CN105806736A - Quantitative detection method for blending product of poly aryl oxadiazole fiber and acrylon or spandex - Google Patents
Quantitative detection method for blending product of poly aryl oxadiazole fiber and acrylon or spandex Download PDFInfo
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- CN105806736A CN105806736A CN201610167311.6A CN201610167311A CN105806736A CN 105806736 A CN105806736 A CN 105806736A CN 201610167311 A CN201610167311 A CN 201610167311A CN 105806736 A CN105806736 A CN 105806736A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
The invention provides a quantitative detection method for a blending product of poly aryl oxadiazole fiber and acrylon or spandex. On the basis of in-depth study, dimethylformamide is selected as a dissolution reagent, the most accurate and effective dissolving temperature, solvent dosage and dissolving mode are determined through a great number of tests, poly aryl oxadiazole fibers can be fully protected under the conditions, acrylon or spandex can be fully and fast dissolved, the final detection result and actual numerical value can be kept highly consistent, and the quantitative detection method is high in precision, shortens detection time, saves detection cost and improves detection efficiency.
Description
Technical field
The invention belongs to textile fiber detection field, be specifically related to the quantitative assay of a kind of poly-virtue diazole fiber and acrylon, spandex blending product.
Background technology
Poly-virtue diazole fiber, English name is aromaticpolyoxadiazolefiber, is called for short POD fiber.On molecular structure, main chain contains phenyl ring and diazole ring, and segment contains aromatic group, and macromolecular chain is rigid rod structure.Compared to common chemical fibre, it has the heat-resisting quantity of brilliance, excellent anti-flammability and electrical insulating property, good hygroscopicity, dyeability and high temperature resistant dimensional stability, is a kind of various aspects of performance excellence, Stability Analysis of Structures the special high temperature-resistant fire resistance fibre with Chinese independent intellectual property right.POD fiber is by the combination property of its excellence, it has also become the new fiber materials of the key areas such as defence and military, Aero-Space, special type protection, Environmental Industry.Jiangsu Baode New Material Co., Ltd. started industrialization production process (trade name: Powerleader synthetic fibre) from 2011, and current production line output is 400 tons/year, and among constantly expanding.POD fiber uses more and more extensive, but it is as poly-virtue diazole fiber and uses more and more extensive, blending functional material in conjunction with poly-virtue diazole fiber with other fiber specialities gets more and more, but the method standard of detection by quantitative poly-virtue diazole fiber is current or blank at present.In quality inspection field, fiber content quantitative analysis for blending product generally adopts chemical dissolution method, so-called chemical dissolution method seeks to the component selecting certain reagent to dissolve in blending product, then the content of other component is calculated, but chemical dissolution method tends to damage residual fiber, causes the inaccurate of certainty of measurement.
Summary of the invention
The present invention is to solve that above-mentioned prior art exists test problems, provide a kind of quick, accurate to poly-virtue diazole fiber and acrylon or the quantitative assay with spandex blending product, use reagent and the dissolving method of the present invention, can fast and effectively dissolved constituent acrylon, spandex, and complete reservation poly-virtue diazole fiber, thus completing the detection by quantitative for blending product.
The technical scheme is that a kind of poly-virtue diazole fiber of offer and acrylon or the quantitative assay with spandex blending product, including following sequential steps:
(1) blending product is carried out pretreatment, remove surface impurity；
(2) pretreated blending product is weighed, obtain gross mass m0；
(3) dissolve blending product with dimethylformamide, keep 75 DEG C～80 DEG C, dissolve 60～90min；
(4) after dissolving, remaining product water cleans to neutral, is subsequently placed in constant temperature oven and dries, weighs the residual mass of blending product after being cooled to room temperature, must gather the quality m of virtue diazole fiber1, in blending product, the quality of acrylon or spandex is then m2=m0-m1, thus quantitative to constituent content in blending product.
The damage of the solution temperature of 75 DEG C～80 DEG C poly-virtue diazole fiber is less, and now acrylon or spandex can almost be completely dissolved so that the degree that final testing result can keep certain with actual numerical value is consistent.Preferably, the solution temperature in step (3) is 78 DEG C, and the damage of poly-virtue diazole fiber is minimum at such a temperature, and now acrylon or spandex can be completely dissolved so that final testing result and actual numerical value can keep highly consistent.
Preferably, the dimethylformamide consumption in step (3) is that every gram of blending product adds 80mL solvent.When the amount of solubilising reagent is too small, dissolving fiber in blending product can not get abundant dissolving, make testing result inaccuracy, when the consumption of solubilising reagent is too much, although blending product can be made fully to dissolve, but can cause the waste of reagent undoubtedly, increase testing cost, when the bath raio controlling blending product and reagent is aforementioned proportion, blending product can either be made fully to dissolve, the consumption of solubilising reagent can be saved again.
Preferably, the dissolving method in step (3) is: first dissolve 60min, changes solvent re-dissolved 30min afterwards, and is shaken gently for 1 time every 10min.Above-mentioned dissolution mechanism can accelerate to dissolve fibrolysis when concussion continuously, detection time is greatly reduced, improves detection efficiency.
Preferably, preprocess method in step (1) is: materialses and is placed in soxhlet's extractor, 1h is extracted, per hour at least circulation 6 times, after the ether in sample volatilizees with ether, sample is immersed in cold water, soaking 60min, then soak 1h in the water of (65 scholar 5) DEG C, the ratio of water and volume of sample is 100:1, it is stirred continuously solution, then suction or centrifuge dehydration, dry.Said method can effectively process poly-virtue diazole fiber and acrylon or generate, with spandex blending product, the impurity produced under peculiar technique, improves final accuracy of detection.
Preferably, the drying temperature in step (4) is 115-120 DEG C.
Invention is on the basis of further investigation; select dimethylformamide as solubilising reagent; and determine the most effective solution temperature, solvent load, dissolution mechanism through substantial amounts of test; can be adequately protected poly-virtue diazole fiber under these conditions, thoroughly dissolves acrylon or spandex so that final testing result and actual numerical value can keep highly consistent; there is significantly high accuracy; and reduce the detection time, save testing cost, improve detection efficiency.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further details, but is not limiting the scope of the invention.
Embodiment 1
Take and gather virtue diazole fiber and acrylon blending product 10 grams (ratio of known wherein poly-virtue diazole fiber and acrylon is 55/45), it is placed in soxhlet's extractor, 1h is extracted, per hour at least circulation 6 times, after the ether in sample volatilizees with ether, sample is immersed in cold water, soaking 60min, then soak 1h in the water of 60 DEG C, the ratio of water and volume of sample is 100:1, it is stirred continuously solution, then suction or centrifuge dehydration, dry.Blending product after processing is weighed, obtains gross mass；Dissolve blending product with 800ml dimethylformamide, keep 75 DEG C, first dissolve 60min, change solvent re-dissolved 30min afterwards, and be shaken gently for 1 time every 10min；After dissolving, remaining product water cleans to neutral, is subsequently placed in 115 DEG C of constant temperature ovens and dries, weighs the residual mass of blending product after being cooled to room temperature, must gather the quality m of virtue diazole fiber1, acrylon in blending product, spandex quality be then m2=m0-m1, thus quantitatively obtaining component ratio in blending product is 54.73/45.27.
Embodiment 2
Take the poly-virtue diazole fiber in 10 grams of embodiments 1 and acrylon blending product (ratio of known wherein poly-virtue diazole fiber and acrylon is 55/45), solution temperature is 80 DEG C, other method is identical with embodiment 1, and finally quantitatively obtaining component ratio in blending product is 55.23/44.77.
Embodiment 3
Take the poly-virtue diazole fiber in 10 grams of embodiments 1 and acrylon blending product (ratio of known wherein poly-virtue diazole fiber and acrylon is 55/45), solution temperature is 78 DEG C, other method is identical with embodiment 1, and finally quantitatively obtaining component ratio in blending product is 55.12/44.88.
Embodiment 4
Take and gather virtue diazole fiber and spandex blending product 10 grams (ratio of known wherein poly-virtue diazole fiber and spandex is 65/35), it is placed in soxhlet's extractor, 1h is extracted, per hour at least circulation 6 times, after the ether in sample volatilizees with ether, sample is immersed in cold water, soaking 60min, then soak 1h in the water of 70 DEG C, the ratio of water and volume of sample is 100:1, it is stirred continuously solution, then suction or centrifuge dehydration, dry.Blending product after processing is weighed, obtains gross mass；Dissolve blending product with 800ml dimethylformamide, keep 75 DEG C, first dissolve 60min, change solvent re-dissolved 30min afterwards, and be shaken gently for 1 time every 10min；After dissolving, remaining product water cleans to neutral, is subsequently placed in 120 DEG C of constant temperature ovens and dries, weighs the residual mass of blending product after being cooled to room temperature, must gather the quality m of virtue diazole fiber1, acrylon in blending product, spandex quality be then m2=m0-m1, thus quantitatively obtaining component ratio in blending product is 64.62/35.38.
Embodiment 5
Taking and gather virtue diazole fiber and spandex blending product 10 grams (ratio of known wherein poly-virtue diazole fiber and spandex is 65/35), solution temperature is 80 DEG C, and other method is identical with embodiment 1, and finally quantitatively obtaining component ratio in blending product is 65.29/34.71.
Embodiment 6
Taking and gather virtue diazole fiber and spandex blending product 10 grams (ratio of known wherein poly-virtue diazole fiber and spandex is 65/35), solution temperature is 78 DEG C, and other method is identical with embodiment 1, and finally quantitatively obtaining component ratio in blending product is 65.11/34.89.
Claims (6)
1. a poly-virtue diazole fiber and acrylon or the quantitative assay with spandex blending product, it is characterised in that include following sequential steps:
(1) blending product is carried out pretreatment, remove surface impurity；
(2) pretreated blending product is weighed, obtain gross mass m0；
(3) dissolve blending product with dimethylformamide, keep 75 DEG C～80 DEG C to dissolve 60～90min；
(4) after dissolving, remaining product water cleans to neutral, is subsequently placed in constant temperature oven and dries, weighs the residual mass of blending product after being cooled to room temperature, must gather the quality m of virtue diazole fiber1, acrylon in blending product, spandex quality be then m2=m0-m1, thus quantitatively obtaining constituent mass in blending product.
2. a kind of poly-virtue diazole fiber according to claim 1 and acrylon or the quantitative assay with spandex blending product, it is characterised in that the solution temperature in step (3) is 78 DEG C.
3. a kind of poly-virtue diazole fiber according to claim 1 and acrylon or the quantitative assay with spandex blending product, it is characterised in that the dimethylformamide consumption in step (3) is that every gram of blending product adds 80mL solvent.
4. a kind of poly-virtue diazole fiber according to claim 1 and acrylon or the quantitative assay with spandex blending product, the concrete dissolving method that it is characterized in that in step (3) is: first dissolve 60min, change solvent re-dissolved 30min afterwards, and be shaken gently for 1 time every 10min.
5. a kind of poly-virtue diazole fiber according to claim 1 and acrylon or the quantitative assay with spandex blending product, the preprocess method that it is characterized in that in step (1) is: materialses and is placed in soxhlet's extractor, 1h is extracted with ether, at least circulation 6 times per hour, after the ether in sample volatilizees, sample is immersed in cold water, soak 60min, 1h is soaked again in the water of (65 scholar 5) DEG C, the ratio of water and volume of sample is 100:1, it is stirred continuously solution, then suction or centrifuge dehydration, dry.
6. a kind of poly-virtue diazole fiber according to claim 1 and acrylon or the quantitative assay with spandex blending product, it is characterised in that the drying temperature in step (4) is 115-120 DEG C.
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| CN201610167311.6A CN105806736A (en) | 2016-03-23 | 2016-03-23 | Quantitative detection method for blending product of poly aryl oxadiazole fiber and acrylon or spandex |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109142124A (en) * | 2018-08-30 | 2019-01-04 | 必维申优质量技术服务江苏有限公司 | A kind of improved modified acrylic fibre qualitative and quantitative analysis method |
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| CN103091415A (en) * | 2012-12-30 | 2013-05-08 | 浙江工业大学 | Method for determining blending components and content in bi-component blending fabric containing dacron |
| CN104122162A (en) * | 2013-04-26 | 2014-10-29 | 广东省东莞市质量监督检测中心 | Quantitative determination method for fiber content of viloft fiber and acrylic fiber or spandex blended textiles |
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- 2016-03-23 CN CN201610167311.6A patent/CN105806736A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103091415A (en) * | 2012-12-30 | 2013-05-08 | 浙江工业大学 | Method for determining blending components and content in bi-component blending fabric containing dacron |
| CN104122162A (en) * | 2013-04-26 | 2014-10-29 | 广东省东莞市质量监督检测中心 | Quantitative determination method for fiber content of viloft fiber and acrylic fiber or spandex blended textiles |
Non-Patent Citations (2)
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| 姜磊等: ""二甲基甲酰胺法和硫氰酸钠法对羊毛/腈纶混纺产品定量分析方法比较"", 《中国纤检》 * |
| 朱庆芳等: "《中华人民共和国国家标准GB/T 2910.12-2009/ISO 1833-12：2006 纺织品 定量化学分析 第12部分：聚丙烯腈纤维、某些改性聚丙烯腈纤维、某些含氯纤维或某些弹性纤维与某些其他纤维的混合物（二甲基甲酰胺法）》", 15 June 2009 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109142124A (en) * | 2018-08-30 | 2019-01-04 | 必维申优质量技术服务江苏有限公司 | A kind of improved modified acrylic fibre qualitative and quantitative analysis method |
| CN109142124B (en) * | 2018-08-30 | 2020-12-08 | 必维申优质量技术服务江苏有限公司 | Improved qualitative and quantitative analysis method for modified polyacrylonitrile fiber |
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Application publication date: 20160727 |