CN106700430B - Optical cable polybutylene terephthalate (PBT) production technology - Google Patents
Optical cable polybutylene terephthalate (PBT) production technology Download PDFInfo
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- CN106700430B CN106700430B CN201510442300.XA CN201510442300A CN106700430B CN 106700430 B CN106700430 B CN 106700430B CN 201510442300 A CN201510442300 A CN 201510442300A CN 106700430 B CN106700430 B CN 106700430B
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Abstract
The invention discloses a kind of optical cable polybutylene terephthalate (PBT) production technologies, its key points of the technical solution are that including step 1: PBT raw material and crystallizing agent being put into togerther stirring at normal temperature 10min~15min in blender, the mass percent of crystallizing agent is between 0.05% to 0.2%;Step 2: the mixture in step 1 is put into reaction kettle, and vacuum degree is -0.1MPa~-0.08MPa in reaction kettle, enters the heating period later, the heating period includes warm-up phase: temperature is between 170 DEG C~190 DEG C, between constant temperature 1h~2h in reaction kettle;The stage of reaction: temperature is between 190 DEG C~210 DEG C, between constant temperature 4h~8h in reaction kettle;The sizing stage: temperature is between 170 DEG C~190 DEG C, between constant temperature 1h~3h in reaction kettle;Achieve the effect that the modeling Guan Yuchang produced with the PBT master batch of this production technology output is small and processing modeling pipe is that tensile speed is high.
Description
Technical field
The present invention relates to a kind of PBT material processing technologys, more specifically, it relates to a kind of optical cable poly terephthalic acid
Butanediol ester production technology.
Background technique
PBT is the abbreviation of polybutylene terephthalate (PBT), has high-fire resistance, toughness, fatigue durability, self-lubricating, low
Coefficient of friction still keeps various physical properties (including electrical property), electrical insulating property in wet environment.
Due to medium-sized PBT its main feature is that molecular weight is small, inherent viscosity is low, and melt flow rate (MFR) is high, mechanical strength phase
To lower, therefore fiber optic ribbon cable cable cannot be directly used as.In recent years, with advances in technology, increase PBT's by some auxiliary agents
Viscosity and intensity improve its performance, can refer to the patent application No. is 201110099419.3.Qualified PBT material could be used
In the plastic sleeve of optical fiber, that is, PBT material is formed into modeling pipe sleeve and is set to outside optical fiber, there is centainly PBT material in factory in processing
Requirement, one be made as modeling pipe after remaining length, second is that processing modeling pipe when tensile speed.Remaining length has one after referring to modeling pipe molding
Fixed contraction, the excessive optical fiber moulded in pipe of shrinkage can be wavy, does not meet product requirement;Tensile speed refer to modeling pipe at
Type is the molding speed of energy per minute, and the tensile speed of processing modeling pipe is usually no more than 500m/min in the prior art, tight in this way
Production efficiency is constrained again.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide a kind of optical cable poly terephthalic acid fourth two
Alcohol ester production technology, tensile speed when the modeling Guan Yuchang produced with the PBT master batch of this production technology output is small and pipe is moulded in processing
It is high.
To achieve the above object, the present invention provides the following technical scheme that a kind of optical cable polybutylene terephthalate
Ester production technology, including
Step 1: being put into togerther stirring at normal temperature 10min~15min in blender for PBT raw material and crystallizing agent, crystallizing agent
Mass percent is between 0.05% to 0.2%;
Step 2: the mixture in step 1 is put into reaction kettle, in reaction kettle vacuum degree be -0.1MPa~-
0.08MPa, later into the heating period, the heating period includes
Warm-up phase: temperature is between 170 DEG C~190 DEG C, between constant temperature 1h~2h in reaction kettle;
The stage of reaction: temperature is between 190 DEG C~210 DEG C, between constant temperature 5h~9h in reaction kettle;
The sizing stage: temperature is between 170 DEG C~190 DEG C, between constant temperature 1h~3h in reaction kettle.
Preferably, the mixing time in step 1 is 13min.
Preferably, the mass percent of crystallizing agent is 0.1% in step 1.
Preferably, vacuum degree is -0.09MPa in reaction kettle in step 2.
Preferably, temperature is 180 DEG C in warm-up phase reaction kettle in step 2, constant temperature time 1.5h.
Preferably, temperature is 200 DEG C in stage of reaction reaction kettle in step 2, constant temperature time 7h.
Preferably, temperature in elementary reaction kettle of being formed in step 2 is 180 DEG C, constant temperature time 2h.
Preferably, crystallizing agent is magnesium sulfate crystal whisker.
Preferably, the revolving speed of blender is 80r/min~100r/min.
Preferably, the revolving speed of reaction kettle is 10r/min~20r/min.
By using above-mentioned technical proposal, first PBT raw material is sufficiently mixed with crystallizing agent, so that mixture is in step 2
It reacts more uniform, while first mixture is preheated in step 2, so that at the liveness of the molecule of crystallizing agent and PBT
In higher state, then reacted between 190 DEG C~210 DEG C so that molecule sufficiently polymerize with intermolecular, then again into
Enter to the sizing stage, so that the performance of completely reacted PBT material is stabilized, guarantees uniform the one of reaction kettle PBT material performance
It causes.
Specific embodiment
A kind of optical cable polybutylene terephthalate (PBT) production technology, including
Step 1: being put into togerther stirring at normal temperature 10min~15min in blender for PBT raw material and crystallizing agent, crystallizing agent
Mass percent is first to be sufficiently mixed PBT raw material with crystallizing agent, between 0.05% to 0.2% so that mixture is in step 2
It reacts more uniform;Step 2: the mixture in step 1 is put into reaction kettle, in reaction kettle vacuum degree be -0.1MPa~-
0.08MPa, later enter the heating period, the heating period includes warm-up phase: in reaction kettle temperature be 170 DEG C~190 DEG C between,
Between constant temperature 1h~2h;The stage of reaction: temperature is between 190 DEG C~210 DEG C, between constant temperature 5h~9h in reaction kettle;Sizing rank
Section: temperature is between 170 DEG C~190 DEG C, between constant temperature 1h~3h in reaction kettle;First mixture is preheated, so that crystallization
The liveness of the molecule of agent and PBT is in higher state, is then reacted between 190 DEG C~210 DEG C so that molecule with
Intermolecular abundant polymerization, then enters back into the sizing stage, so that the performance of completely reacted PBT material is stabilized, guarantees anti-
Answer the uniformity of kettle PBT material performance.It is cooled down after taking out finished product, can only be cooled to finished product temperature is 80 DEG C to 100
Between DEG C, it can be packed after being cooled to.
Embodiment one: the mixing time in step 1 is 10min;The mass percent of crystallizing agent is 0.05% in step 1;
Vacuum degree is -0.1MPa in reaction kettle in step 2;Temperature is 170 DEG C in warm-up phase reaction kettle in step 2, constant temperature time
1h;Temperature is 190 DEG C in stage of reaction reaction kettle in step 2, constant temperature time 5h;Sizing elementary reaction kettle medium temperature in step 2
Degree is 170 DEG C, constant temperature time 1h.The PBT master batch produced with process above is managed to process modeling, through detecting remaining a length of 0.131 ‰,
Highest tensile speed is 642m/min.Illustrate herein, the optical cable that one section or more master batch is produced can be intercepted when surveying remaining long, is measured
The length of pipe and the length of the inside optical fiber are moulded, the difference of the length of modeling pipe is subtracted with the length of optical fiber, is then divided by the length of optical fiber
Remaining length;It can be tested in actual production when surveying highest tensile speed, when being more than highest tensile speed when production, modeling pipe
Will appear the non-uniform situation of property, pipe is moulded in part can be relatively thin, or even be easily broken off, the above are one of test method,
Such mode can be used in the following examples, is not repeated here in embodiment below.
Embodiment two: the mixing time in step 1 is 12min;The mass percent of crystallizing agent is 0.07% in step 1;
Vacuum degree is -0.095MPa in reaction kettle in step 2;Temperature is 175 DEG C, when constant temperature in warm-up phase reaction kettle in step 2
Between 1.2h;Temperature is 195 DEG C in stage of reaction reaction kettle in step 2, constant temperature time 6h;Sizing elementary reaction kettle in step 2
Middle temperature is 175 DEG C, constant temperature time 1.5h.The PBT master batch produced with process above is managed to process modeling, is detected remaining a length of
0.084 ‰, highest tensile speed is 796m/min.
Embodiment three: the mixing time in step 1 is 13min;The mass percent of crystallizing agent is 0.1% in step 1;
Vacuum degree is -0.09MPa in reaction kettle in step 2;Temperature is 180 DEG C in warm-up phase reaction kettle in step 2, constant temperature time
1.5h;Temperature is 200 DEG C in stage of reaction reaction kettle in step 2, constant temperature time 7h;It is formed in elementary reaction kettle in step 2
Temperature is 180 DEG C, constant temperature time 2h.The PBT master batch produced with process above is managed to process modeling, is detected remaining a length of
0.051 ‰, highest tensile speed is 1021m/min.
Example IV: the mixing time in step 1 is 14min;The mass percent of crystallizing agent is 0.17% in step 1;
Vacuum degree is -0.085MPa in reaction kettle in step 2;Temperature is 185 DEG C, when constant temperature in warm-up phase reaction kettle in step 2
Between 1.7h;Temperature is 205 DEG C in stage of reaction reaction kettle in step 2, constant temperature time 8h;Sizing elementary reaction kettle in step 2
Middle temperature is 185 DEG C, constant temperature time 2.5h.The PBT master batch produced with process above is managed to process modeling, is detected remaining a length of
0.072 ‰, highest tensile speed is 803m/min.
Embodiment five: the mixing time in step 1 is 15min;The mass percent of crystallizing agent is 0.2% in step 1;
Vacuum degree is -0.2MPa in reaction kettle in step 2;Temperature is 190 DEG C in warm-up phase reaction kettle in step 2, constant temperature time
2h;Temperature is 210 DEG C in stage of reaction reaction kettle in step 2, constant temperature time 9h;Sizing elementary reaction kettle medium temperature in step 2
Degree is 190 DEG C, constant temperature time 3h.The PBT master batch produced with process above is managed to process modeling, through detecting remaining a length of 0.101 ‰,
Highest tensile speed is 721m/min.
Integrated embodiment one is to embodiment five, reference can be made to following table:
In the case that other conditions are all the same, using the remaining length of the PBT master batch of technique output in different embodiments and most
Big tensile speed is as follows:
Embodiment one | Embodiment two | Embodiment three | Example IV | Embodiment five | |
Remaining length/‰ | 0.131 | 0.084 | 0.051 | 0.072 | 0.101 |
Tensile speed m/min | 642 | 796 | 1021 | 803 | 721 |
In conclusion can be more preferred using the process of embodiment three.
Crystallizing agent is magnesium sulfate crystal whisker, and magnesium sulfate crystal whisker is current material, can be network address http: //
It is previously mentioned in www.doc88.com/p-694270676268.html, material property can be improved and facilitates crystallization, this is
The prior art, therefore not in this to go forth.
The revolving speed of blender is 80r/min~100r/min, can be preferably 90r/min, not by the revolving speed of blender
Can be too fast, the phase mutual friction aggravation between too fast PBT and crystallizing agent generates biggish heat, influences whether the property of the two, turns
Fast excessively slow, the working efficiency that will affect, being also easy, which overturns PBT and crystallizing agent, is uniformly mixed.
The revolving speed of reaction kettle is 10r/min~20r/min, can be preferably 15r/min, when revolving speed is too fast, reaction kettle
Middle material overturning is too fast, reacts not uniform enough, and when revolving speed is excessively slow, material stops for a long time, so that partial material reaction is not filled
Point, but when revolving speed more than selecting, material reaction more full and uniform.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of optical cable polybutylene terephthalate (PBT) production technology, it is characterised in that: including
Step 1: PBT raw material and crystallizing agent are put into togerther stirring at normal temperature 10min~15min in blender, the quality of crystallizing agent
Percentage is between 0.05% to 0.2%, and the crystallizing agent is magnesium sulfate crystal whisker;
Step 2: the mixture in step 1 is put into reaction kettle, and vacuum degree is -0.1MPa~-0.08MPa in reaction kettle,
Later into the heating period, the heating period includes
Warm-up phase: temperature is between 170 DEG C~190 DEG C, between constant temperature 1h~2h in reaction kettle;
The stage of reaction: temperature is between 190 DEG C~210 DEG C, between constant temperature 5h~9h in reaction kettle;
The sizing stage: temperature is between 170 DEG C~190 DEG C, between constant temperature 1h~3h in reaction kettle.
2. optical cable according to claim 1 polybutylene terephthalate (PBT) production technology, it is characterised in that: the step
Mixing time in rapid one is 13min.
3. optical cable according to claim 1 polybutylene terephthalate (PBT) production technology, it is characterised in that: the step
The mass percent of crystallizing agent is 0.1% in rapid one.
4. optical cable according to claim 1 polybutylene terephthalate (PBT) production technology, it is characterised in that: the step
Vacuum degree is -0.09MPa in reaction kettle in rapid two.
5. optical cable according to claim 1 polybutylene terephthalate (PBT) production technology, it is characterised in that: the step
Temperature is 180 DEG C in warm-up phase reaction kettle in rapid two, constant temperature time 1.5h.
6. optical cable according to claim 1 polybutylene terephthalate (PBT) production technology, it is characterised in that: the step
Temperature is 200 DEG C in stage of reaction reaction kettle in rapid two, constant temperature time 7h.
7. optical cable according to claim 1 polybutylene terephthalate (PBT) production technology, it is characterised in that: the step
Temperature in elementary reaction kettle of being formed in rapid two is 180 DEG C, constant temperature time 2h.
8. optical cable according to claim 1 polybutylene terephthalate (PBT) production technology, it is characterised in that: described to stir
The revolving speed for mixing machine is 80r/min~100r/min.
9. optical cable according to claim 1 polybutylene terephthalate (PBT) production technology, it is characterised in that: described anti-
The revolving speed for answering kettle is 10r/min~20r/min.
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1152716A (en) * | 1994-11-24 | 1997-06-25 | 汎塑料株式会社 | Optical fiber covering tube |
CN1332201A (en) * | 2000-06-22 | 2002-01-23 | 帝人株式会社 | Resin composition for optical fiber loose concentrated pipe and optical fiber loose concentrated pipe |
CN1194855C (en) * | 2002-12-31 | 2005-03-30 | 冯晓旭 | Method for producing high viscosity polyethylene glycol terephthalate sheet by multiple one-way stretching |
CN102888084A (en) * | 2012-04-19 | 2013-01-23 | 上海德鸿高新材料有限公司 | Secondary coating material polybutylene terephthalate (PBT) composite for optical fiber and preparation method for secondary coating material PBT composite |
CN103525045A (en) * | 2013-04-15 | 2014-01-22 | 扬州金森光电材料有限公司 | Processing technology of PBT (Polybutylene Terephthalate) blue color masterbatch |
CN103668679A (en) * | 2013-12-18 | 2014-03-26 | 浙江铭龙基布有限公司 | Method for manufacturing base cloth in pool cloth |
CN104109351A (en) * | 2013-04-18 | 2014-10-22 | 扬州金森光电材料有限公司 | Manufacturing technology of PBT used for loose tube of optical cable |
-
2015
- 2015-07-24 CN CN201510442300.XA patent/CN106700430B/en active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1152716A (en) * | 1994-11-24 | 1997-06-25 | 汎塑料株式会社 | Optical fiber covering tube |
CN1332201A (en) * | 2000-06-22 | 2002-01-23 | 帝人株式会社 | Resin composition for optical fiber loose concentrated pipe and optical fiber loose concentrated pipe |
CN1194855C (en) * | 2002-12-31 | 2005-03-30 | 冯晓旭 | Method for producing high viscosity polyethylene glycol terephthalate sheet by multiple one-way stretching |
CN102888084A (en) * | 2012-04-19 | 2013-01-23 | 上海德鸿高新材料有限公司 | Secondary coating material polybutylene terephthalate (PBT) composite for optical fiber and preparation method for secondary coating material PBT composite |
CN103525045A (en) * | 2013-04-15 | 2014-01-22 | 扬州金森光电材料有限公司 | Processing technology of PBT (Polybutylene Terephthalate) blue color masterbatch |
CN104109351A (en) * | 2013-04-18 | 2014-10-22 | 扬州金森光电材料有限公司 | Manufacturing technology of PBT used for loose tube of optical cable |
CN103668679A (en) * | 2013-12-18 | 2014-03-26 | 浙江铭龙基布有限公司 | Method for manufacturing base cloth in pool cloth |
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