CN102778374A - Method for preparing polyvinyl chloride standard fiber sample - Google Patents
Method for preparing polyvinyl chloride standard fiber sample Download PDFInfo
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- CN102778374A CN102778374A CN2012102379070A CN201210237907A CN102778374A CN 102778374 A CN102778374 A CN 102778374A CN 2012102379070 A CN2012102379070 A CN 2012102379070A CN 201210237907 A CN201210237907 A CN 201210237907A CN 102778374 A CN102778374 A CN 102778374A
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- ester plasticizer
- phthalic ester
- phthalic acid
- polyvinyl chloride
- phthalic
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Abstract
The invention relates to a method for preparing a polyvinyl chloride standard fiber sample. The method comprises the following steps of: taking 100 weight parts of polyvinyl chloride resin, 100 weight parts of phthalic acid ester plasticizer, 2-4 weight parts of heat stabilizer and 1-3 weight parts of lubricant; carrying out blending and drawing to obtain polyvinyl chloride resin fiber; measuring the content of the phthalic acid ester plasticizer in the sample by gas chromatography; working out the loss of the phthalic acid ester plasticizer, and repeating the above steps to obtain the average loss of the phthalic acid ester plasticizer; and establishing the preparation procedures for a standard sample. The content of the phthalic acid ester plasticizer in the sample prepared by the method provided by the invention can be determined in advance, the sample can be used as the polyvinyl chloride standard sample, and with the method, the content of the phthalic acid ester plasticizer in the polyvinyl chloride resin fiber has good repeatability.
Description
Technical field
The invention belongs to standard fibers specimen preparation field, particularly a kind of method for preparing PVC standard fibers sample.
Background technology
By the prepared Corvic fiber of PVC (PVC) resin spinned fiber,, and be used in the various uses owing to its good weatherability, the transparency, anti-flammability, cheap.The phthalic ester that in the Corvic fiber, is used is one of the most frequently used industrial plastifier; Because of itself and Corvic good compatibility, wide adaptability, chemical stability is good, working method is simple, raw material is easy to get, advantage such as with low cost, is often classified as universal plastifier.
But phthalic ester plasticizer type of having estrogen action and antiandrogen effect, but interference body internal system influence body growth and grow, and the long-term accumulation meeting causes deformity, canceration and mutagenesis in the body.Particularly fetus, infant and puberty the men and women when growing, need a large amount of androgen and estrogen, phthalic ester is prone to above crowd's health is produced infringement.
Health for the consumer; Chemical fibre manufacturing enterprise has all strengthened the detection to phthalate plasticizers with relevant mechanism for testing; But because the hysteresis of domestic chemical fibre standard industry development, the making that contains the PVC standard fibers sample of phthalate plasticizers also is in blank.Owing to lack the standard fibers sample, can not estimate the accuracy that phthalate plasticizers detects, in relevant mensuration and trace to the source, there are more serious detection technique defective in fields such as method affirmation and checking, Laboratory Accreditation, instrument calibration.
Summary of the invention
Technical matters to be solved by this invention provides a kind of method for preparing PVC standard fibers sample.The amount of the phthalic ester plasticizer that is contained in the sample of the present invention's preparation can confirm in advance that sample can be used as PVC standard fibers sample; Under the method, the content of phthalic ester plasticizer has good repeatability in the Corvic fiber.
A kind of method for preparing PVC standard fibers sample of the present invention comprises:
(1) gets the lubricant of 100 weight portion Corvics, 100 weight portion phthalic ester plasticizers, 2 ~ 4 weight portion thermal stabilizers, 1 ~ 3 weight portion;
(2) raw material of getting in the step (1) being put into ultrasonic oscillator vibrates under 20 ~ 30 ℃ and mixes the thing that is uniformly mixed;
(3) be 175 ~ 190 ℃ in temperature, rotating speed is under the condition of 75 ~ 80 commentaries on classics/min, and step (2) uniform mix is put into miniature blender blend 1 ~ 2min;
(4) after the blend, under the protection of anti-bellows, utilize the constant speed filament winding machine to carry out the drawing-off wire drawing, cooling obtains polyvinyl chloride fibre.
(5) the Corvic fiber that makes in the step (4) is carried out the ultrasonic extraction phthalic ester plasticizer, adopt gas chromatography-GC-MS to measure the content of phthalic ester plasticizer in the sample;
(6) step (5) gained testing result is carried out data analysis, draw under step (1) ~ (5) loss of phthalic ester plasticizer in the Corvic fiber;
(7) repeating step (1) ~ (6), under the method, the content of phthalic ester plasticizer has good repeatability in the Corvic fiber, obtains the average loss amount of phthalic ester plasticizer;
(8) according to average loss amount and step (1) ~ (5) determined method of step (7) gained phthalic ester plasticizer, set up the standard model preparation procedure.
The model of the Corvic in the said step (1) is PVC-SG5, and the degree of polymerization is 1000 ~ 1150, and viscosity number is 107 ~ 118ml/g, and the K value is 66 ~ 68, and physical aspect is Powdered.
Phthalic ester plasticizer in the said step (1) is the potpourri of butyl phthalate DBP, butyl benzyl phthalate BBP, the own ester DEHP of phthalic acid two (2-ethyl), o-phthalic acid dibutyl ester DNOP, diisononyl phthalate DINP, diisooctyl phthalate DIDP, repefral DMP and diethyl phthalate DEP.Wherein butyl phthalate DBP, butyl benzyl phthalate BBP, the own ester DEHP of phthalic acid two (2-ethyl), o-phthalic acid dibutyl ester DNOP, diisononyl phthalate DINP and six kinds of plastifier of diisooctyl phthalate DIDP are for needing the adjacent benzene class plastifier of monitoring.
Thermal stabilizer in the said step (1) is one or more in dibutyl tin laurate stabilizing agent, the barium stearate.
Lubricant in the said step (1) is one or more in calcium stearate, the cadmium stearate.
Beneficial effect
The amount of the phthalic ester plasticizer that is contained in the sample of the present invention's preparation can confirm in advance that sample can be used as PVC standard fibers sample; Under the method, the content of phthalic ester plasticizer has good repeatability in the Corvic fiber.
Description of drawings
Fig. 1 is a working method schematic flow sheet of the present invention.1 supersonic oscillations appearance, 2 raw materials, 3 miniature blend appearance 4 screw rods 5 anti-bellows 6 well heaters 7 extrusions 8 constant speed filament winding machines
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
The raw material of the Corvic fiber of producing is that PVC SG-5 resin, phthalic ester plasticizer, thermal stabilizer and mix lubricant form.Job operation: with the PVC SG-5 resin of 100g; The butyl phthalate DBP of 2g; The butyl benzyl phthalate BBP of 2g; The own ester DEHP of the phthalic acid two of 2g (2-ethyl); The o-phthalic acid dibutyl ester DNOP of 2g; The diisononyl phthalate DINP of 2g; The diisooctyl phthalate DIDP of 2g; 41.2g repefral DMP; 41.2g diethyl phthalate DEP; Barium stearate 2g; Calcium stearate 1.6g; Mix in the dibutyl tin laurate 2g ultrasonic oscillator up to mixing fully.Well-mixed material is carried out blend in miniature twin-screw blend appearance, after the blend, under the protection of anti-bellows, utilize the constant speed filament winding machine to carry out the drawing-off wire drawing, cooling obtains polyvinyl chloride fibre.The working temperature of miniature twin-screw blend appearance is 176 ℃, and screw speed is 73 rev/mins.The Corvic fiber that makes is carried out the ultrasonic extraction phthalic ester plasticizer, adopt gas chromatography-GC-MS to measure the content of phthalic ester plasticizer in the sample.The well data analysis obtains the waste of phthalic ester plasticizer in the Corvic fiber, repeats above step, and the average loss amount that gets phthalic ester plasticizer is 25% under the method.According to the average loss amount of phthalic ester plasticizer under the method, confirm that the composition of raw materials of PVC standard fibers sample is: the own ester DEHP of phthalic acid two (2-ethyl) of the butyl benzyl phthalate BBP of the PVC SG-5 resin of 100g, the butyl phthalate DBP of 2.5g, 2.5g, 2.5g, the o-phthalic acid dibutyl ester DNOP of 2.5g, the diisononyl phthalate DINP of 2.5g, the diisooctyl phthalate DIDP of 2.5g, the repefral DMP of 41.2g, the diethyl phthalate DEP of 41.2g, barium stearate 2g, calcium stearate 1.6g, dibutyl tin laurate 2g.
Claims (5)
1. method for preparing PVC standard fibers sample may further comprise the steps:
(1) gets the lubricant of 100 weight portion Corvics, 100 weight portion phthalic ester plasticizers, 2 ~ 4 weight portion thermal stabilizers, 1 ~ 3 weight portion;
(2) raw material of getting in the step (1) is carried out ultrasonic agitation under 20 ~ 30 ℃ and get uniform mix;
(3) be 175 ~ 190 ℃ in temperature, rotating speed is under 75 ~ 80 rev/mins the condition, with step (2) uniform mix blend 1 ~ 2min;
(4) after the blend, drawing-off wire drawing under windproof protection, cooling obtains polyvinyl chloride fibre;
(5) the Corvic fiber that makes in the step (4) is carried out the ultrasonic extraction phthalic ester plasticizer, measure the content of phthalic ester plasticizer in the sample;
(6) step (5) gained testing result is carried out data analysis, draw under step (1) ~ (5) loss of phthalic ester plasticizer in the Corvic fiber;
(7) the average loss amount of phthalic ester plasticizer is obtained in repeating step (1) ~ (6);
(8) according to average loss amount and step (1) ~ (5) determined method of step (7) gained phthalic ester plasticizer, set up the standard model preparation procedure.
2. a kind of method for preparing PVC standard fibers sample according to claim 1 is characterized in that the model of the Corvic in the said step (1) is PVC-SG5; The degree of polymerization is 1000 ~ 1150; Viscosity number is 107 ~ 118ml/g, and the K value is 66 ~ 68, and physical aspect is Powdered.
3. a kind of method for preparing PVC standard fibers sample according to claim 1; It is characterized in that the phthalic ester plasticizer in the said step (1) is the potpourri of butyl phthalate DBP, butyl benzyl phthalate BBP, the own ester DEHP of phthalic acid two (2-ethyl), o-phthalic acid dibutyl ester DNOP, diisononyl phthalate DINP, diisooctyl phthalate DIDP, repefral DMP and diethyl phthalate DEP.
4. a kind of method for preparing PVC standard fibers sample according to claim 1 is characterized in that, the thermal stabilizer in the said step (1) is one or more in dibutyl tin laurate stabilizing agent, the barium stearate.
5. a kind of method for preparing PVC standard fibers sample according to claim 1 is characterized in that, the lubricant in the said step (1) is one or more in calcium stearate, the cadmium stearate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012102379070A CN102778374A (en) | 2012-07-10 | 2012-07-10 | Method for preparing polyvinyl chloride standard fiber sample |
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| CN2012102379070A CN102778374A (en) | 2012-07-10 | 2012-07-10 | Method for preparing polyvinyl chloride standard fiber sample |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104451943A (en) * | 2014-12-29 | 2015-03-25 | 大连工业大学 | Flame-retardant hair polyvinyl chloride/chlorinated polyvinyl chloride fiber and melt preparation method |
| CN104611781A (en) * | 2014-12-29 | 2015-05-13 | 大连工业大学 | Production method for preparing polyvinyl chloride fibers for hair by melting method |
| CN106633505A (en) * | 2016-11-26 | 2017-05-10 | 金发科技股份有限公司 | Preparation method of standard sample composed of more than ten elements (As, Se, P and the like) and multiple phthalates in polyvinyl chloride (PVC) |
| CN106751217A (en) * | 2016-12-28 | 2017-05-31 | 广东出入境检验检疫局检验检疫技术中心 | A kind of preparation method of plasticizer-containing plastic cement standard sample |
| CN106832881A (en) * | 2017-01-16 | 2017-06-13 | 浙江省计量科学研究院 | Phthalic ester plasticizer and phosphorus flame retardant standard sample and sample preparation methods in polyurethane |
| CN108254472A (en) * | 2017-09-30 | 2018-07-06 | 广东华科检测技术服务有限公司 | Phthalic acid ester standard sample and preparation method thereof in PVC coating textile fabrics |
| CN114196139A (en) * | 2021-12-27 | 2022-03-18 | 国高材高分子材料产业创新中心有限公司 | PVC matrix atomization standard substance and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04257312A (en) * | 1991-02-07 | 1992-09-11 | Mitsubishi Rayon Co Ltd | Production of polyvinyl chloride-based fiber |
| CN101035935A (en) * | 2004-09-30 | 2007-09-12 | 钟渊化学工业株式会社 | Polyvinyl chloride fiber and process for production thereof |
| CN101143954A (en) * | 2007-10-24 | 2008-03-19 | 华东理工大学 | Polyvinyl chloride modified resin |
| CN101994166A (en) * | 2009-08-17 | 2011-03-30 | 河南瑞贝卡发制品股份有限公司 | Negative ion polyvinyl chloride fiber for wig and preparation method thereof |
-
2012
- 2012-07-10 CN CN2012102379070A patent/CN102778374A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04257312A (en) * | 1991-02-07 | 1992-09-11 | Mitsubishi Rayon Co Ltd | Production of polyvinyl chloride-based fiber |
| CN101035935A (en) * | 2004-09-30 | 2007-09-12 | 钟渊化学工业株式会社 | Polyvinyl chloride fiber and process for production thereof |
| CN101143954A (en) * | 2007-10-24 | 2008-03-19 | 华东理工大学 | Polyvinyl chloride modified resin |
| CN101994166A (en) * | 2009-08-17 | 2011-03-30 | 河南瑞贝卡发制品股份有限公司 | Negative ion polyvinyl chloride fiber for wig and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 房丽萍 等: "邻苯二甲酸酯类增塑剂分析方法进展", 《分析科学学报》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104451943A (en) * | 2014-12-29 | 2015-03-25 | 大连工业大学 | Flame-retardant hair polyvinyl chloride/chlorinated polyvinyl chloride fiber and melt preparation method |
| CN104611781A (en) * | 2014-12-29 | 2015-05-13 | 大连工业大学 | Production method for preparing polyvinyl chloride fibers for hair by melting method |
| CN106633505A (en) * | 2016-11-26 | 2017-05-10 | 金发科技股份有限公司 | Preparation method of standard sample composed of more than ten elements (As, Se, P and the like) and multiple phthalates in polyvinyl chloride (PVC) |
| CN106751217A (en) * | 2016-12-28 | 2017-05-31 | 广东出入境检验检疫局检验检疫技术中心 | A kind of preparation method of plasticizer-containing plastic cement standard sample |
| CN106832881A (en) * | 2017-01-16 | 2017-06-13 | 浙江省计量科学研究院 | Phthalic ester plasticizer and phosphorus flame retardant standard sample and sample preparation methods in polyurethane |
| CN108254472A (en) * | 2017-09-30 | 2018-07-06 | 广东华科检测技术服务有限公司 | Phthalic acid ester standard sample and preparation method thereof in PVC coating textile fabrics |
| CN114196139A (en) * | 2021-12-27 | 2022-03-18 | 国高材高分子材料产业创新中心有限公司 | PVC matrix atomization standard substance and preparation method thereof |
| CN114196139B (en) * | 2021-12-27 | 2023-08-18 | 国高材高分子材料产业创新中心有限公司 | PVC matrix atomization standard substance and preparation method thereof |
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Application publication date: 20121114 |