CN108822234A - A kind of preparation facilities and method of low-loss plastic optical fiber - Google Patents
A kind of preparation facilities and method of low-loss plastic optical fiber Download PDFInfo
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- CN108822234A CN108822234A CN201810601247.7A CN201810601247A CN108822234A CN 108822234 A CN108822234 A CN 108822234A CN 201810601247 A CN201810601247 A CN 201810601247A CN 108822234 A CN108822234 A CN 108822234A
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- extraction
- pipe
- condenser
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- extraction flask
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/001—Removal of residual monomers by physical means
- C08F6/005—Removal of residual monomers by physical means from solid polymers
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Optical Fibers, Optical Fiber Cores, And Optical Fiber Bundles (AREA)
Abstract
The present invention provides the preparation facilities and method of a kind of low-loss plastic fiber optic materials, this method includes at reduced pressure conditions by the extracting solution heating and gasifying in extraction flask, the extracting solution of gasification enters PMMA after condensing in condenser pipe, extract PMMA, leaching liquor is back to extraction flask by siphon pipe, such circulating reflux obtains the low-loss plastic fiber optic materials.The present invention realizes the small molecule simply and quickly removed in PMMA, and the PMMA of macromolecule, is effectively reduced the transmission loss of optical fiber in reservation.
Description
Technical field
The present invention relates to plastic optical fiber technical fields, more particularly to a kind of preparation facilities of low-loss plastic fiber optic materials
And method.
Background technique
PMMA (polymethyl methacrylate) is a kind of optical material with high transmittance, is widely used in illuminating equipment,
The fields such as optical fiber.PMMA generally uses free radical polymerization to prepare, and molecular weight distribution is wider, is unfavorable for optical property
, for the especially PMMA of small-molecular-weight under the irradiation of feux rouges, PMMA has stronger C-H absorption of vibrations, causes a large amount of damages of light
Consumption, still, still further aspect is unfavorable for processing if PMMA molecular weight is narrow, causes much to adversely affect to molding of towing.
So studying, one kind is simple, efficiently method removes the small molecule in PMMA, the PMMA of macromolecule in reservation,
Have great importance for preparation low-loss plastic optical fiber.
Summary of the invention
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of low-loss plastic fiber optic materials
Preparation facilities and method, for solving the problems such as small molecule content in existing PMMA is high, transmission loss of optical fiber is big.
In order to achieve the above objects and other related objects, the present invention provides a kind of preparation side of low-loss plastic fiber optic materials
Method, including by the extracting solution heating and gasifying in extraction flask, the extracting solution of gasification enters condensation by bypass pipe at reduced pressure conditions
Pipe enters extraction tube after condensing in condenser pipe, extracts PMMA, and leaching liquor is back to extraction flask by siphon pipe, so recycles
Reflux, obtains the low-loss plastic fiber optic materials.
In some embodiments of the invention, extraction processing is carried out using Soxhlet extractor, the Soxhlet extractor it is cold
Solidifying pipe is communicated with decompressor.
In some embodiments of the invention, the extracting solution includes tetrahydrofuran and acetic acid.
In some embodiments of the invention, the volume ratio of tetrahydrofuran and acetic acid is 1 in the extracting solution:(40~
60)。
In some embodiments of the invention, the volume ratio of tetrahydrofuran and acetic acid is 1 in the extracting solution:50.
In some embodiments of the invention, when under reduced pressure by the extracting solution heating and gasifying in extraction flask, vacuum degree
For 0.6-0.8bar.
In some embodiments of the invention, circulation time 1.5-2.5h, preferably 2h.
Second aspect of the present invention provides low-loss plastic fiber optic materials made from the above method.
Third aspect present invention provides a kind of device for being used to prepare low-loss plastic fiber optic materials, including extraction flask, mentions
Take pipe, condenser, decompressor, the extraction flask is connected to the condenser by the extraction tube, the condenser it is cold
Solidifying pipe is connected to the decompressor, and the extraction flask is connected to the extraction tube by bypass pipe, and the extraction tube is communicated with
Shunt valve upward, the shunt valve is interior to be equipped with the siphon pipe for being connected to the extraction flask, the liquid gasification in the extraction flask
The condenser pipe is entered by the bypass pipe afterwards, gas flows into the extraction tube, the extraction after the condensing tube condensation
Liquid in pipe is successively back to the extraction flask by the shunt valve, siphon pipe.
In some embodiments of the invention, the decompressor includes vacuum pump, for taking out to space in device
It is vacuum-treated.
It in some embodiments of the invention, further include vacuum governor for vacuum of space in regulating device, institute
It states on the pipeline that vacuum governor is mounted between the condenser and the vacuum pump.
In some embodiments of the invention, pressure is also equipped on the pipeline between the condenser and the vacuum pump
Table, the vacuum degree for space in real-time displaying device.
In some embodiments of the invention, the top of the siphon pipe is equipped with inlet, the upper connection of the bypass pipe
Mouth is higher than the inlet of the siphon pipe or flushes with the inlet of the siphon pipe, and the top of the shunt valve is equipped with opening,
The top of horizontal plane where the opening is located at the inlet.
As described above, the preparation facilities and method of a kind of low-loss plastic fiber optic materials of the invention, have beneficial below
Effect：The present invention realizes the small molecule simply and quickly removed in PMMA, and the PMMA of macromolecule, is effectively reduced light in reservation
Fine transmission loss.
Detailed description of the invention
Fig. 1 is shown as the apparatus structure schematic diagram that the embodiment of the present invention is used to prepare low-loss plastic fiber optic materials.
Piece mark explanation
1-extraction flask
2-extraction tubes
21-siphon pipes
22-bypass pipes
23-shunt valves
3-condensers
4-vacuum governors
5-vacuum pumps
6-pressure gauges
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
It should be clear that in the following example not specifically dated process equipment or device be all made of conventional equipment in the art or
Device；All pressure values and range all refer to absolute pressure.
In addition, it should also be understood that, one or more method and step mentioned in the present invention does not repel before and after the combination step
It can also be inserted into other methods step there may also be other methods step or between these explicitly mentioned steps, unless separately
It is described；It should also be understood that the combination connection relationship between one or more equipment/device mentioned in the present invention is not repelled
The two equipment/devices specifically mentioned before and after the unit equipment/device there may also be other equipment/device or at these it
Between can also be inserted into other equipment/device, unless otherwise indicated.Moreover, unless otherwise indicated, the number of various method steps is only
Identify the convenient tool of various method steps, rather than for the arrangement order of limitation various method steps or limits the enforceable model of the present invention
It encloses, relativeness is altered or modified, and without material changes in technical content, when being also considered as, the present invention is enforceable
Scope.
The present invention provides a kind of device and method that plastic optical fiber is prepared using PMMA, and this method is specifically by radical polymerization
Close the method that the molecular weight polymers in obtained PMMA remove.
Referring to Fig. 1, the device of use includes extraction flask 1, extraction tube 2, condenser 3, decompressor, and extraction flask 1 is by mentioning
Pipe 2 is taken to be connected to condenser 3, the condenser pipe of condenser 3 is connected to decompressor, and extraction flask 1 and extraction tube 2 pass through bypass pipe 22
Connection, the side wall of extraction tube 2 are communicated with shunt valve 23 upward, are equipped with the siphon pipe 21 for being connected to extraction flask 1 in shunt valve 23,
Condenser pipe 3 is entered by bypass pipe 22 after liquid gasification in extraction flask 1, gas flows into extraction tube 2 after the condensation of condenser pipe 3,
Liquid in extraction tube 2 successively passes through shunt valve 23, siphon pipe 21 is back to extraction flask 1, in other words, the liquid in extraction flask 1
After the heated gasification of body, successively flow back by bypass pipe 22, extraction tube 2, condenser pipe 3, extraction tube 2, shunt valve 23, siphon pipe 21
To extraction flask 1, so that the liquid in extraction tube 2 effectively removes impurity in product.
In some embodiments of the invention, decompressor includes vacuum pump 5, for vacuumizing to space in device
Processing.
It in some embodiments of the invention, further include vacuum governor 4 for vacuum of space in regulating device, very
Air conditioner 4 is mounted on the pipeline between condenser 3 and vacuum pump 5.
In some embodiments of the invention, it is also equipped with pressure gauge 6 on the pipeline between condenser 3 and vacuum pump 5, uses
Vacuum degree in space in real-time displaying device.
In some embodiments of the invention, the top of siphon pipe 21 is equipped with inlet, and the upper connector of bypass pipe 22 is high
It is flushed in the inlet of siphon pipe 21 or with the inlet of siphon pipe 21, the top of shunt valve 23 is equipped with opening, which is located at
The top of horizontal plane where inlet, so that the liquid in extraction tube 2 passes through shunt valve 23, siphon pipe 21 is back to extraction
Bottle 1.
Embodiment 1
PMMA is added in extraction tube 2, (tetrahydrofuran and acetic acid are according to 1 for the extracting solution in extraction flask 1:50 volume ratio
Mixing) gasify after the heating, enter condenser 3 after rising to extraction tube 1, congeals into liquid and instill in extraction tube 1, extract PMMA,
And extraction flask 1 is back to by the extraction of siphon 21.Since the other end of condenser 3 is connected with vacuum pump 5, and it is correspondingly arranged on
Vacuum governor 4, can adjust the air pressure inside of the extraction element by the vacuum governor 4, (vacuum degree control of device exists
0.6-0.8bar).Reduced-pressure backflow 2h, remaining polymer carries out processing of towing again in extraction tube 2, obtained plastic optical fiber light decay
Subtract the polymer being significantly less than without above-mentioned processing.
Embodiment 2
PMMA is added in extraction tube 2, (tetrahydrofuran and acetic acid are according to 1 for the extracting solution in extraction flask 1:60 volume ratio
Mixing) gasify after the heating, enter condenser 3 after rising to extraction tube 1, congeals into liquid and instill in extraction tube 1, extract PMMA,
And extraction flask 1 is back to by the extraction of siphon 21.Since the other end of condenser 3 is connected with vacuum pump 5, and it is correspondingly arranged on
Vacuum governor 4, can adjust the air pressure inside of the extraction element by the vacuum governor 4, (vacuum degree control of device exists
0.6-0.8bar).Reduced-pressure backflow 2.5h, remaining polymer carries out processing of towing again in extraction tube 2, obtained plastic optical fiber light
Decaying is significantly less than the polymer without above-mentioned processing.
Embodiment 3
PMMA is added in extraction tube 2, (tetrahydrofuran and acetic acid are according to 1 for the extracting solution in extraction flask 1:40 volume ratio
Mixing) gasify after the heating, enter condenser 3 after rising to extraction tube 1, congeals into liquid and instill in extraction tube 1, extract PMMA,
And extraction flask 1 is back to by the extraction of siphon 21.Since the other end of condenser 3 is connected with vacuum pump 5, and it is correspondingly arranged on
Vacuum governor 4, can adjust the air pressure inside of the extraction element by the vacuum governor 4, (vacuum degree control of device exists
0.6-0.8bar).Reduced-pressure backflow 1.5h, remaining polymer carries out processing of towing again in extraction tube 2, obtained plastic optical fiber light
Decaying is significantly less than the polymer without above-mentioned processing.
Method for drawing optical fibers
Sandwich layer and cortical material are separately added into two extruders after granulation, by a co-extrusion die head after heating, after
Through supercooling, traction, curling and etc. completion.
For the plastic optical fiber using PMMA as core material, the important indicator for measuring fibre loss performance is decaying,
Test method is cutback technique, uses wavelength for the red-light source of 650nm, and testing result is shown in Table 1.
1 PMMA plastic optical fiber performance test results table of table
| Sample number | Decay (dB/km) | Light transmission uniformity | Toughness | Diameter fluctuation range |
| Comparative example 1 | 178 | Well | It is qualified | It is qualified |
| Embodiment 1 | 135 | Well | It is qualified | It is qualified |
| Embodiment 2 | 144 | Well | It is qualified | It is qualified |
| Embodiment 3 | 140 | Well | It is qualified | It is qualified |
In table 1, comparative example 1 is the PMMA material sample before extraction, as can be found from Table 1, plastic optical fiber after extraction
Pad value is substantially reduced, and achieves significant technological progress.
In conclusion the pad value of plastic optical fiber is effectively reduced by extraction in the present invention, and then effectively promote product matter
Amount, achieves significant technological progress.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (10)
1. a kind of preparation method of low-loss plastic fiber optic materials, it is characterised in that：Including at reduced pressure conditions will be in extraction flask
Extracting solution PMMA heating and gasifying, the extracting solution of gasification enters condenser pipe by bypass pipe, enters after condensing in condenser pipe and mentions
Pipe is taken, PMMA is extracted, leaching liquor is back to extraction flask by siphon pipe, and such circulating reflux obtains the low-loss plastic light
Fiber material.
2. preparation method according to claim 1, it is characterised in that：The leaching liquor includes tetrahydrofuran and acetic acid.
3. preparation method according to claim 2, it is characterised in that：The volume of tetrahydrofuran and acetic acid in the leaching liquor
Than being 1:(40~60), preferably 1:50.
4. preparation method according to claim 1, it is characterised in that：The extracting solution in extraction flask is heated under reduced pressure
When gasification, vacuum degree 0.6-0.8bar.
5. preparation method according to claim 1, it is characterised in that：The circulating reflux time is 1.5-2.5h, preferably 2h.
6. low-loss plastic fiber optic materials made from preparation method as claimed in any of claims 1 to 5.
7. a kind of device for being used to prepare low-loss plastic fiber optic materials, it is characterised in that：Including extraction flask (1), extraction tube
(2), condenser (3), decompressor, the extraction flask (1) is connected to the condenser (3) by the extraction tube (2), described
The condenser pipe of condenser (3) is connected to the decompressor, and the extraction flask (1) and the extraction tube (2) pass through bypass pipe
(22) it is connected to, the extraction tube (2) is communicated with shunt valve (23) upward, is equipped in the shunt valve (23) and is connected to described mention
The siphon pipe (21) of bottle (1) is taken, passes through the bypass pipe (22) entrance condensation after the liquid gasification in the extraction flask (1)
It manages (3), gas flows into the extraction tube (2) after the condenser pipe (3) condense, and the liquid in the extraction tube (2) successively passes through
Cross the shunt valve (23), siphon pipe (21) is back to the extraction flask (1).
8. device according to claim 7, it is characterised in that：The decompressor includes vacuum pump (5), for device
Interior space carries out vacuumize process.
9. device according to claim 8, it is characterised in that：It further include the vacuum for vacuum of space in regulating device
Adjuster (4), the vacuum governor (4) are mounted on the pipeline between the condenser (3) and the vacuum pump (5)；Institute
It states and is also equipped with pressure gauge (6) on the pipeline between condenser (3) and the vacuum pump (5), for empty in real-time displaying device
Between vacuum degree.
10. device according to claim 7, it is characterised in that：The top of the siphon pipe (21) is equipped with inlet, described
The upper connector of bypass pipe (22) is higher than the inlet of the siphon pipe (21) or flushes with the inlet of the siphon pipe (21),
The top of the shunt valve (23) is equipped with opening, the top of horizontal plane where which is located at the inlet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810601247.7A CN108822234A (en) | 2018-06-12 | 2018-06-12 | A kind of preparation facilities and method of low-loss plastic optical fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810601247.7A CN108822234A (en) | 2018-06-12 | 2018-06-12 | A kind of preparation facilities and method of low-loss plastic optical fiber |
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| Publication Number | Publication Date |
|---|---|
| CN108822234A true CN108822234A (en) | 2018-11-16 |
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|---|---|---|---|
| CN201810601247.7A Pending CN108822234A (en) | 2018-06-12 | 2018-06-12 | A kind of preparation facilities and method of low-loss plastic optical fiber |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09255715A (en) * | 1996-03-21 | 1997-09-30 | Tonen Corp | Method for temperature-rise fractionation of crystalline polyolefin and apparatus therefor |
| WO2004009145A1 (en) * | 2002-07-19 | 2004-01-29 | Advanced Cardiovascular Systems, Inc. | Purified polymers for coatings of implantable medical devices |
| CN202961958U (en) * | 2012-11-13 | 2013-06-05 | 东华理工大学 | Decompressed soxhlet extractor |
-
2018
- 2018-06-12 CN CN201810601247.7A patent/CN108822234A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09255715A (en) * | 1996-03-21 | 1997-09-30 | Tonen Corp | Method for temperature-rise fractionation of crystalline polyolefin and apparatus therefor |
| WO2004009145A1 (en) * | 2002-07-19 | 2004-01-29 | Advanced Cardiovascular Systems, Inc. | Purified polymers for coatings of implantable medical devices |
| CN202961958U (en) * | 2012-11-13 | 2013-06-05 | 东华理工大学 | Decompressed soxhlet extractor |
Non-Patent Citations (1)
| Title |
|---|
| 许玉明等: "《创新性国家战略实施路径研究 以塑料光纤产业创新发展为例》", 30 September 2014 * |
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Application publication date: 20181116 |