CN1814866A - Method for preparing polyamide 66 fiber - Google Patents
Method for preparing polyamide 66 fiber Download PDFInfo
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- CN1814866A CN1814866A CN 200510023771 CN200510023771A CN1814866A CN 1814866 A CN1814866 A CN 1814866A CN 200510023771 CN200510023771 CN 200510023771 CN 200510023771 A CN200510023771 A CN 200510023771A CN 1814866 A CN1814866 A CN 1814866A
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Abstract
This invention relates to a preparation method for PA 66 fibers including its preparation and filature, in which, the inventer optimizes the spinning process and technological conditions to prepare the PA 66 fiber of good performance meeting the needs of special fields, such as parachutes used in space flight and aviation and lifesaving rafts.
Description
Technical field
The present invention relates to a kind of polyamide 66 fiber preparation method.
Background technology
Polyamide fiber is also referred to as nylon fiber, is a kind of high strength, the fabulous material of anti-wear performance, is widely used in various fields.But, adopting the conventional at present prepared polyamide 66 fiber of method, its performance still can not satisfy the requirement of some special dimensions, and the needs of the lining of the parachute of using as space flight, aviation, the material of life raft are demanded urgently improving.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of polyamide 66 fiber preparation method, to overcome the defective that prior art exists, satisfy the needs of relevant field development.
Polyamide 66 fiber preparation method of the present invention comprises the steps:
(1) preparation of polyamide 66:
Nylon " 66 " salt and acetic acid are made molecular weight regulator reacted 20～40 minutes under the pressure of 210～265 ℃ of temperature and 1.75～1.85MPa, the pH value of reaction system is 7.9～7.95, obtains polyamide melt; Under vacuum condition, carry out aftercondensated then, vacuum is 0.035～0.045MPa (gauge pressure), temperature is 270～280 ℃, and preferred 272～276 ℃, temperature is too high, to cause producing gel and thermal decomposition, molecular weight is done not high, and the aftercondensated time is 30～60 minutes, and polymerization time is oversize, be easy to generate gel, to fiber quality with to stretch oneself and yawn performance all influential;
The ratio of nylon " 66 " salt and acetic acid is:
600 kilograms of acetic acid add 30～50ml acetic acid;
The pH of system is 7.9～7.95, can adopt hexamethylene diamine or adipic acid to regulate;
The inventor thinks, in the preparation process of polyamide 66, the mol ratio of temperature, pH and adipic acid, hexamethylene diamine is the key factor that influences fibre property, must strict control, the especially vacuum of aftercondensated, be formed with directly with moisture content, amine end groups number, carboxyl end group number and gel in the product and get in touch, to influence melt viscosity and ropiness energy, simultaneously, the proportioning raw materials of reaction system also is crucial
(2) with spinning on spinning machine behind the polymer melt of step (1), reel then, stretch oneself and yawn, twist, and adopt conventional method qualitative, promptly obtain product;
The preferred West Germany Ka Erfeilin of said spinning machine, the trade mark is the spinning machine of KF, the spinneret of this spinning machine is provided with gradually device for cooling, so that the tensile stress of the extrusion temperature of controlling fiber and coiling;
The inventor finds that under the situation that polymer is determined, the process conditions of spinning are very big to the performance impact of fiber, for this reason, the inventor optimizes the process conditions of spinning by a large amount of experiments, determined the process conditions that the polymer of employing step (1) carries out spinning, specific as follows:
Gradually cold temperature is 100～200 ℃, this temperature is than conventional temperature height, make from the polymer melt thread temperature on every side of spinning head ejection and raise, freezing point moves down, the construction unit of the fiber of nascent state is strengthened at the deorientation of elasticity to the plastically deforming area, the axial velocity gradient reduces and causes orientation to reduce, the birefringence of fiber increases, thereby owing property that can stable fibers and other inherent qualities, under the constant situation of other conditions, gradually cold temperature is as follows to owing property and other Effect on Performance of fiber:
| Fiber dimensious | Performance project | 50℃ | 100℃ | 150℃ | 200℃ |
| 33.3dtex | Powerful CN/dtex | 6.1 | 6.3 | 6.5 | 6.4 |
| Elongation % | 14.7 | 18.0 | 18.5 | 18.1 | |
| End breakage rate % | 11.2 | 8.7 | 7.8 | 9.0 |
For this reason, determine that gradually cold temperature is 100～200 ℃;
After the molten mass of polymer sprays from spinning head, cooling forming is the key issue that becomes fine, to the fiber number of fiber, dyeability stretch and the uniformity of elongation all influential, molten mass is 207～285 ℃ from the temperature of shower nozzle ejection, when reaching first draw-off godet, its temperature is dropped to below the sticking temperature, preferably reach solidification point, but, this cooling procedure should fully take into account cooling velocity and the mode uniformity to the permutation degree of the molecule of the cortex of fiber and sandwich layer, the present invention adopts air cooling, and leeway is 0.1～0.2mmH
2O, wind speed are 0.30～0.40 meter per second, under this condition, can guarantee the uniformity of fiber cooling forming and the birefringence of fiber;
Stretching ratio also is an important parameters, and one-level stretching ratio of the present invention is 1.2～1.6, and total stretching ratio is 4.6～5.0;
Stretching wire vent speed is also influential to the machinability of fiber, and stretching wire vent speed of the present invention is 300～400 meter per seconds;
Draft temperature heat dish is 65～85 ℃, and hot plate is 160～180 ℃.
Adopt the polyamide 66 fiber of above-mentioned method preparation, function admirable adopts the performance of the lining of this fiber production, can satisfy special dimension fully, the needs of the lining of the parachute of using as space flight, aviation, the material of life raft.
The specific embodiment
Embodiment 1
(1) preparation of polyamide 66:
600 kilograms of nylon " 66 " salt and 30ml acetic acid were reacted 40 minutes under the pressure of 210 ℃ of temperature and 1.75MPa, and the pH value of reaction system is 7.93, obtains polyamide prepolymer polycondensation melt; Carry out aftercondensated then under vacuum condition, obtain polyamide 66, vacuum is 0.045MPa (gauge pressure), and temperature is 276 ℃, and the aftercondensated time is 45 minutes;
The pH of system adopts hexamethylene diamine to regulate;
(2) spinning machine is West Germany Ka Erfeilin, and the trade mark is KF, and gradually cold temperature is 150 ℃, adopts air cooling, and leeway is 0.1mmH
2O, wind speed are 0.30 meter per second, and the one-level stretching ratio is 1.2, and total stretching ratio is 4.8, and stretching wire vent speed is 350 meter per seconds, and draft temperature is 65 ℃.
Adopt " People's Republic of China's textile industry standard---extraordinary industrial POLYAMIDE YARNS " (FZ66001---1995) standard that above-mentioned fiber is detected, the result is as follows:
150 ℃ of kind project/temperature
33.3dtex powerful CN/dtex 6.5
Elongation % 18.5
End breakage rate thousand ingots/time 7.8
Embodiment 2
(1) preparation of polyamide 66:
600 kilograms of nylon " 66 " salt and 50ml acetic acid were reacted 40 minutes under the pressure of 265 ℃ of temperature and 1.8MPa, and the pH value of reaction system is 7.93, obtains polyamide prepolymer polycondensation melt; Carry out aftercondensated then under vacuum condition, obtain polyamide 66, vacuum is 0.04MPa (gauge pressure), and temperature is 276 ℃, and the aftercondensated time is 45 minutes;
The pH of system can adopt adipic acid to regulate;
(2) spinning machine is West Germany Ka Erfeilin, and the trade mark is KF, and gradually cold temperature is 200 ℃, adopts air cooling, and leeway is 0.2mmH
2O, wind speed are 0.30 meter per second, and the one-level stretching ratio is 1.2, and total stretching ratio is 4.8, and stretching wire vent speed is 350 meter per seconds, and draft temperature is 65 ℃.
Adopt " People's Republic of China's textile industry standard---extraordinary industrial POLYAMIDE YARNS " (FZ66001---1995) standard that above-mentioned fiber is detected, the result is as follows:
200 ℃ of kind project/temperature
33.3dtex powerful CN/dtex 6.4
Elongation % 18.1
End breakage rate thousand ingots/time 9.0.
Claims (10)
1. a polyamide 66 fiber preparation method is characterized in that, comprises the steps:
(1) preparation of polyamide 66:
Nylon " 66 " salt is done to react 20～40 minutes under the pressure of molecular weight regulator at 1.75～1.85MPa 210～265 ℃ of temperature with acetic acid, the pH value of reaction system is 7.9～7.95, under vacuum condition, carry out aftercondensated then, obtain polyamide 66, vacuum is gauge pressure 0.035～0.045MPa, temperature is 270～280 ℃, and the aftercondensated time is 30～60 minutes;
(2) with spinning on spinning machine behind the polymer melt of step (1), reel then, stretch oneself and yawn, twist, and adopt conventional method typing, promptly obtain product.
2. method according to claim 1 is characterized in that, the aftercondensated temperature is 272～276 ℃.
3. according to the described method of claim 1, it is characterized in that the pH of system adopts hexamethylene diamine or adipic acid to regulate.
4. according to the described method of claim 1, it is characterized in that, adopt spinneret to be provided with the gradually spinning machine of device for cooling.
5. according to the described method of claim 4, its feature exists, and gradually cold temperature is 100～200 ℃.
6. according to the described method of claim 5, its feature exists, and adopting the leeway of air cooling is 0.1～0.2mmH2O, and wind speed is 0.30～0.40 meter per second.
7. according to the described method of claim 6, its feature exists, and the one-level stretching ratio is 1.2～1.6, and total stretching ratio is 4.6～5.0.
8. according to the described method of claim 7, it is characterized in that stretching wire vent speed is 300～400 meter per seconds.
9. according to the described method of claim 8, it is characterized in that draft temperature is 65～85 ℃.
10. according to the described method of claim 9, it is characterized in that the ratio of nylon " 66 " salt and acetic acid is: 600 kilograms of acetic acid add 30～50ml acetic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510023771 CN1814866A (en) | 2005-02-02 | 2005-02-02 | Method for preparing polyamide 66 fiber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510023771 CN1814866A (en) | 2005-02-02 | 2005-02-02 | Method for preparing polyamide 66 fiber |
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| CN1814866A true CN1814866A (en) | 2006-08-09 |
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| CN 200510023771 Pending CN1814866A (en) | 2005-02-02 | 2005-02-02 | Method for preparing polyamide 66 fiber |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104160074A (en) * | 2012-02-29 | 2014-11-19 | 东丽株式会社 | Polyamide fiber and method for producing same |
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2005
- 2005-02-02 CN CN 200510023771 patent/CN1814866A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104160074A (en) * | 2012-02-29 | 2014-11-19 | 东丽株式会社 | Polyamide fiber and method for producing same |
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