art without departing from the spirit of the invention. And improvements are intended to fall within the scope of protection defined by the claims of the invention. Industrial applicability
本发明的塑料中六价铬的提取方法， 从塑料中提取的总 Cr和六价铬的回收率高， 能 够准确检测塑料制品中的 Cr(VI)。  The method for extracting hexavalent chromium from the plastic of the present invention has high recovery rate of total Cr and hexavalent chromium extracted from plastic, and can accurately detect Cr(VI) in plastic products.

Claims

权利要求 Rights request
1、 塑料中六价铬的提取方法， 包括如下步骤： 1. A method for extracting hexavalent chromium from plastics, comprising the following steps:
将塑料和提取液混合， 得到混合物；  Mixing the plastic and the extract to obtain a mixture;
密闭环境中， 混合物在温度 80~160°C持续混匀若干时间；  In a closed environment, the mixture is continuously mixed at a temperature of 80 to 160 ° C for a certain period of time;
静置回收无机相， 无机相离心分层， 得到含有六价铬的无机层清液；  The inorganic phase is continuously recovered, and the inorganic phase is centrifugally layered to obtain an inorganic layer clear liquid containing hexavalent chromium;
所述提取液为有机溶剂与碱性溶液的混合物。  The extract is a mixture of an organic solvent and an alkaline solution.
2、 根据权利要求 1所述的方法， 其特征在于： 所述有机溶剂为苯系物， 酯和脂肪烃 中的任一种或任几种。  The method according to claim 1, wherein the organic solvent is any one or any of a benzene series, an ester and an aliphatic hydrocarbon.
3、 根据权利要求 1所述的方法， 其特征在于： 所述碱性溶液的溶质为氢氧化锂、 氢 氧化钠、 氢氧化钾、 碳酸钠和碳酸钾中的任一种或任几种。  3. The method according to claim 1, wherein the solute of the alkaline solution is any one or any of lithium hydroxide, sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate.
4、 根据权利要求 1-3中任一所述的方法， 其特征在于： 每克所述塑料和 0.01 1L所述 提取液混合。  A method according to any one of claims 1 to 3, characterized in that: 克 of said plastic and 0.01 1 L of said extract are mixed.
5、 根据权利要求 1-3中任一所述的方法， 其特征在于： 所述有机溶剂和所述碱性溶液 的体积比为 （1~10) ： ( 1-30) 。  The method according to any one of claims 1 to 3, wherein the volume ratio of the organic solvent to the alkaline solution is (1 to 10): (1-30).
6、 根据权利要求 3所述的方法， 其特征在于： 所述碱性溶液中溶质的浓度为  6. The method according to claim 3, wherein: the concentration of the solute in the alkaline solution is
0.01mol/L~lmol/L。 0.01mol/L~lmol/L.
7、 根据权利要求 1所述的方法， 其特征在于： 所述若干时间为至少 10min。  7. The method of claim 1 wherein: said plurality of times is at least 10 minutes.
8、 根据权利要求 1所述的方法， 其特征在于： 所述持续混匀的方式为搅拌、 微波、 超声、 混旋中的任一种或任几种。  8. The method according to claim 1, wherein: the manner of continuously mixing is any one or any of stirring, microwave, ultrasonic, and mixing.
9、 根据权利要求 2所述的方法， 其特征在于： 所述有机溶剂为苯、 壬烷、 乙酸乙 酯、 甲苯或二甲苯。  9. The method according to claim 2, wherein the organic solvent is benzene, decane, ethyl acetate, toluene or xylene.
PCT/CN2010/075879 2010-08-11 2010-08-11 Method for extracting hexavalent chromium from plastic WO2012019341A1 (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105806790A (en) * 2016-03-15 2016-07-27 通标标准技术服务有限公司广州分公司 Measuring method of hexavalent chromium in plastic

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB843027A (en) * 1956-11-19 1960-08-04 Phillips Petroleum Co Method for recovery of polymers
JP2006132979A (en) * 2004-11-02 2006-05-25 Fujikura Ltd Method of extracting hexavalent chromium in plastic material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB843027A (en) * 1956-11-19 1960-08-04 Phillips Petroleum Co Method for recovery of polymers
JP2006132979A (en) * 2004-11-02 2006-05-25 Fujikura Ltd Method of extracting hexavalent chromium in plastic material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
LUO DAOJUN ET AL.: "Extraction Methods for Hexavalent Chromium in Polymers", CHINESE JOURNAL OF ANALYTICAL CHEMISTRY, vol. 36, no. 9, September 2008 (2008-09-01), pages 1253 - 1256 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105806790A (en) * 2016-03-15 2016-07-27 通标标准技术服务有限公司广州分公司 Measuring method of hexavalent chromium in plastic
CN105806790B (en) * 2016-03-15 2019-02-19 通标标准技术服务有限公司广州分公司 The measuring method of Cr VI in a kind of plastics

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