CN103543088A - Test method for rheological property of fiber-grade nylon 6 slice melt - Google Patents
Test method for rheological property of fiber-grade nylon 6 slice melt Download PDFInfo
- Publication number
- CN103543088A CN103543088A CN201310395971.6A CN201310395971A CN103543088A CN 103543088 A CN103543088 A CN 103543088A CN 201310395971 A CN201310395971 A CN 201310395971A CN 103543088 A CN103543088 A CN 103543088A
- Authority
- CN
- China
- Prior art keywords
- slice
- fibre
- grade nylon
- nylon
- grade
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a test method for rheological property of a fiber-grade nylon 6 slice melt. The test method comprises the following steps: (1) preheating the fiber-grade nylon 6 slice; (2) measuring the water content of the preheated fiber-grade nylon 6 slice; (3) measuring the apparent shear rate and the apparent shear stress of the fiber-grade nylon 6 slice melt through a capillary rheometer; (4) checking to obtain a real apparent shear rate and a real apparent shear stress; (5) calculating the real apparent shear viscosity of the fiber-grade nylon 6 slice melt. Through the test method for the rheological property of the fiber-grade nylon 6 slice melt, the problems that the nylon 6 is easy to degrade, the experimental results fluctuate seriously and the reproducibility of experimental data is poor in the previous test process for the rheological property of the fiber-grade nylon 6 slice melt are solved.
Description
Technical field
The invention belongs to the technical field that fibre-grade section melt rheological property can be tested, more particularly, relate to thermal pretreatment and the rheology testing method of fibre-grade nylon 6 slice.
Background technology
Polyamide fibre (nylon) was developed in 1938, was develop the earliest in the world and realize industrialized synthon the earliest, and of many uses, output is only second to dacron, is second largest synthon kind.Polycaprolactam (nylon 6) is one of principal item in polyamide, and nylon 6 long filaments have good wearing quality, intensity and elastic recovery, is the very good material of grade textiles.Civilian high speed spinning is in great demand with section in recent years, keeps rapid growth.But the material quality of PA6 fiber is with abroad gap is obvious in actual use for a long time, and high speed spinning is mainly monopolized by external and Taiwan minority enterprise with section.The quality index disappearance of PA6 section and raw material for high-speed spinning in industry, domestic new technology CPL and polymerization PA6 section thereof are also immature for high-speed spinning, and high-end lack of material becomes the bottleneck of restriction industry development.Domestic high-speed spinning is cut into slices with PA6 in recent years, has the problems such as spinnability is poor always, seriously restricts the development of China PA6 fiber, therefore study domestic and international civilian high speed spinning, with composition, structure and the performance difference of section, has important using value.
The factor that affects fiber spinnability is a lot, and wherein the quality of section is one of key factor.The PA6 spinnability Study on influencing factors of open report is less both at home and abroad, is mostly the experience in practical application.The people such as Khanna have investigated respectively, different drying conditions, and different water cut is on the impact of PA6 section rheological property.Experiment shows in spinning process, needs the strict water cut of controlling section, cuts into slices moisture too high, can be hydrolyzed, and molecular weight and molecular weight, produces bubble and head while causing spinning; Moisture too low, when high temperature stops for a long time, can cause viscosity to increase.The spinnability situation that generally, can indirectly reflect fiber by the rheological property of section melt.Yet the person's character very easily absorbing water due to nylon 6 slice itself, in rheometer test process, cuts into slices and moisturely very easily fluctuate, so rheological data often fluctuates, and is difficult to repeat.So the rheological property that accurately characterizes fibre-grade nylon 6 slice melt all has great importance for theoretical basis research and actual production.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, proposed a kind of method of testing of fibre-grade nylon 6 slice melt rheological behaviour, solved in the past in test process, rheological data fluctuation is larger, the problem that Data duplication is poor.
Technical purpose of the present invention is achieved by following technical proposals:
A method of testing for fibre-grade nylon 6 slice rheological behaviour, according to following step, carry out:
Step 1, carries out thermal pretreatment by fibre-grade nylon 6 slice;
Step 2, measures the fibre-grade nylon 6 slice water percentage after thermal pretreatment;
Step 3, by the apparent shear rate γ of capillary rheometer determining fibre-grade nylon 6 slice melt
awith apparent shear stress σ
a;
Step 4, by Weissenberg-Rabinowitch proofread and correct and Bagely proofread and correct try to achieve the true shear rate γ of fibre-grade nylon 6 slice melt and true shear stress σ (Zhou Chixing chief editor. polymeric rheology experiment and application [M]. Shanghai: publishing house of Shanghai Communications University, 2003);
Step 5, by the true shear viscosity η of following formula calculating fibre-grade nylon 6 slice melt,
Wherein:
η is true shear viscosity;
γ is true shear rate;
σ is true shear stress.
In the method for testing of the invention described above, in described step (1), thermal pretreatment is that constant temp. heating is processed in vacuum drying oven, fibre-grade nylon 6 slice is placed in to the weighing disk with ground, and then being placed in constant-temperature vacuum baking oven thermal pretreatment, the temperature of constant-temperature vacuum baking oven is greater than the glass temperature of fibre-grade nylon 6 slice; For fibre-grade nylon 6 slice, oven temperature is 90-130 ℃, preferably 100-120 ℃; In baking oven, be 10-20h standing time, preferably 15-19h.
In the method for testing of the invention described above, in described step (2), the weighing disk that fills fibre-grade nylon 6 slice band ground is taken out from vacuum drying oven, be positioned in vacuum dryer, then measure its water percentage, use Chengdu Instruement Factory of manufacturer model: UGI-IC solid drimeter.
In the method for testing of the invention described above, by the pre-service of step (1), so that moisture control is at 200-300ppm.
In the method for testing of the invention described above, in described step (3), in rheometer test process, the melting time is 3-6min.
In technical scheme of the present invention, section is placed on and in weighing disk, is then placed in vacuum drying oven thermal pretreatment, and be positioned over immediately in vacuum dryer after thermal pretreatment, can be fine the water percentage of control section, reduce the impact of water percentage fluctuation on rheological results, solved in the past in fibre-grade nylon 6 slice rheometer test process, easily there is degradation reaction in nylon 6, experimental result fluctuation is larger, the problem that experimental data repeatability is poor.
Embodiment
Below in conjunction with specific embodiment, further illustrate technical scheme of the present invention.
Embodiment 1:
1) fibre-grade nylon 6 slice is carried out to thermal pretreatment; Be specially: the section that takes constant weight is positioned in the weighing disk with ground, be then placed in vacuum drying oven dry, vacuum drying oven temperature is greater than the glass temperature of fibre-grade nylon 6 slice, and oven temperature is 115 ℃; In baking oven, be 17h standing time;
2) the fibre-grade nylon 6 slice after thermal pretreatment is put into vacuum drying, measure water percentage, water percentage is 220ppm;
3) by the rheological property of capillary rheometer determining fibre-grade nylon 6 slice melt, the melting time is 5min, repeated test three times;
4) calculate the shear viscosity of fibre-grade nylon 6 slice, resulting rheological data undulatory property is less, and better, standard deviation is 0.068 to repeatability.
Embodiment 2:
1) fibre-grade nylon 6 slice is carried out to thermal pretreatment; Be specially: the section that takes constant weight is positioned in the weighing disk with ground, be then placed in vacuum drying oven dry, vacuum drying oven temperature is greater than the glass temperature of fibre-grade nylon 6 slice, and oven temperature is 80 ℃; In baking oven, be 15h standing time;
2) the fibre-grade nylon 6 slice after thermal pretreatment is put into vacuum drying, measure water percentage, water percentage is 500ppm;
3) by the rheological property of capillary rheometer determining fibre-grade nylon 6 slice melt, the melting time is 5min, repeated test three times;
4) calculate the shear viscosity of fibre-grade nylon 6 slice, resulting rheological data undulatory property is larger, and repeatability is poor, and standard deviation is 12.478.
Embodiment 3:
1) fibre-grade nylon 6 slice is carried out to thermal pretreatment; Be specially: the section that takes constant weight is positioned in the weighing disk with ground, be then placed in vacuum drying oven dry, vacuum drying oven temperature is greater than the glass temperature of fibre-grade nylon 6 slice, and oven temperature is 115 ℃; In baking oven, be 15h standing time;
2) the fibre-grade nylon 6 slice after thermal pretreatment is put into vacuum drying, measure water percentage, water percentage is 229ppm;
3) by the rheological property of capillary rheometer determining fibre-grade nylon 6 slice melt, the melting time is 20min, repeated test three times;
4) calculate the shear viscosity of fibre-grade nylon 6 slice, resulting rheological data undulatory property is larger, and repeatability is poor, and standard deviation is 8.246.
Embodiment 4:
1) fibre-grade nylon 6 slice is carried out to thermal pretreatment; Be specially: the section that takes constant weight is positioned in the weighing disk with ground, be then placed in vacuum drying oven dry, vacuum drying oven temperature is greater than the glass temperature of fibre-grade nylon 6 slice, and oven temperature is 160 ℃; In baking oven, be 15h standing time;
2) the fibre-grade nylon 6 slice after thermal pretreatment is put into vacuum drying, measure water percentage, water percentage is 80ppm;
3) by the rheological property of capillary rheometer determining fibre-grade nylon 6 slice melt, the melting time is 5min, repeated test three times;
4) calculate the shear viscosity of fibre-grade nylon 6 slice, resulting rheological data undulatory property is larger, and repeatability is poor, and standard deviation is 4.246.
Above the present invention has been done to exemplary description; should be noted that; in the situation that not departing from core of the present invention, the replacement that is equal to that any simple distortion, modification or other those skilled in the art can not spend creative work all falls into protection scope of the present invention.
Claims (6)
1. a method of testing for fibre-grade nylon 6 slice rheological behaviour, is characterized in that, according to following step, carries out:
Step 1, carries out thermal pretreatment by fibre-grade nylon 6 slice;
Step 2, measures the fibre-grade nylon 6 slice water percentage after thermal pretreatment;
Step 3, by apparent shear rate and the apparent shear stress of capillary rheometer determining fibre-grade nylon 6 slice melt;
Step 4, proofreaies and correct and Bagely proofreaies and correct and to try to achieve the true shear rate of fibre-grade nylon 6 slice melt and true shear stress by Weissenberg-Rabinowitch;
Step 5, by the true shear viscosity η of following formula calculating fibre-grade nylon 6 slice melt,
Wherein:
η is true shear viscosity;
γ is true shear rate;
σ is true shear stress.
2. the method for testing of a kind of fibre-grade nylon 6 slice rheological behaviour according to claim 1, it is characterized in that, in described step (1), thermal pretreatment is that constant temp. heating is processed in vacuum drying oven, fibre-grade nylon 6 slice is placed in to the weighing disk with ground, and then being placed in constant-temperature vacuum baking oven thermal pretreatment, the temperature of constant-temperature vacuum baking oven is greater than the glass temperature of fibre-grade nylon 6 slice.
3. the method for testing of a kind of fibre-grade nylon 6 slice rheological behaviour according to claim 1, is characterized in that, in described step (1), for fibre-grade nylon 6 slice, oven temperature is 90-130 ℃, preferably 100-120 ℃; In baking oven, be 10-20h standing time, preferably 15-19h.
4. the method for testing of a kind of fibre-grade nylon 6 slice rheological behaviour according to claim 1, is characterized in that, by the pre-service of step (1), so that moisture control is at 200-300ppm.
5. the method for testing of a kind of fibre-grade nylon 6 slice rheological behaviour according to claim 1, it is characterized in that, in described step (2), the weighing disk that fills fibre-grade nylon 6 slice band ground is taken out from vacuum drying oven, be positioned in vacuum dryer, then measure its water percentage, use Chengdu Instruement Factory of manufacturer model: UGI-IC solid drimeter.
6. the method for testing of a kind of fibre-grade nylon 6 slice rheological behaviour according to claim 1, is characterized in that, in described step (3), in rheometer test process, the melting time is 3-6min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310395971.6A CN103543088A (en) | 2013-09-03 | 2013-09-03 | Test method for rheological property of fiber-grade nylon 6 slice melt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310395971.6A CN103543088A (en) | 2013-09-03 | 2013-09-03 | Test method for rheological property of fiber-grade nylon 6 slice melt |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103543088A true CN103543088A (en) | 2014-01-29 |
Family
ID=49966759
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310395971.6A Pending CN103543088A (en) | 2013-09-03 | 2013-09-03 | Test method for rheological property of fiber-grade nylon 6 slice melt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103543088A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1773245A (en) * | 2005-11-12 | 2006-05-17 | 大连理工大学 | On-line type polymer double-capillary extrusion rheometer |
-
2013
- 2013-09-03 CN CN201310395971.6A patent/CN103543088A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1773245A (en) * | 2005-11-12 | 2006-05-17 | 大连理工大学 | On-line type polymer double-capillary extrusion rheometer |
Non-Patent Citations (2)
| Title |
|---|
| D. J. DIJKSTRA AND W. F. ZOETELIEF: "IUPAC GUIDELINE FOR RHEOLOGICAL CHARACTERISATION OF POLYAMIDE MELTS", 《PROCEEDINGS OF THE POLYMER PROCESSING SOCIETY 24TH ANNUAL MEETING》, 19 June 2008 (2008-06-19) * |
| 吴其晔，巫静安: "《高分子材料流变学》", 31 December 2002, article "第六章 流变测量学", pages: 173-183 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US12000065B2 (en) | Method for preparing PET/PTT parallel complex filament with high self-crimpiness | |
| Xiao et al. | Smart water-saving irrigation system in precision agriculture based on wireless sensor network | |
| CN103255498B (en) | Method for preparing colored polyester fiber by coloring stock solution | |
| CN103837777B (en) | Electric power system electricity quality evaluation method and system | |
| CN103543088A (en) | Test method for rheological property of fiber-grade nylon 6 slice melt | |
| CN204065685U (en) | A kind of light digital relay protection tester time response verifying attachment | |
| CN203705930U (en) | PM 2.5 real-time monitor system based on Zigbee | |
| CN104819912B (en) | A kind of asphalt foaming determination method for parameter | |
| CN202334531U (en) | Plastic silica fiber converter and electric energy meter remote reading system | |
| CN107383846A (en) | Glass fiber reinforcement two-component pultrusion polyurethane material and its application in direct-drive permanent magnet synchronous aerogenerator magnet steel press strip | |
| CN103352262A (en) | Chemical fiber cross air blasting cooling device | |
| CN107651855A (en) | A kind of wear-resisting glass fibre and preparation method thereof | |
| CN204832377U (en) | Reactive power compensator specifications test system | |
| CN103471795A (en) | Method for highly accelerated life testing of mainboard | |
| CN111161811B (en) | Method for predicting crack resistance of aerated concrete | |
| CN104529149A (en) | FSU intelligent online spinning mode self-regulation system and method thereof | |
| CN202928714U (en) | Internal instant temperature measuring device for high temperature high pressure developed diamonds | |
| CN102680836B (en) | Intelligent terminal testing device with automatic metering function | |
| CN214881971U (en) | System for stably adjusting pH value of oil bath on viscose fibers | |
| CN104559805A (en) | Solar panel pouring sealant and processing process thereof | |
| CN204417635U (en) | A kind of sapphire growth lowering means | |
| CN201921838U (en) | Automatic SR (Scanning Radiometer) dotting jig | |
| CN108964131B (en) | Method and system for evaluating comprehensive performance of grid-connected operation of photovoltaic power station | |
| CN202485833U (en) | Multi-point temperature detection device for crosslinking cable current-carrying capacity test | |
| CN106625936A (en) | Novel timber waterproof modification liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140129 |