CN110437591A - A kind of optical cable high viscosity PBT material and preparation method thereof - Google Patents
A kind of optical cable high viscosity PBT material and preparation method thereof Download PDFInfo
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- C08K5/52—Phosphorus bound to oxygen only
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Abstract
The invention discloses a kind of optical cable high viscosity PBT material and preparation method thereof, the PBT material be by by a part of PBT resin by freezing after, it is stand-by to be ground to powdery；Gained powdery PBT and the auxiliary agent including chain extender are premixed again, add remaining not ground granular PBT, by heating melting, mixing reaction, the optical cable high viscosity PBT material is obtained to idle discharge gas, vacuum evacuation, extruding pelletization.Obtained PBT material inherent viscosity is in 1.3dL/g or more, and viscosity stability is good, it is possible to prevente effectively from the bulge phenomenon generated, and does not also have an adverse effect to performances such as its mechanical strengths in Loose tube production line.The method of preparation PBT material provided by the invention, raw material are easy to get, and process is simple, the equipment for not needing complex and expensive, double screw extruder can be completed, and is a kind of method of economic, efficient production optical cable high viscosity PBT material, is suitble to large-scale industrial production.
Description
Technical field
The invention belongs to polyester material fields, and in particular to a kind of optical cable high viscosity PBT material and its preparation side
Method.
Background technique
5G technology is just grown rapidly at present, and as the infrastructure in 5G epoch, optical cable will be played in development from now on and be closed
Key effect.The requirement of industry interior focusing cable Loose tube is also higher and higher, and general Loose tube is provided with the optical fiber of several and band,
It requires that Loose tube diameter is big, has stable aperture and hard and soft appropriate.
Optical cable, optical fiber are mainly PBT material with Loose tube at present, and the full name of PBT is polybutylene terephthalate (PBT), is had
Higher tensile strength and elongation at break are able to maintain stabilization under high temperature and wet environment, and excellent comprehensive performance makes
It obtains PBT resin and is widely used in various fields, especially optical cable, optical fiber loose tube, be protection optical cable in optical cable manufacturing procedure
The last layer can protect optical fiber from internal stress and outer side pressure influence, play the role of cladding, protection optical fiber.With
It is usually squeeze out with high viscosity PBT resin being processed into the PBT material of optical cable, the requirement to inherent viscosity is very high
(in 1.3dL/g or so), while also requiring varying less for viscosity.
General purpose grade PBT inherent viscosity is generally 0.7-1.1dL/g, to obtain high viscosity PBT, domestic main production method
It is solid-phase tack producing, i.e., the medium-viscosity PBT resin that inherent viscosity is 1.0-1.1dL/g is passed through and add suitable additive, warp
Mixed, thickening, cooling and dedusting are crossed, the programs such as feed bin, packed and transported is delivered to and obtains the high viscosity PBT resin of 1.2-1.3dL/g.
Entire production process needs to add different additives, can be divided into different specifications according to the difference of additive.According to existing
Knowhow, added additive are largely pulverulence, and blocking vacuum pump is easy in subsequent vacuum, causes equipment
Failure.In order to solve this problem, patent CN104109352A and CN104109354A, which is proposed, first prepares PBT functional agglomerate
Functional agglomerate and PBT resin are added in solid-phase tack producing device, to solve powder additive by method according to the ratio of 1:10
Problem.But the difficult point of this method is the master batch by 10% and is evenly mixed in PBT resin that common tack producing device can not
Reach uniform mixing.And this mode is batch process, differing greatly between batch, plant energy consumption is higher, yield
It is lower, it can not accomplish continuous production, in the application of downstream optical cable enterprise, the pultrude process of high speed optical cable can not be adapted to, held
Easily cause the disadvantages of optical cable bulge, pipe thickness are uneven, caliber is unstable, surface is not clean.
Patent CN107602835A proposes the mode using chemical chain extension, is viscosified online using double screw extruder
Reaction, reach continuous production and control product viscosity stability, while start can be by the various auxiliary agents one of needs
It rises and is added in system, avoid and first do the process that master batch is mixed even rear thickening after progress, simplify technique, improve production
The advantages that efficiency has equipment investment few, easy to operate, strong applicability, easy to spread, makes some progress.
However, the requirement with optical cable manufacturing enterprise to optical cable pultrusion speed is higher and higher, optical cable is wanted with PBT material
Ask also higher and higher, the method that above-mentioned patent is mentioned also is encountered by more and more challenges, and prepared material is unable to satisfy down
Tourist family more stringent requirement, is mainly reflected in the following: (1) during viscosifying PBT material, if needing to add
Dry kind of auxiliary agent, these auxiliary agents be all it is powdered, the fusing point of some auxiliary agents is also relatively low, will melt in the hopper oral area of charging
Change, to affect the accuracy of addition, eventually leads to that prepared PBT mass is uneven, and then the optical cable pine set prepared
Tube thickness, caliber are uneven, and some areas are easy to happen bulge phenomenon, cause to complain；(2) due to the ratio of the various auxiliary agents of addition
Example is all fewer, and to mix in the PBT resin of particle shape, and the specific surface area of PBT particle is smaller, and mixing is unable to reach
The effect of even dispersion, and then it is unable to reach the viscosity consistency of thickening particle.The high viscosity PBT resin produced in this way
Viscosity is not easy to control, color is partially yellow and strand is unstable degradable, is difficult to meet current optical cable industry to the quality of raw material
It is required that.
Deficiency that the present invention is faced in view of the above technology and market user provide the excelsior requirement of material
New resolving ideas and scheme adjusts existing process conditions and step using existing equipment, and preparation meets market and wants
It asks, stable uniform, solid colour optical cable pine PBT material.
Summary of the invention
Present invention aim to address the above method there are the problem of, a kind of high quality, viscosity stabilization, production process are provided
The optical cable PBT material of smooth bubble-free when highly controllable, extrusion molding surface.
To achieve the above object, the invention adopts the following technical scheme:
A kind of optical cable high viscosity PBT material, the raw material including following parts by weight: 100 parts of PBT base resins, 0.5-3 parts
Chain extender；It is obtained by the preparation method included the following steps:
1) after a part of PBT resin is by freezing, it is stand-by to be ground to powdery；
2) powdery PBT and the auxiliary agent including chain extender are premixed, adds remaining not ground PBT basic tree
Rouge by heating melting, mixing reaction, obtains the optical cable high viscosity PBT material to idle discharge gas, vacuum evacuation, extruding pelletization
Material.
The freezing, grinding can pass through method known in the field, such as liquid nitrogen frozen pulverizer, cryogenic temperature
It is -50 DEG C to -190 DEG C, cooling time 1-10 minutes；Preferably, cryogenic temperature is -90 DEG C to -130 DEG C, cooling time 1-3
Minute.The PBT of freezing is sent into pulverizer again, achievees the effect that sufficiently to crush by repeated stock grinding.
The inherent viscosity of the PBT base resin is 1.0-1.1dL/g, and original state is particle shape, regulates and controls grinder
Revolving speed and milling time adjust partial size, it is 100-500 μm of PBT powder, preferably 200-400 μ that sieving, which obtains D50, after grinding
The PBT powder of m.
The PBT resin by freeze grinding is 20-40 parts.
Inventor is it has been unexpectedly found that within the above range by the ratio of powdery PBT and partial size D50 control, obtain
PBT material consistency it is good, and then prepare optical cable loose tube thickness, uniform diameter, significantly improve general PBT material
Bulge phenomenon.If the PBT content for premix is very little, effectively and the auxiliary agents mixing such as chain extender PBT also just can not be unable to reach
The good effect of material consistency；And the PBT content for being used to premix is too many, and may generate shadow to the mechanical property of gained PBT
It rings.
There is no particular limitation for the chain extender, chain extender of this field conventionally used for pet reaction, general to use
The multiple copolymer of acrylate with high activity group, such as isocyanates, bisoxazoline class and di-epoxy compounds
At least one of class.The example that chain extender can be enumerated includes but is not limited to methyl diphenylene diisocyanate (MDI), 2,4- first
Phenylene diisocyanate (TDI), 2,6- toluene di-isocyanate(TDI), isophorone diisocyanate (IPDI).
Optionally, the auxiliary agent further includes 0.1-0.4 parts of antioxidant, 0.5-2.0 parts of end-capping reagent, 0.3-0.8 parts of profits
Lubrication prescription.Preferably, antioxidant is selected from tetrapentaerythritol ester (antioxidant 1010), triphosphite ester (irgasfos 168), double Ji Wusi
At least one of alcohol diphosphites (antioxidant 626)；And/or lubricant is selected from pentaerythritol stearate (PETS) and gathers
At least one of ethylene waxes；End-capping reagent is ethylenediamine.
The present invention uses single screw rod or double screw extruder, preferably double screw extruder, wherein to the spiral shell of empty exhaust section
Bar sufficiently allows bubble to overflow using large area shallow thread；The screw pitch of the large area shallow flight worm is 56mm-112mm；Vacuum
The vacuum degree of exhaust section be 100-500Pa, preferably 100-300Pa, using vacuum evacuation further removal lower-molecular substance and
Bubble.
Heretofore described vacuum degree refers both to " absolute vacuum degree ".
Due to the process of material melting extrusion in screw rod, it may occur that a small amount of degradation generates a small amount of lower-molecular substance,
To form bubble.If this part bubble cannot remove, can quality conformance to subsequent product PBT material and viscosity generate
Adverse effect, and then it is unable to get the PBT material of required excellent combination property.
The present invention also provides the purposes of above-mentioned PBT material, for manufacturing optical cable Loose tube.It is made using the present invention
PBT material is as optical cable Loose tube, including mechanical property, and the performance indexes of electric property is very excellent, especially
Bulge number significantly reduces.It is a kind of PBT material of the optical cable Loose tube of excellent combination property.
The present invention compared with the existing technology, achieves following advantageous effects:
One, for the present invention creatively by a part of PBT base resin after freeze grinding, being made as D50 partial size is 200-
400 μm of powdery, then pass through double-screw extruding pelletizing together with remaining PBT bulk material, obtain high viscosity PBT material, one
Cause property is excellent, and for optical cable, the Loose tube of optical fiber, not only mechanical property, electric property are excellent, but also bulge phenomenon greatly subtracts
It is few, it meets customer need.
Two, optical cable provided by the invention high viscosity PBT material only needs that a small amount of chain extender is added in preparation method,
It can produce to obtain inherent viscosity and effectively prevent chain extender since chain extender additional amount is few in 1.3dL/g or more PBT material
Dosage greatly caused by unstable product quality the problem of.
Three, it in twin screw extrusion, by the exhaust process to idle discharge gas and two stages of vacuum evacuation, will remain
Monomer, the abundant off the row of small molecule volatile matter are more advantageous to consistency of the PBT material for optical cable, optical fiber loose tube product.
Specific embodiment:
Optical cable high viscosity PBT material that the following examples are intended to illustrate the invention, but should not be construed as limiting the invention
Range.In the examples where no specific technique or condition is specified, described technology or conditions according to the literature in the art, or
It is carried out according to product description.Reagents or instruments used without specified manufacturer is that can be bought by regular distributor
The conventional products arrived.
Described " part " refers both to mass parts, the vacuum degree refers both to " absolute vacuum degree " if undeclared in embodiment.
Embodiment 1
Step 1: weigh 100 parts of PBT base resin, inherent viscosity 1.02dL/g, wherein 20 parts with liquid nitrogen by one
The resin of certainty ratio freezes 3min at -130 DEG C, and the resin under freezing state is worn into powdery PBT, partial size using grinder
D50 is about 400 μm；
Step 2: by powdery PBT and 1.2 parts of chain extender MDI, 0.2 part of antioxidant AT10,0.2 part of irgasfos 168,
0.3 part of lubricant PETS is mixed together；
Step 3: the mixture that step 2 is obtained is by pipeline to double screw extruder feed opening, with 80 parts of residue
PBT particle enters double screw extruder feeding inlet together；
Step 4: before double screw extruder is to empty exhaust section, 1.0 parts of end-capping reagent hexamethylene diamine is added and terminates reaction；
Sufficiently bubble is allowed to overflow with large area shallow thread again empty exhaust section in double screw extruder；In the vacuum of double screw extruder
Exhaust section removes low molecule and bubble with condition of high vacuum degree 100Pa again.
Step 5: the material strip of extrusion is cooling by step, is granulated, is dry, packaging, obtains final products.
Embodiment 2
Operating condition and step and embodiment 1 are identical, and difference is that the powdery PBT that freeze grinding obtains in step 1 is 30
Part, enter double screw extruder feeding inlet together with 70 parts of granular PBT of residue.
Embodiment 3
Operating condition and step and embodiment 1 are identical, and difference is that the powdery PBT that freeze grinding obtains in step 1 is 40
Part, enter double screw extruder feeding inlet together with 60 parts of granular PBT of residue.
Embodiment 4
Operating condition and step and embodiment 1 are identical, and difference is that the powdery PBT that freeze grinding obtains in step 1 is D50
About 300 μm.
Embodiment 5
Operating condition and step and embodiment 2 are identical, and difference is that the powdery PBT that freeze grinding obtains in step 1 is D50
About 300 μm.
Embodiment 6
Operating condition and step and embodiment 3 are identical, and difference is that the powdery PBT that freeze grinding obtains in step 1 is D50
About 300 μm.
Embodiment 7
Operating condition and step and embodiment 1 are identical, and difference is that the powdery PBT that freeze grinding obtains in step 1 is D50
About 200 μm.
Embodiment 8
Operating condition and step and embodiment 2 are identical, and difference is that the powdery PBT that freeze grinding obtains in step 1 is D50
About 200 μm.
Embodiment 9
Operating condition and step and embodiment 3 are identical, and difference is that the powdery PBT that freeze grinding obtains in step 1 is D50
About 200 μm.
Embodiment 10
Operating condition and step and embodiment 1 are identical, and difference is that the powdery PBT that freeze grinding obtains in step 1 is 10
Part, enter double screw extruder feeding inlet together with 90 parts of granular PBT of residue.
Embodiment 11
Operating condition and step and embodiment 1 are identical, and difference is that the powdery PBT that freeze grinding obtains in step 1 is 50
Part, enter double screw extruder feeding inlet together with 50 parts of granular PBT of residue.
Embodiment 12
Operating condition and step and embodiment 1 are identical, and difference is that the powdery PBT that freeze grinding obtains in step 1 is D50
About 100 μm.
Embodiment 13
Operating condition and step and embodiment 1 are identical, and difference is that the powdery PBT that freeze grinding obtains in step 1 is D50
About 500 μm.
Embodiment 14
Operating condition and step and embodiment 1 are identical, and difference is in step 1 to freeze 10min at -90 DEG C for resin,
The resin under freezing state is worn into powdery PBT using grinder, partial size D50 is about 400 μm.
Embodiment 15
Operating condition and step and embodiment 1 are identical, and difference is in step 1 to freeze 20min at -30 DEG C for resin,
The resin under freezing state is worn into powdery PBT using grinder, partial size D50 is about 400 μm；
Comparative example 1
The PBT material for commonly passing through solid-phase tack producing on the market is directlyed adopt, buying is full of luxuriant photoelectric material share from Suzhou
Co., Ltd, trade mark PBT-61008.
Comparative example 2
Step 1: the inherent viscosity for weighing 100 parts is 1.02dL/gPBT base resin, with 1.2 parts of chain extender MDI, 0.2
The antioxidant AT10,0.2 part of irgasfos 168,0.3 part of lubricant PETS of part mix 5min together, enter twin-screw together
Extruder feeding inlet；
Step 2: before double screw extruder is to empty exhaust section, 1.0 parts of end-capping reagent hexamethylene diamine is added and terminates reaction；
Sufficiently bubble is allowed to overflow with large area shallow thread again empty exhaust section in double screw extruder；In the vacuum of double screw extruder
Exhaust section removes low molecule and bubble with condition of high vacuum degree again.
Step 3: the material strip of extrusion is cooling by step, is granulated, is dry, packaging, obtains final products.
PBT base resin is other same as Example 1 without freeze grinding in the as embodiment 1 of comparative example 2.
Application examplesThe test of PBT material performance
Following performance indicator is tested to the PBT material that the embodiment of the present invention and comparative example obtain:
Inherent viscosity: inherent viscosity: being tested according to ISO1628 standard, is tested 15 batches of samples altogether, is averaged.
CPK (Complex Process Capability index) process capability index of inherent viscosity, refers to process
Actual processing ability in certain time, under state of a control.
CPK calculation formula bibliography (" calculating of process capability index CPK under state-of-art ", Jia Xinzhang etc.,
" Xian Electronics Science and Technology University's journal (natural science edition) ", the 4th phase of volume 28, the 452-455 pages):
CPK=(T/6 σ) * (1- | (X-U)/(T/2) |)
Wherein σ is the standard deviation of technological parameter distribution, and X is the average value of all sampled datas；T is tolerance, i.e. specification
The upper limit-lower specification limit；U is specification central value, i.e. (upper specification limit+lower specification limit)/2.
CPK value is bigger, indicates that quality is better, the rating scale of CPK is as shown in table 1 below:
Table 1
It is surveyed according to the method described above with performance of the standard to the obtained PBT material of the embodiment of the present invention and comparative example
Examination, as a result as shown in table 2 below:
Table 2
The test method of bulge number * is by PBT material made from embodiment and comparative example in optical cable loose tube production line
On with same technique 48 hours on probation, record bulge quantity.
PBT, which is made, in the present invention has high viscosity, and in 1.290dL/g or more, most of embodiment exists inherent viscosity
1.30dL/g or more can satisfy the demand of optical cable PBT material.
The product that embodiment 5 and comparative example 1, comparative example 2 are obtained, to be squeezed under same technique in Haake torque rheometer
Out, temperature setting be 235 DEG C, 245 DEG C, 270 DEG C, 260 DEG C of head temperature, revolving speed 60rpm.Its change in torque curve is recorded, such as
Shown in Fig. 1, as can be seen from the figure at high temperature, viscosity keeps stablizing the PBT material of embodiment 5, and torque maintains always one
A more stable numberical range, and the PBT material of comparative example 1 and comparative example 2, change in torque fluctuation is very big, especially compares
The PBT material change in torque of example 2 is very big, and it is very heavy to illustrate that the technique ground again after freezing has the consistency inside PBT material
The influence wanted.The PBT viscosity stability that comparative example is prepared is bad, is produced in PBT material processing and fabricating optical cable with Loose tube
Bulge phenomenon is easy to appear when line.According to the data and Fig. 1 of table 2, it can be seen that produced using high viscosity PBT produced by the invention
The viscosity stability of product is substantially better than the product of solid-phase tack producing and directly addition chain extender reaction thickening, most of embodiment characteristic
Inherent viscosity CPK reaches A+ rank to viscosity CPK all in A rank, preferred embodiment, and the PBT material characteristic that comparative example obtains
It is poor or even unacceptable that viscosity CPK value, which evaluates rank,.Illustrate that method provided by the invention can be effectively improved in PBT material
The consistency in portion has been obviously improved the stability of viscosity, so that when manufacturing optical cable loose tube, the phenomenon that bulge greatly reduces,
It meets in the market to such material more stringent requirement.
Meanwhile it can also be seen that the other performance of PBT material provided by the invention, such as mechanical strength, color by table 2
Pool, the performance in terms of electricity are not affected.
The above specific embodiment only schematically illustrates the content of present invention, does not represent the limitation of the content of present invention.
It may occur to persons skilled in the art that be that specific structure can have other versions in the present invention.
Claims (10)
1. a kind of optical cable high viscosity PBT material, the raw material including following parts by weight: 100 parts of PBT base resins, 0.5-3 parts
Chain extender；It is obtained by the preparation method included the following steps:
1) after a part of PBT resin is by freezing, it is stand-by to be ground to powdery；
2) powdery PBT and the auxiliary agent including chain extender are premixed, add remaining not ground PBT base resin,
By heating melting, mixing reaction, the optical cable high viscosity PBT material is obtained to idle discharge gas, vacuum evacuation, extruding pelletization.
2. optical cable as described in claim 1 high viscosity PBT material, which is characterized in that cryogenic temperature is -50 DEG C to -190 DEG C,
Cooling time 1-10 minutes；Preferably, cryogenic temperature is -90 DEG C to -130 DEG C, and cooling time is 1-3 minutes.
3. optical cable as described in claim 1 high viscosity PBT material, which is characterized in that the characteristic of the PBT base resin is viscous
Degree is 1.0-1.1dL/g, and original state is particle shape, is ground to the PBT powder that D50 is 100-500 μm, preferably 200-400 μ
m。
4. optical cable as described in claim 1 high viscosity PBT material, which is characterized in that the PBT resin by freeze grinding
It is 20-40 parts.
5. optical cable as described in claim 1 high viscosity PBT material, which is characterized in that the chain extender is with high activity base
The multiple copolymer of the acrylate of group；Preferably isocyanates, bisoxazoline class and di-epoxy compounds class.
6. optical cable as claimed in claim 5 high viscosity PBT material, which is characterized in that the chain extender is selected from diphenyl methane
Diisocyanate (MDI), 2,4 toluene diisocyanate (TDI), 2,6- toluene di-isocyanate(TDI), isophorone diisocyanate
At least one of (IPDI).
7. optical cable as described in claim 1 high viscosity PBT material, which is characterized in that the auxiliary agent further includes 0.1-0.4 parts
Antioxidant, 0.5-2.0 parts of end-capping reagent, 0.3-0.8 parts of lubricants.
8. optical cable as claimed in claim 7 high viscosity PBT material, which is characterized in that the antioxidant is selected from tetrapentaerythritol
Ester (antioxidant 1010), triphosphite ester (irgasfos 168), in dipentaerythritol diphosphites (antioxidant 626) at least
It is a kind of；And/or the lubricant is selected from least one of pentaerythritol stearate (PETS) and polyethylene wax；The sealing end
Agent is ethylenediamine.
9. optical cable as described in claim 1 high viscosity PBT material, which is characterized in that step (2) uses single screw rod or twin-screw
Extruder, preferably double screw extruder, wherein the screw rod to empty exhaust section uses large area shallow thread, the screw pitch of screw rod is
56mm-112mm；The vacuum degree for being vacuum-evacuated section is 100-500Pa, preferably 100-300Pa.
10. the purposes of any one of the right 1-9 PBT material, which is characterized in that for manufacturing optical cable Loose tube.
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| CN201910758361.5A CN110437591B (en) | 2019-08-16 | 2019-08-16 | High-viscosity PBT (polybutylene terephthalate) material for optical cable and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102558754A (en) * | 2011-12-23 | 2012-07-11 | 四川大学 | Chain-extended modified and copolymerized formaldehyde resin and preparation method thereof |
| CN107629420A (en) * | 2017-09-07 | 2018-01-26 | 滁州优胜高分子材料有限公司 | A kind of preparation method of PBT carbon fibers heat-conductive composite material |
| JP2018020535A (en) * | 2016-08-05 | 2018-02-08 | 三菱ケミカル株式会社 | Coextrusion non-stretched film for deep draw packaging, laminate film for freezing package and package using them |
-
2019
- 2019-08-16 CN CN201910758361.5A patent/CN110437591B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102558754A (en) * | 2011-12-23 | 2012-07-11 | 四川大学 | Chain-extended modified and copolymerized formaldehyde resin and preparation method thereof |
| JP2018020535A (en) * | 2016-08-05 | 2018-02-08 | 三菱ケミカル株式会社 | Coextrusion non-stretched film for deep draw packaging, laminate film for freezing package and package using them |
| CN107629420A (en) * | 2017-09-07 | 2018-01-26 | 滁州优胜高分子材料有限公司 | A kind of preparation method of PBT carbon fibers heat-conductive composite material |
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