CN1418902A - Solide phase polycondensation method for optical fibre secondary coated material-polybutylene telephalate - Google Patents
Solide phase polycondensation method for optical fibre secondary coated material-polybutylene telephalate Download PDFInfo
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- CN1418902A CN1418902A CN 02148419 CN02148419A CN1418902A CN 1418902 A CN1418902 A CN 1418902A CN 02148419 CN02148419 CN 02148419 CN 02148419 A CN02148419 A CN 02148419A CN 1418902 A CN1418902 A CN 1418902A
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- polybutylene terephthalate
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Abstract
The solid phase polycondensation method of optical-fibre secondary covering material-polytetramethylene terephthalate is characterized by that it adopts the lower-viscosity polytetramethylene terephthalate basic resin as base material, and adds 0.3-2% of monofunctional group or oxazoline end-capping agent as additive and makes them produce reaction to obtain the invented product in the solid phase polycondensation reactor, also can added 0.2-2% of fatty acid amide or fatty acid and lipoid metallic soap and hydrocarbon lubricating agent as additive or adding 0.1-2 % of lubricating agent as additive to prepare said invented product. Its reaction condition is moderate, its product quality is high and stable.
Description
Technical field:
The present invention relates to a kind of optical fiber secondary cocoon material---the solid phase polycondensation method of polybutylene terephthalate (hereinafter to be referred as PBT).Product is mainly as all kinds of optical fiber jacket material.Can be widely used in the secondary coated of each type optical fiber.
Background technology:
The secondary coated material of optical fiber---solid phase polycondensation polybutylene terephthalate is a thermoplastic engineering plastic of making fiber secondary coating (beam tube).Along with the continuous development of telecommunications, also increasing to the demand of optical cable, the corresponding with it consumption to this PBT is also in cumulative year after year.The optical cable new product emerges in an endless stream, from till now ADSS optical cable of initial central tubular optical cable, submarine optical fiber cable etc.The requirement of optical cable under varying environment also improved greatly.Thus the PBT material of wherein protecting optical fiber is also had higher requirement.We can say that fibre core is the most important parts in the optical cable,, select suitable optical fiber secondary cocoon material most important good optical cable for the optical fiber in the pipe is played a good protection.
Existing optical fiber secondary cocoon material---polybutylene terephthalate adopts usually and extrudes the tackify that the tackify technology realizes the PBT material by the reaction formula twin screw extruder.The reactive extruder tackify utilizes the reactive group of PBT material self such as the reaction between hydroxyl, carboxyl etc. and the chainextender by adding a certain amount of chainextender in process of production, by the chainextender molecule two PBT molecules is coupled together the realization tackify.The PBT material of producing by this technology is because it self unstable causes the certain limitation in the application.
Summary of the invention:
The object of the present invention is to provide a kind of optical fiber secondary cocoon material of excellent performance---the solid phase polycondensation method of polybutylene terephthalate.
Technology contents of the present invention is: the solid phase polycondensation method of a kind of optical fiber secondary cocoon material---polybutylene terephthalate, it is to adopt more low viscous polybutylene terephthalate base resin as base-material, and the adding single tube can roll into a ball or oxazole pouring type end-capping reagent is made additive, react in the solid state polycondensation device and make, the add-on of end-capping reagent accounts for the 0.3-2% of raw material gross weight.Best 0.3-0.6%.
The present invention also can add fatty acid acyl amine or lipid acid and lipid, metallic soap class in above-mentioned raw materials, the hydro carbons lubricant is made additive, and the add-on of lubricant accounts for the 0.2-2% of raw material gross weight.Best 0.2-1.0%.
The present invention also can add slipping agent and make additive in above-mentioned raw materials, the add-on of slipping agent accounts for raw material gross weight 0.1-2%.Best 0.1-0.5%.
Described simple function group type or oxazoline type end-capping reagent are ethanol or Virahol, phenol, 2, the two 2-oxazolines of 2-.Its mechanism is for reducing the content of carboxyl end group of PBT material.
Described fatty acid amide series lubricant agent is stearylamide or oleylamide, mustard acid amides; Lipid acid and lipid lubricant are stearic acid; The metallic soap series lubricant agent is calcium stearate, magnesium or zinc; The hydro carbons lubricant is polyethylene wax or Poly Propylene Wax, oxidized polyethlene wax.Mechanism is improved processibility, is improved output and extruded velocity for improving the flowability of PBT material.
Described slipping agent is talcum powder or white carbon black, barium sulfate.Its mechanism is for improving the non-stick property of PBT material.
The solid phase polycondensation polybutylene terephthalate is the polybutylene terephthalate base resin carries out polycondensation under solid state a method, it belongs to homogeneous reaction, temperature is controlled at below the poly-fusing point to the benzene butanediol fat, be reflected in the solid phase and carry out, and along with the increase speed of response of temperature also increases accordingly.This reaction is that substep is finished.When temperature of reaction was between monomer and polymer melt, the first step of polycondensation was carried out under the molten monomer state, then in the solid of oligopolymer further polycondensation become the polybutylene terephthalate finished product of viscosity higher.
Above-mentioned polycondensation heats first, second stage and first, second stage four-stage of cooling carries out.
Heating temperature 40-160 ℃ of the fs, 160 ± 5 ℃ of holding temperatures, soaking time 0.5～1.5 hour; Heating temperature 160-205 ℃ of subordinate phase, 205 ± 5 ℃ of holding temperatures, soaking time 5～15 hours; Cool off fs temperature 205-150 ℃, 150 ± 5 ℃ of holding temperatures, soaking time 0.5～1.5 hour; 150-100 ℃ of cooling subordinate phase temperature; Vacuum tightness≤0.1mbar.
The present invention utilizes this comparatively gentle reaction of solid phase polycondensation, by the viscosity of optimizing reaction process condition such as temperature of reaction, reaction time and vacuum tightness and selecting affine additive of suitable and PBT and adding technique to improve the PBT material.This material is processed easily and is had higher melt strength, lower thermal expansivity, lower post-shrinkage ratio and good dimensional stability, stable processing technology, shaping speed height, more excellent product purity, more excellent characteristics such as batch stability extruded.Shortened operational path, the performance of PBT material has been brought up to a new height, thereby reached the requirement of fiber secondary coating with material.
The present invention with extrude the tackify product performance and be compared as follows:
| Performance | Unit | This patent product | Extrude the tackify product |
| Fusing point (DSC) | ℃ | ?226 | ?226 |
| Melting index (MTI250/2.16KG) | Cm 3/10min | ?11.1 | ?8 |
| Coefficient of linear expansion (23-80 ℃) | 10 -4K -1 | ?0.81 | ?1.6 |
| Saturated water absorption | ％ | ?0.04 | ?0.45 |
| Tensile yield strength | Mpa | ?54 | ?52 |
| The elongation at yield rate | ％ | ?9 | ?7 |
| Elongation at break | ％ | ?352 | ?160 |
| Modulus in tension | Mpa | ?2258 | ?2070 |
| Stress in bending (3.5% strain) | Mpa | ?65.5 | ?61 |
| Modulus in flexure | Mpa | ?2255 | ?2220 |
| Notched Izod impact strength (23 ℃) | KJ/m 2 | ?5.9 | ?5.5 |
| Shore hardness HD | / | ?76.9 | ?70 |
Description of drawings:
Fig. 1 is technological process of production figure of the present invention.
Embodiment:
Embodiment 1: drop into polybutylene terephthalate resin 99.7kg as base-material in the solid state polycondensation device, and adding end-capping reagent ethanol 0.3kg carries out polycondensation as additive.Polycondensation heats first, second stage and first, second stage four-stage of cooling carries out.Heating temperature 40-160 ℃ of the fs, 160 ℃ of holding temperatures, soaking time 1 hour; Heating temperature 160-205 ℃ of subordinate phase, 205 ℃ of holding temperatures, soaking time 10 hours; Cool off fs temperature 205-150 ℃, 150 ℃ of holding temperatures, soaking time 1 hour; 150-100 ℃ of cooling subordinate phase temperature; Vacuum tightness≤0.1mbar.
Embodiment 2: drop into polybutylene terephthalate resin 99.55kg as base-material and add end-capping reagent Virahol 0.45kg and carry out polycondensation as additive in the solid state polycondensation device.All the other are with example 1.
Embodiment 3: drop into polybutylene terephthalate resin 99.4kg as base-material in the solid state polycondensation device, and adding end-capping reagent phenol 0.6kg carries out polycondensation as additive.All the other are with example 1.
Embodiment 4: drop into polybutylene terephthalate resin 99kg as base-material in the solid state polycondensation device, and add end-capping reagent 2, the two 2-oxazoline 1kg of 2-carry out polycondensation as additive.All the other are with example 1.
Embodiment 5: drop into polybutylene terephthalate resin 98.5kg as base-material in the solid state polycondensation device, and adding end-capping reagent ethanol 1.5kg carries out polycondensation as additive.All the other are with example 1.
Embodiment 6: drop into polybutylene terephthalate resin 98kg as base-material in the solid state polycondensation device, and adding end-capping reagent Virahol 2kg carries out polycondensation as additive.All the other are with example 1.
Embodiment 7: drop into polybutylene terephthalate resin 99.2kg as base-material in the solid state polycondensation device, and add end-capping reagent phenol 0.6kg, lubricant stearylamide 0.2kg and make additive, polycondensation heats first, second stage and first, second stage four-stage of cooling carries out.Heating temperature 40-160 ℃ of the fs, 155 ℃ of holding temperatures, soaking time 0.5 hour; Heating temperature 160-205 ℃ of subordinate phase, 210 ℃ of holding temperatures, soaking time 5 hours; Cool off fs temperature 205-150 ℃, 145 ℃ of holding temperatures, soaking time 1.5 hours; 150-100 ℃ of cooling subordinate phase temperature; Vacuum tightness≤0.1mbar.
Embodiment 8: drop into polybutylene terephthalate resin 98.7kg as base-material in the solid state polycondensation device, and add end-capping reagent 2,2-two 2-oxazoline 0.3kg, lubricant oils acid amides 1.0kg carry out polycondensation as additive.All the other are with example 7.
Embodiment 9: drop into polybutylene terephthalate resin 98.95kg as base-material in the solid state polycondensation device, and adding end-capping reagent ethanol 0.45kg, lubricant mustard acid amides 0.6kg carry out polycondensation as additive.All the other are with example 7.
Embodiment 10: drop into polybutylene terephthalate resin 98kg as base-material in the solid state polycondensation device, and adding end-capping reagent Virahol 1kg, lubricant stearic acid 1kg carry out polycondensation as additive.All the other are with example 7.
Embodiment 11: drop into polybutylene terephthalate resin 97.4kg as base-material in the solid state polycondensation device, and adding end-capping reagent phenol 0.6kg, lubricant stearic acid calcium 2kg carry out polycondensation as additive.All the other are with example 7.
Embodiment 12: drop into polybutylene terephthalate resin 98.2kg as base-material in the solid state polycondensation device, and add end-capping reagent 2,2-two 2-oxazoline 0.3kg, magnesium stearate lubricant 1.5kg carry out polycondensation as additive.All the other are with example 7.
Embodiment 13: drop into polybutylene terephthalate resin 98.9kg as base-material in the solid state polycondensation device, and add end-capping reagent ethanol 0.6kg, slipping agent talcum powder 0.5kg and make additive, polycondensation heats first, second stage and first, second stage four-stage of cooling carries out.Heating temperature 40-160 ℃ of the fs, 165 ℃ of holding temperatures, soaking time 1.5 hours; Heating temperature 160-205 ℃ of subordinate phase, 200 ℃ of holding temperatures, soaking time 5 hours; Cool off fs temperature 205-150 ℃, 155 ℃ of holding temperatures, soaking time 0.5 hour; 150-100 ℃ of cooling subordinate phase temperature; Vacuum tightness≤0.1mbar.
Embodiment 14: drop into polybutylene terephthalate resin 98.45kg as base-material in the solid state polycondensation device, and add end-capping reagent Virahol 0.45kg and slipping agent white carbon black 0.1kg carries out polycondensation as additive.All the other are with example 13.
Embodiment 15: drop into polybutylene terephthalate resin 98.7kg as base-material in the solid state polycondensation device, and add end-capping reagent phenol 1kg and slipping agent barium sulfate 0.3kg carries out polycondensation as additive.All the other are with example 13.
Embodiment 16: drop into polybutylene terephthalate resin 98.55kg as base-material in the solid state polycondensation device, and add end-capping reagent 2, two 2-oxazoline 0.45kg of 2-and slipping agent talcum powder 1kg carry out polycondensation as additive.All the other are with example 13.
Embodiment 17: drop into polybutylene terephthalate resin 97.7kg as base-material in the solid state polycondensation device, and add end-capping reagent ethanol 0.3kg and slipping agent white carbon black 2kg carries out polycondensation as additive.All the other are with example 13.
Embodiment 18: drop into polybutylene terephthalate resin 96.5kg as base-material in the solid state polycondensation device, and add end-capping reagent ethanol 2kg and slipping agent barium sulfate 1.5kg carries out polycondensation as additive.All the other are with example 13.
Embodiment 19: drop into polybutylene terephthalate resin 98.65kg as base-material in the solid state polycondensation device, and adding end-capping reagent Virahol 0.45kg, lubricant stearic acid zinc 0.6kg and slipping agent talcum powder 0.3kg makes additive, polycondensation heats first, second stage and first, second stage four-stage of cooling carries out.Heating temperature 40-160 ℃ of the fs, 160 ℃ of holding temperatures, soaking time 1 hour; Heating temperature 160-205 ℃ of subordinate phase, 200 ℃ of holding temperatures, soaking time 10 hours; Cool off fs temperature 205-150 ℃, 155 ℃ of holding temperatures, soaking time 1.5 hours; 150-100 ℃ of cooling subordinate phase temperature; Vacuum tightness≤0.1mbar.
Embodiment 20: drop into polybutylene terephthalate resin 98.2kg as base-material in the solid state polycondensation device, and add end-capping reagent phenol 0.3kg, lubricant polyethylene wax 1.0kg and slipping agent white carbon black 0.5kg carries out polycondensation as additive.All the other are with example 19.
Embodiment 21: drop into polybutylene terephthalate resin 99.1kg as base-material in the solid state polycondensation device, and adding end-capping reagent 2,2-two-2 oxazoline 0.6kg, lubricant Poly Propylene Wax 0.2kg and slipping agent barium sulfate 0.1kg carry out polycondensation as additive.All the other are with example 19.
Embodiment 22: drop into polybutylene terephthalate resin 95.5kg as base-material in the solid state polycondensation device, and add end-capping reagent ethanol 1kg, lubricant oxidation polyethylene wax 2kg and slipping agent talcum powder 1.5kg carries out polycondensation as additive.All the other are with example 19.
Embodiment 23: drop into polybutylene terephthalate resin 96kg as base-material in the solid state polycondensation device, and add end-capping reagent ethanol 1.5kg, lubricant stearylamide 1.5kg and slipping agent white carbon black 1kg carries out polycondensation as additive.All the other are with example 19.
Embodiment 24: drop into polybutylene terephthalate resin 94kg as base-material in the solid state polycondensation device, and add end-capping reagent Virahol 2kg, lubricant oils acid amides 2kg and slipping agent barium sulfate 2kg carries out polycondensation as additive.All the other are with example 19.
Claims (10)
1, a kind of solid phase polycondensation method of optical fiber secondary cocoon material-polybutylene terephthalate, it is characterized in that adopting more low viscous polybutylene terephthalate base resin as base-material, and the adding single tube can roll into a ball or oxazole pouring type end-capping reagent is made additive, react in the solid state polycondensation device and make, the add-on of end-capping reagent accounts for the 0.3-2% of raw material gross weight.
2, the solid phase polycondensation method of a kind of optical fiber secondary cocoon material-polybutylene terephthalate according to claim 1, it is characterized in that in the raw material also adding fatty acid acyl amine or lipid acid and lipid are arranged, metallic soap class, hydro carbons lubricant make additive, the add-on of lubricant accounts for the 0.2-2% of raw material gross weight.
3, the solid phase polycondensation method of a kind of optical fiber secondary cocoon material-polybutylene terephthalate according to claim 1 and 2 is characterized in that in the raw material also adding have slipping agent to make additive, and the add-on of slipping agent accounts for raw material gross weight 0.1-2%.
4, the solid phase polycondensation method of a kind of optical fiber secondary cocoon material-polybutylene terephthalate according to claim 1 is characterized in that simple function group type or oxazoline type end-capping reagent are ethanol or Virahol, phenol, 2, the two 2-oxazolines of 2-.
5, the solid phase polycondensation method of a kind of optical fiber secondary cocoon material-polybutylene terephthalate according to claim 2 is characterized in that lubricant is stearylamide or oleylamide, mustard acid amides, stearic acid, calcium stearate, magnesium, zinc, polyethylene wax or Poly Propylene Wax, oxidized polyethlene wax.
6, the solid phase polycondensation method of a kind of optical fiber secondary cocoon material-polybutylene terephthalate according to claim 3 is characterized in that slipping agent is talcum powder or white carbon black, barium sulfate.
7, the solid phase polycondensation method of a kind of optical fiber secondary cocoon material-polybutylene terephthalate according to claim 1 is characterized in that the end-capping reagent add-on accounts for the 0.3-0.6% of raw material gross weight.
8, the solid phase polycondensation method of a kind of optical fiber secondary cocoon material-polybutylene terephthalate according to claim 2 is characterized in that the lubricant add-on accounts for the 0.2-1.0% of raw material gross weight.
9, the solid phase polycondensation method of a kind of optical fiber secondary cocoon material-polybutylene terephthalate according to claim 3 is characterized in that the slipping agent add-on accounts for the 0.1-0.5% of raw material gross weight.
10, according to the solid phase polycondensation method of claim 1 or 2 one of them described a kind of optical fiber secondary cocoon material-polybutylene terephthalate, it is characterized in that reaction divides first and second stage of heating and four of first and second stages of cooling to carry out, heating temperature 40-160 ℃ of the fs, 160 ± 5 ℃ of holding temperatures, heating temperature 160-205 ℃ of subordinate phase, 205 ± 5 ℃ of holding temperatures; Cool off fs temperature 205-150 ℃, 150 ± 5 ℃ of holding temperatures; 150-100 ℃ of cooling subordinate phase temperature; Vacuum tightness≤0.1mbar.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB021484198A CN1176134C (en) | 2002-11-30 | 2002-11-30 | Solide phase polycondensation method for optical fibre secondary coated material-polybutylene telephalate |
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| CNB021484198A CN1176134C (en) | 2002-11-30 | 2002-11-30 | Solide phase polycondensation method for optical fibre secondary coated material-polybutylene telephalate |
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| CN1418902A true CN1418902A (en) | 2003-05-21 |
| CN1176134C CN1176134C (en) | 2004-11-17 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106220836A (en) * | 2016-08-30 | 2016-12-14 | 无锡市兴盛新材料科技有限公司 | A kind of preparation method of high viscosity resistance to thermal degradation PBT polyester |
| CN107418162A (en) * | 2017-07-21 | 2017-12-01 | 苏州盈茂光电材料股份有限公司 | A kind of modified PBT preparation method and products thereof and application |
| CN107417931A (en) * | 2017-07-21 | 2017-12-01 | 苏州盈茂光电材料股份有限公司 | A kind of modified PBT preparation technology and modified PBT and its application |
| CN111154240A (en) * | 2020-01-20 | 2020-05-15 | 湖北工业大学 | Modification method of high-performance and hydrolysis-resistant polybutylene terephthalate resin for optical cable sheath |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100349951C (en) * | 2005-11-04 | 2007-11-21 | 东华大学 | Solid phase polymerization process for preparing ethylene telephthalate and aromatic diamine copolymer |
-
2002
- 2002-11-30 CN CNB021484198A patent/CN1176134C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106220836A (en) * | 2016-08-30 | 2016-12-14 | 无锡市兴盛新材料科技有限公司 | A kind of preparation method of high viscosity resistance to thermal degradation PBT polyester |
| CN107418162A (en) * | 2017-07-21 | 2017-12-01 | 苏州盈茂光电材料股份有限公司 | A kind of modified PBT preparation method and products thereof and application |
| CN107417931A (en) * | 2017-07-21 | 2017-12-01 | 苏州盈茂光电材料股份有限公司 | A kind of modified PBT preparation technology and modified PBT and its application |
| CN111154240A (en) * | 2020-01-20 | 2020-05-15 | 湖北工业大学 | Modification method of high-performance and hydrolysis-resistant polybutylene terephthalate resin for optical cable sheath |
| CN111154240B (en) * | 2020-01-20 | 2022-02-01 | 湖北工业大学 | Modification method of high-performance and hydrolysis-resistant polybutylene terephthalate resin for optical cable sheath |
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