CN106198785B - A kind of supercritical CO2The method of fire retardant in quick separating textile - Google Patents
A kind of supercritical CO2The method of fire retardant in quick separating textile Download PDFInfo
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- CN106198785B CN106198785B CN201610495232.8A CN201610495232A CN106198785B CN 106198785 B CN106198785 B CN 106198785B CN 201610495232 A CN201610495232 A CN 201610495232A CN 106198785 B CN106198785 B CN 106198785B
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- 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
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- 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
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- 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
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Abstract
Supercritical CO is used the present invention relates to a kind of2The method of fire retardant in quick separating textile.It is long the present invention be directed to prohibit/limit the use of fire retardant (bromine system and organic phosphorus) disengaging time in current textile, and organic solvent usage amount it is big, it is toxic not environmentally the disadvantages of, the method for proposing separation polycyclic aromatic hydrocarbon in the Supercritical fluid chromatography technology short time, this method have many advantages, such as quickly, it is favorable reproducibility, easy to operate, it is few using quantity of solvent, environmentally protective.The Instrument crosslinkings such as technical solution of the present invention and gas chromatograph-mass spectrometer (GC-MS), gas chromatograph or Liquid Chromatography-Tandem Mass Spectrometry instrument are, it can be achieved that prohibiting/limiting the use of the quick separating detection of fire retardant in textile.
Description
Technical field
The present invention relates to a kind of methods of quick separating fire retardant, in particular to a kind of to use supercritical CO2Fluid is quick
The method for separating the fire retardant in textile.
Background content
In recent years, fire is increased, caused by lose and get worse, therefore the demand to fire retardant is increasing.Mesh
Preceding common fire retardant both at home and abroad is mostly bromine system, organic phosphorus product.However numerous studies prove, the bromine in clothing or textile
Flame retardant can penetrate into environment, and accumulate in living organism as time goes by, destroy Endocrine Activity, influence first
Shape gland function point analysis, causes hormonal disorder, influences brain development, if especially pregnant woman excessively contacts, can directly result in new
Raw birth weight is too low, IQ is relatively low and capacity is impaired.In addition, the organic phosphorus flame retardant in clothing or textile
With bioaccumulation, cerebral tissue can be encroached on and then permanently damage the behavior, memory and learning ability of people, and had
Carcinogenicity.European Union's dangerous material and related amendment: this 3 regulations of 79/663EC, 83/264EEC and 2003/1/1/EC are to bromine
System and use of the organic phosphorus flame retardant in textile are limited.Oeko-Tex 100 (2016) ecological textile and skin
It requires that 20 kinds of bromine systems and organic phosphorus flame retardant must not be contained in all kinds of textiles in leather goods Recognized Standards.China standard GB/T
18885-2009 has also carried out stringent limitation to 6 kinds of fire retardants.Due to textile complicated composition, to obtain data it is accurate,
The analysis of favorable reproducibility is as a result, sample pre-treatments are important a link.Prohibit/limit the use of the pretreatment technology master of fire retardant at present
Have: Soxhlet extraction, ultrasonic extraction, microwave radiation exaraction, Solid Phase Extraction etc..These technologies, which all have time-consuming, organic solvent, to be made
The defects of dosage is big.
In recent years, supercritical carbon dioxide has become research heat as a kind of environmentally protective source and extensive fluid media (medium)
Point is widely used in the research and application process of supercritical liquid extraction technique (SFE).Supercritical fluid extraction is modern age
The new and high technology occurred in chemical separating, SFE integrally combine traditional distillation and organic solvent extraction, utilize supercritical CO2
Matrix is efficiently separated, extracted and purified with extract by excellent solvent power.SFE uses supercritical CO2Material is extracted
It takes.Supercritical CO2It is safe and nontoxic and cheap liquid, there is the diffusion coefficient of similar gas, the dissolving power of liquid, table
Face tension is zero, can be penetrated among solid matter rapidly, have it is efficient, not oxidizable, pure natural, without spies such as chemical contaminations
Point.Supercritical fluid extraction isolation technics is to utilize the solvability of supercritical fluid and its density closely related, passes through change
Pressure or temperature change the density of supercritical fluid substantially, in the supercritical state, by supercritical fluid and object to be separated
Matter contact extracts it selectively successively polarity size, boiling point height and relative molecular mass ingredient of different sizes
Out.At present both at home and abroad about supercritical CO2The report of abstraction technique is mainly it in Chinese herbal medicine, food technology, perfume industry
With the application in terms of environmental protection technology, but for the supercritical CO for prohibiting/limiting the use of fire retardant in textile2Extraction not yet has been reported that.And
Prohibit in traditional textile/limit the use of fire retardant detection method it is not only time-consuming but also pollution environment.
Summary of the invention
Supercritical CO is used the object of the present invention is to provide a kind of2The side of fire retardant in fluid quick separating textile
Method.It the described method comprises the following steps:
A) textile sample is added in extraction kettle, adds cosolvent, set extraction temperature and pressure, then to weaving sample
Product carry out supercritical carbon dioxide static extracting；
The fire retardant extracted is used collection solvent molten by the outlet valve for b) opening extraction kettle in cooling separating and collecting in device
Solution recycling；
C) it carries out qualitative and quantitative analysis to extract solution.
In step a), the cosolvent is selected from normal propyl alcohol, methanol, toluene, acetonitrile, tetrahydrofuran and theirs is mixed
Close object.
In step a), set extraction temperature is 40 DEG C -100 DEG C.
In step a), set pressure is 12MPa-50MPa.
In step a), the duration for carrying out supercritical carbon dioxide static extracting to textile sample is 20 minutes to 70
Minute.
In step a), the flow velocity of the supercritical carbon dioxide is 10mL/min-100mL/min.
In step b), the collection solvent is selected from methanol, n-hexane+acetone (7+3, volume ratio), acetone, acetonitrile, with
And their mixture.
In step c), the Qualitative and quantitative analysis is selected from gas chromatograph-mass spectrometer (GC-MS), gas chromatograph and liquid phase
Chromatographic tandem mass spectrograph.
It is long the present invention be directed to prohibit/limit the use of fire retardant (bromine system and organic phosphorus) disengaging time in current textile, and
Organic solvent usage amount is big, it is toxic not environmentally the disadvantages of, propose the side of separation polycyclic aromatic hydrocarbon in the Supercritical fluid chromatography technology short time
Method, this method have many advantages, such as quickly, it is favorable reproducibility, easy to operate, it is few using quantity of solvent, environmentally protective.Technology of the invention
The Instrument crosslinkings such as scheme and gas-chromatography-mass spectrometer, gas chromatograph or Liquid Chromatography-Tandem Mass Spectrometry instrument are, it can be achieved that spin
Prohibit/limit the use of the quick separating detection of fire retardant in fabric.
Specific embodiment
Below with reference to following embodiment, the present invention will be described in more detail.
Embodiment 1:
10g or so textile sample is added in extraction kettle, cosolvent-normal propyl alcohol of 1mL is added, sets extraction temperature 60
DEG C, pressure 30MPa, supercritical carbon dioxide static extracting 20min is carried out to it；Outlet valve is opened, is to collect solvent with acetone,
Coutroi velocity is 20mL/min so that acetone volatile quantity is preferably minimized, and the fire retardant extracted is used in cooling separating and collecting in device
The recycling of 13mL acetone solution, extract solution gas chromatograph-mass spectrometer (GC-MS), gas chromatograph or Liquid Chromatography-Tandem Mass Spectrometry
Instrument carries out qualitative and quantitative analysis.
Embodiment 2:
10g or so textile sample is added in extraction kettle, cosolvent-methanol of 1mL is added, sets extraction temperature 60
DEG C, pressure 30MPa, supercritical carbon dioxide static extracting 20min is carried out to it；Open outlet valve, coutroi velocity 20mL/
Min (appropriate adjustment speed is preferably minimized acetone volatile quantity), the fire retardant extracted is used in cooling separating and collecting in device
The recycling of 13mL acetone solution, extract solution gas chromatograph-mass spectrometer (GC-MS), gas chromatograph or Liquid Chromatography-Tandem Mass Spectrometry
Instrument carries out qualitative and quantitative analysis.
Embodiment 3:
10g or so textile sample is added in extraction kettle, cosolvent-normal propyl alcohol of 1mL is added, sets extraction temperature 60
DEG C, pressure 30MPa, supercritical carbon dioxide static extracting 40min is carried out to it；Open outlet valve, coutroi velocity 20mL/
Min, the fire retardant extracted are recycled in cooling separating and collecting in device with 13mL acetone solution, extract solution gas phase color
Spectrum-mass spectrometer, gas chromatograph or Liquid Chromatography-Tandem Mass Spectrometry instrument carry out qualitative and quantitative analysis.
Embodiment 4:
10g or so textile sample is added in extraction kettle, cosolvent-normal propyl alcohol of 1mL is added, sets extraction temperature 50
DEG C, pressure 40MPa, supercritical carbon dioxide extracting 40min is carried out to it；13mL acetone is added in collection device, opens out
Expect that valve, coutroi velocity 50mL/min collect precipitate, extract solution gas chromatograph-mass spectrometer (GC-MS), gas chromatograph
Or Liquid Chromatography-Tandem Mass Spectrometry instrument carries out qualitative and quantitative analysis.
Embodiment 5:
10g or so textile sample is added in extraction kettle, cosolvent-methanol of 1mL is added, sets extraction temperature 40
DEG C, pressure 30MPa, supercritical carbon dioxide extracting 40min is carried out to it；13mL acetone is added in collection device, opens out
Expect that valve, coutroi velocity 30mL/min collect precipitate, extract solution gas chromatograph-mass spectrometer (GC-MS), gas chromatograph
Or Liquid Chromatography-Tandem Mass Spectrometry instrument carries out qualitative and quantitative analysis.
Embodiment 6:
10g or so textile sample is added in extraction kettle, cosolvent-methanol of 1mL is added, sets extraction temperature 80
DEG C, pressure 50MPa, supercritical carbon dioxide extracting 30min is carried out to it；13mL acetone is added in collection device, opens out
Expect that valve, coutroi velocity 60mL/min collect precipitate, extract solution gas chromatograph-mass spectrometer (GC-MS), gas chromatograph
Or Liquid Chromatography-Tandem Mass Spectrometry instrument carries out qualitative and quantitative analysis.
The textile sample used in above-described embodiment 1-6 is the sample of textile sampling common in the industry, including fiber, yarn
Line, fabric and finished product etc..Separately below by gas chromatograph-mass spectrometer (GC-MS), gas chromatograph, liquid chromatograph to aforementioned reality
The extract solution that a 1-6 is obtained is applied to carry out qualitative and quantitative analysis.
Each detecting instrument parameter is as follows:
Test case 1- gas chromatograph test parameter
Chromatographic column: DB-5 quartz capillary column (30m × 0.32mm × 0.25 μm)；Injector temperature: 280 DEG C；Carrier gas:
Nitrogen, purity >=99.999%, flow velocity 1.34mL/min；FPD detector temperature: 250 DEG C；Temperature program: initial temperature 150
DEG C, 300 DEG C are raised to 30 DEG C/min, keeps 3min；Hydrogen flowing quantity: 75mL/min；Air mass flow: 100mL/min；Sample volume:
1.0μL；Input mode: Splitless injecting samples, valve opening after 1.0min.
Test case 2- gas chromatograph-mass spectrometer (GC-MS) test parameter
Chromatographic column: DB-5MS capillary chromatographic column (30m × 0.25mm × 0.25 μm)；Temperature program: 100 DEG C (keep
250 DEG C 1min) are raised to 30 DEG C/min, then is raised to 300 DEG C with 10 DEG C/min；Injector temperature: 250 DEG C；Chromatography-mass spectroscopy interface
Temperature: 300 DEG C；Carrier gas: helium, purity >=99.999%, flow 1.0mL/min；Ionization mode: EI；Ionization energy: 70eV；From
Source temperature: 230 DEG C；Test mode: it sweeps entirely and sweeps while carrying out with ion；Input mode: Splitless injecting-Sample；Sampling volume: 1 μ
L；Solvent delay: 1min.
Test case 3- Liquid Chromatography-Tandem Mass Spectrometry instrument test parameter
Input mode: automatic sampling；Sampling volume: 5uL；Pillar: Acquity UPLC BEH C18 (100mm×2.1mm
×1.7μm)；Mobile phase: acetonitrile, 5mmol/mL ammonium acetate solution；Flow velocity: 0.3mL/min；Gradient: 10% acetonitrile maintains
1min, 3min become 60% acetonitrile, and 5min becomes 70% acetonitrile, and 6min becomes 100% acetonitrile, and 6.1min becomes 10% acetonitrile；
Ion source: electric spray ion source (ESI)；Detection mode: negative ions multiple-reaction monitoring (MRM) mode；Capillary voltage:
3.0kV (positive/negative ion)；Ion source temperature: 110 DEG C；Desolvation temperature: 380 DEG C；Desolventizing gas (N2) flow velocity: 600L/
h；Taper hole blowback air (N2) flow velocity: 50L/h；Collision gas (Ar) flow velocity: 0.16mL/min.
The fire retardant rate of recovery (%)
By the analyzing detecting method of above-mentioned test case 1-3 respectively to the fire retardant rate of recovery in the sample of embodiment 1-6
When being detected, the discovery fire retardant rate of recovery has reached higher level, and is further discovered that the specified conditions of embodiment 1
The fire retardant rate of recovery of final textile sample under (extraction temperature, pressure and extraction time) is obviously higher than other embodiments
Textile sample.
In the methods of the invention, organic solvent amount used in 10g textile samples is seldom, and wherein cosolvent is only 100
~1000 μ L collect solvent and also only use 10mL to 30mL.And standard GB/T/and T 24279-2009 " textile is prohibited/it limits the use of
The measurement of fire retardant " in entire test method it is as follows: 1g textile sample is surpassed using 30mL n-hexane-acetone (7+3, volume ratio)
Sound extracts, and extracting solution rotation is steamed near dry, and is dissolved with n-hexane-acetone (7+3) and is settled to 2mL.1g weaves in the national standard
Sample at least uses 32mL n-hexane-acetone (7+3).
The present invention relates to the new method for prohibiting/limiting the use of fire retardant (bromine system and organic phosphorus) in a kind of Rapid Extraction textile,
Its technical characterstic is using supercritical carbon dioxide extracting and separation process action principle, using supercritical carbon dioxide to bromine system
With organic phosphorus flame retardant solubility with higher, i.e., the pressure and temperature of carbon dioxide is controlled by special device, to two
The influence of carbonoxide supercritical solvent ability and carry out.The deficiencies of this method avoid conventional method time-consuming consumptive materials, at 30 points
Ten several above bromine systems and organic phosphorus flame retardant can be separated in clock, the method is quick, and environmental protection, process is simple, and reproducibility
It is good.And technical solution of the present invention and gas chromatograph, gas chromatograph-mass spectrometer (GC-MS), Liquid Chromatography-Tandem Mass Spectrometry instrument connect
With, it can be achieved that prohibiting/limiting the use of the quick separating detection of fire retardant in textile.Taboo through the method detection/limit the use of fire retardant recycling
Rate is between 90%~105%.
Although described above is use supercritical CO2The embodiment of fire retardant in fluid quick separating textile, still,
Under above-mentioned introduction of the invention, those skilled in the art can carry out various improvement and change on the basis of the above embodiments
Shape, and these are improved or deformation is within the scope of the present invention.It will be understood by those skilled in the art that above specific
Description is intended merely to explain the purpose of the present invention, is not intended to limit the present invention.Protection scope of the present invention by claim and
Its equivalent limits.
Claims (1)
1. a kind of method of quick separating fire retardant, it is characterised in that the method uses supercritical CO2The weaving of fluid quick separating
Fire retardant in product；
It the described method comprises the following steps:
A) textile sample is added in extraction kettle, adds cosolvent, set extraction temperature and pressure, then to textile sample into
Row supercritical carbon dioxide static extracting；
B) outlet valve for opening extraction kettle dissolves back the fire retardant extracted in cooling separating and collecting in device with collection solvent
It receives；
C) it carries out qualitative and quantitative analysis to extract solution；
In step b), the solvent of collecting is selected from methanol, volume ratio as the n-hexane and acetone, acetone, acetonitrile of 7:3, and
Their mixture；
Wherein extraction temperature is 60 DEG C, pressure 30MPa, and the time is 20 minutes, and the flow velocity of supercritical carbon dioxide is 20mL/
min；
Wherein 10g textile only needs the collection solvent of cosolvent and 10mL-30mL using 100 μ L-1000 μ L；
Wherein the fire retardant is bromine system and organic phosphorus flame retardant；The cosolvent be selected from normal propyl alcohol, methanol, toluene, acetonitrile,
Tetrahydrofuran and their mixture.
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| CN101768286A (en) * | 2009-12-31 | 2010-07-07 | 茂名学院 | Method for separating polybrominated diphenylether from waste electronic plastic |
| CN102043031A (en) * | 2010-11-18 | 2011-05-04 | 江苏大学 | Propolis supercritical CO2 extract GC-MS fingerprint and construction method thereof |
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| DE10139479A1 (en) * | 2001-08-10 | 2003-02-27 | Schwabe Willmar Gmbh & Co | Hop extracts, process for their preparation and use |
| CN1275969C (en) * | 2002-03-14 | 2006-09-20 | 北京同源医药科技有限公司 | Application of active ingredient of coumarin category distilled from dahurian angelica in preparing medicine for curing high blood pressure and its extracting method |
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|---|---|---|---|---|
| CN101768286A (en) * | 2009-12-31 | 2010-07-07 | 茂名学院 | Method for separating polybrominated diphenylether from waste electronic plastic |
| CN102043031A (en) * | 2010-11-18 | 2011-05-04 | 江苏大学 | Propolis supercritical CO2 extract GC-MS fingerprint and construction method thereof |
Non-Patent Citations (4)
| Title |
|---|
| Extraction of brominated flame retardants from polymeric waste material using different solvents and supercritical carbon dioxide;Abdel mnim Altwaiq et al.;《Analytica Chimica Acta》;20031231;第491卷;第111-123页 * |
| 超临界C02萃取废电路板中阻燃剂的研究;王璟等;《厦门大学学报》;20080731;第47卷(第4期);第547-551页 * |
| 超临界CO2流体萃取软体家具中的新型溴系阻燃剂;陈英杰;《商品与质量》;20141231;第252页 * |
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