CN105738601B - The online oxygen content detection method of high-performance polyethylene fibres dry spinning - Google Patents
The online oxygen content detection method of high-performance polyethylene fibres dry spinning Download PDFInfo
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- CN105738601B CN105738601B CN201410755714.3A CN201410755714A CN105738601B CN 105738601 B CN105738601 B CN 105738601B CN 201410755714 A CN201410755714 A CN 201410755714A CN 105738601 B CN105738601 B CN 105738601B
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000001301 oxygen Substances 0.000 title claims abstract description 68
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 68
- 239000004698 Polyethylene Substances 0.000 title claims abstract description 57
- -1 polyethylene Polymers 0.000 title claims abstract description 57
- 229920000573 polyethylene Polymers 0.000 title claims abstract description 57
- 238000001514 detection method Methods 0.000 title claims abstract description 33
- 238000000578 dry spinning Methods 0.000 title claims abstract description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 33
- 238000004458 analytical method Methods 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 20
- 239000007789 gas Substances 0.000 claims abstract description 18
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005070 sampling Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 239000012456 homogeneous solution Substances 0.000 claims description 10
- 238000001179 sorption measurement Methods 0.000 claims description 10
- 239000003463 adsorbent Substances 0.000 claims description 9
- 238000012360 testing method Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 230000008961 swelling Effects 0.000 claims description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 3
- 239000005977 Ethylene Substances 0.000 claims description 3
- 238000009434 installation Methods 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims 1
- 239000003960 organic solvent Substances 0.000 abstract description 5
- 239000003595 mist Substances 0.000 abstract description 4
- 208000027418 Wounds and injury Diseases 0.000 abstract description 3
- 230000006378 damage Effects 0.000 abstract description 3
- 208000014674 injury Diseases 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract 1
- 239000000835 fiber Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 241000521257 Hydrops Species 0.000 description 2
- 206010030113 Oedema Diseases 0.000 description 2
- GEIAQOFPUVMAGM-UHFFFAOYSA-N Oxozirconium Chemical compound [Zr]=O GEIAQOFPUVMAGM-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000010525 oxidative degradation reaction Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 238000002166 wet spinning Methods 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Sampling And Sample Adjustment (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a kind of online oxygen analysis detection methods of high-performance polyethylene fibres dry spinning, when preparing high-performance polyethylene fibres using dry spinning, with the polyethylene powders of decahydronaphthalene solution dissolving super high molecular weight in closed container, it is ultimately delivered to online oxygen conten analyser by filtering, adsorbing to dissolving the gas sampling above liquid in closed container and is detected oxygen content, when carrying out oxygen content detection, it is controlled and sampled by solenoid valve SV1, carry out the waste that blowback avoids resource to filter using compressed nitrogen anti-blowpipe by solenoid valve SV2；The present invention can effectively remove injury of the polyethylene powders reduction of the mist that organic solvent is carried secretly in gas and high molecular weight to online oxygen conten analyser, keep the normal operation of online oxygen analysis detection device, quick online it can accurately analyze the oxygen content detected in high-performance polyethylene fibres, it is ensured that work efficiency；The back suction circulation recycling for also using nitrogen economizes on resources.
Description
Technical field
The present invention relates to polyethylene fibre oxygen analysis detection fields, particularly a kind of high-performance polyethylene fibres dry method
The online oxygen content detection method of spinning.
Background technology
High-performance polyethylene fibres, also known as high strength and modulus polyethylene fibre have high intensity, high-modulus, highly oriented
The characteristics such as degree.The existing high-performance polyethylene fibres that prepare mainly have dry spinning method and wet spinning process, and the two main distinction is
Using different solvent and subsequent technique, dry spinning compared with wet spinning, in dry spinning production technology solvent content compared with
Few, strength is high, resists compacted performance good, is chiefly used in high-end product, due in dry spinning route using solvent directly recycle without
By continuous multi-stage extraction and hot-air drying process, and speed of production is fast, so as to improve production efficiency.
The technical process of dry spinning is polymer first to be carried out to swelling dissolving and then by metering pump feeding at present,
Via spinneret meet and discuss spray liquid stream enter in nitrogen stream, the pre- hot nitrogen of the solvent in thread is pulled away, and high polymer coagulates therewith
Gu into silk, using preliminary draft, high drafting obtains high-performance polyethylene fibres；In dry-spinning process flow, homogeneous is molten
The preparation of liquid is one of key technology of superhigh molecular weight polyethylene fibers spinning, since the preparation of homogeneous solution is lasting
It being carried out under higher temperature environment, polyethylene is easy to that thermal cracking and oxidative degradation occurs, in order to reduce the oxidation rate of polymer,
Bathed using nitrogen, in solvent add antioxidant can effectively inhibit thermal oxidative degradation reaction progress, so gathering to high-performance
Vinyl fiber oxygen content in production is detected and controls just very necessary.
High-performance polyethylene fibres in production need that its oxygen content is detected to ensure oxygen content in prescribed limit
It is interior.When carrying out on-line checking to its oxygen content during producing high-performance polyethylene fibres, organic solvent conveying is easily appeared in
Aggregation is formed in pipeline in the process, causes online oxygen content detection failure.Research and development are a kind of quickly, can extend online oxygen content
The service life of analyzer, the online oxygen analysis detection method of detection high-performance polyethylene fibres dry spinning for reducing environmental pollution
As those skilled in the art it is urgently to be resolved hurrily the technical issues of.
The content of the invention
It is fine to provide a kind of high-performance polyethylene for the shortcomings that technical problems to be solved by the invention are, overcome the prior art
The online oxygen analysis detection method of dry spinning is tieed up, which can effectively remove organic in gas
The mist of solvent entrainment and the polyethylene powders of high molecular weight, reduce the injury to online oxygen conten analyser, keep online oxygen
The normal operation of content analysis detection device can detect in online quick accurate analysis when high-performance polyethylene fibres produce
Oxygen content in high-performance polyethylene fibres, it is ensured that work efficiency；The back suction circulation for also using nitrogen recycles saving money
Source.
In order to solve the above technical problems, the present invention provides a kind of online oxygen content of high-performance polyethylene fibres dry spinning
Analyzing detecting method specifically includes following steps：
（1）Using the polyethylene powders of high molecular weight as raw material, using decahydronaphthalene as solvent, in high temperature environments in closed container
The polyethylene powders of high molecular weight are subjected to swelling dissolving with solvent, homogeneous solution, the take over road by the top of closed container is made
Connect the gas above homogeneous solution；
（2）Draw homogeneous solution overhead gas side take over road on successively installation collection air pump, filter, solenoid valve SV1,
Adsorption box and online oxygen conten analyser, one bypass line of connection passes through on the pipeline between filter and solenoid valve SV1
Solenoid valve SV2 is connected with nitrogen anti-blowpipe；
In closed container in addition to nitrogen necessary to technique and due to system is in tiny structure and penetrates into air, also press from both sides
The polyethylene powders and solvent of band eventually enter into online oxygen content analyzer by collecting air pump by pipeline, and in real time tie detection
For fruit now on the display of online oxygen conten analyser, online oxygen content analyzer passes through electric wire and the computer of remote monitoring room
Connection, the data of detection are transmitted on computer；
（3）Solenoid valve SV2 is first shut off, solenoid valve SV1 is opened and is sampled, the poly- of high molecular weight will be mixed in technique
The gas of ethylene powder eventually enters into online oxygen-containing analysis under gas collection pumping action, by filter, solenoid valve SV1 and adsorption box
Instrument, and testing result is apparent on the display of online oxygen conten analyser in real time；
（4）Solenoid valve SV1 is closed, solenoid valve SV2 is opened, blowback is carried out to filter with compressed nitrogen anti-blowpipe, is compressed
Nitrogen pressure in nitrogen anti-blowpipe is 0.7-0.9MP.
The further preferred technical solution of the present invention is：
In the foregoing online oxygen analysis detection method of high-performance polyethylene fibres dry spinning, employed in filter
Filter core is 7 μm of filter cores.
Filter present invention uses 7 μm of filter cores effectively can prevent polyethylene powders from entering oxygen conten analyser, can
To greatly improve the service life of oxygen conten analyser.
In the foregoing online oxygen analysis detection method of high-performance polyethylene fibres dry spinning, suction used in adsorption box
Attached dose is activated carbon, preferably silica type adsorbent, activated carbon class adsorbent.
Organic solvent entrainment in gas is solved by the way of activated carbon adsorption, is prevented due to caused by pipeline hydrops
Online oxygen analysis test failure extends the service life of online oxygen conten analyser；Adsorbent used is activated carbon class
Adsorbent can be used with circular regeneration, this not only lowers use cost, while can also reduce environmental pollution.
In the foregoing online oxygen analysis detection method of high-performance polyethylene fibres dry spinning, used in nitrogen anti-blowpipe
Time-devision system, blowback and sampling alternately, i.e., per 20min blowback 1s, i.e., accumulate filter inner cavity in 20min sampling period
Polyethylene powders blow back closed container with the nitrogen of 0.7-0.9MPa in 1s.
In the foregoing online oxygen analysis detection method of high-performance polyethylene fibres dry spinning, online oxygen content analyzer is
Zirconia oxygen analyzer；Zirconium oxide formula oxygen instrument checks that the accuracy of oxygen content is high, and sensitivity is good.
The beneficial effects of the invention are as follows：
The processing mode of the present invention online oxygen content analysis detection suitable for some industrial enterprise, especially suitable for high property
The online oxygen content analysis of energy polyethylene fibre dry spinning, solves organic solvent mist in gas by the way of activated carbon adsorption
Entrainment prevents from, due to online oxygen analysis test failure caused by pipeline hydrops, extending the use of online oxygen conten analyser
Service life.
The method that blowback nitrogen is employed in the present invention solves the problems, such as that system is often blocked, and uses nitrogen backblowing can be with
Greatly reduce operating personnel and be replaced as frequently as filter core, this has not only saved material, it is often more important that reduce environmental pollution.
The closure that the present invention is switched using solenoid valve control, the work that this not only greatly reduces operating personnel are strong
Degree, also improves work efficiency.
It is same due to closing SV1 and opening SV2 within the blowback time of 1s in the nitrogen blowback system that the present invention uses
Shi Jinhang's, therefore the nitrogen of 0.7MPa can only be blown by filter in closed container, without blowing into nutrient analyzer, institute
With blowback nitrogen will not cause harmful effect to the oxygen amount detection agency of instrument, simultaneously, moreover it is possible to by what is filtered down by filter
The polyethylene powders of high molecular weight are blown back into closed container to be reacted again, has saved resource, and resource is fully utilized,
Reduce cost.
Description of the drawings
Fig. 1 is the flow of the online oxygen analysis detection method embodiment of high-performance polyethylene fibres dry spinning of the present invention
Schematic diagram.
Specific embodiment
Embodiment 1
The online oxygen analysis detection method of a kind of high-performance polyethylene fibres dry spinning provided in this embodiment, flow
Schematic diagram is as shown in Figure 1, specifically include following steps：
（1）High-performance polyethylene fibres are prepared using dry spinning method, using the polyethylene powders of high molecular weight as raw material, with
Decahydronaphthalene is solvent, and the polyethylene powders of high molecular weight are carried out swelling dissolving system with solvent in closed container in high temperature environments
It obtains homogeneous solution and then carries out subsequent technique and finally obtain high-performance polyethylene fibres, take over road connects by the top of closed container
Gas above logical homogeneous solution；
（2）Sequentially installation collection air pump, the filtering that filter core is 7 μm on the side take over road for drawing homogeneous solution overhead gas
Device, solenoid valve SV1, the adsorption box of interior active charcoal class adsorbent and on-line oxidation zirconium oxygen analyzer, in filter and solenoid valve
A bypass line is connected on pipeline between SV1 by solenoid valve SV2 with nitrogen anti-blowpipe to be connected；
In closed container in addition to nitrogen necessary to technique and due to system is in tiny structure and penetrates into air, also press from both sides
The polyethylene powders and solvent of band eventually enter into online oxygen content analyzer by collecting air pump by pipeline, and in real time tie detection
Fruit is now on the display of online oxygen conten analyser；
（3）Solenoid valve SV2 is first shut off, solenoid valve SV1 is opened and is sampled, the poly- of high molecular weight will be mixed in technique
The gas of ethylene powder eventually enters into on-line oxidation zirconium oxygen under gas collection pumping action, by filter, solenoid valve SV1 and adsorption box
Analyzer, and testing result is apparent on the display of online oxygen conten analyser in real time；
（4）Solenoid valve SV1 is closed, solenoid valve SV2 is opened, blowback is carried out to filter with compressed nitrogen anti-blowpipe, is compressed
Nitrogen pressure in nitrogen anti-blowpipe is 0.7-2.0MPa；
Using time-devision system in nitrogen anti-blowpipe, blowback and sampling alternately, i.e., often 20min blowback 1s, i.e., filter
Inner cavity blows back closed container with the nitrogen of 0.7-0.9MPa in the polyethylene powders that 20min sampling period accumulates in 1s, carries out
It reacts again.
Oxygen content is carried out when dry spinning is used to prepare high-performance polyethylene fibres using the method for the present invention
Detection can effectively remove the mist of organic solvent entrainment and the polyethylene powders of high molecular weight in gas and reduce to online oxygen content
The injury of analyzer keeps the normal operation of online oxygen analysis detection device, can be when high-performance polyethylene fibres produce
Online quick accurate analysis detects the oxygen content in high-performance polyethylene fibres, it is ensured that work efficiency；Also use nitrogen
Back suction circulation recycling economize on resources.
In addition to the implementation, the present invention can also have other embodiment.It is all to use equivalent substitution or equivalent transformation shape
Into technical solution, all fall within the present invention claims protection domain.
Claims (8)
1. a kind of online oxygen analysis detection method of high-performance polyethylene fibres dry spinning, it is characterised in that including following step
Suddenly：
（1）Using the polyethylene powders of super high molecular weight as raw material, using decahydronaphthalene as solvent, used in high temperature environments in closed container
The polyethylene powders of high molecular weight are carried out swelling dissolving and homogeneous solution are made by solvent, and take over road connects by the top of closed container
Gas above logical homogeneous solution；
（2）Sequentially installation collection air pump, filter, solenoid valve SV1, the absorption on the side take over road for drawing homogeneous solution overhead gas
Case and online oxygen conten analyser, one bypass line of connection passes through electromagnetism on the pipeline between filter and solenoid valve SV1
Valve SV2 is connected with nitrogen anti-blowpipe；
（3）Solenoid valve SV2 is first shut off, solenoid valve SV1 is opened and is sampled, by the polyethylene for being mixed with high molecular weight in technique
The gas of powder eventually enters into online oxygen content analyzer under gas collection pumping action, by filter, solenoid valve SV1 and adsorption box,
And testing result is apparent on the display of online oxygen conten analyser in real time；
（4）Solenoid valve SV1 is closed, solenoid valve SV2 is opened, blowback, the pressure is carried out to filter with compressed nitrogen anti-blowpipe
Nitrogen pressure in contracting nitrogen anti-blowpipe is 0.7-2.0MP.
2. the online oxygen analysis detection method of high-performance polyethylene fibres dry spinning according to claim 1, special
Sign is：Filter core employed in the filter is 4-12 μm of filter core.
3. the online oxygen analysis detection method of high-performance polyethylene fibres dry spinning according to claim 2, special
Sign is：Filter core employed in the filter is 7 μm of filter cores.
4. the online oxygen analysis detection method of high-performance polyethylene fibres dry spinning according to claim 1, special
Sign is：Adsorbent used is activated carbon, silica type adsorbent in the adsorption box.
5. the online oxygen analysis detection method of high-performance polyethylene fibres dry spinning according to claim 4, special
Sign is：Adsorbent used is activated carbon class adsorbent in the adsorption box.
6. the online oxygen analysis detection method of high-performance polyethylene fibres dry spinning according to claim 1, special
Sign is：Using time-devision system in the nitrogen anti-blowpipe, blowback and sampling are alternately.
7. the online oxygen analysis detection method of high-performance polyethylene fibres dry spinning according to claim 6, special
Sign is：Per 20min blowback 1s in the nitrogen anti-blowpipe, i.e., filter inner cavity is gathered what 20min sampling period accumulated
Ethylene powder blows back closed container with the nitrogen of 0.7-0.9MPa in 1s.
8. the online oxygen analysis detection method of high-performance polyethylene fibres dry spinning according to claim 1, special
Sign is；The online oxygen content analyzer is zirconia oxygen analyzer.
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| CN106198888A (en) * | 2016-08-16 | 2016-12-07 | 北京京城环保股份有限公司 | A kind of zirconium oxide analysis of oxygen content combination unit and method |
| CN108707988B (en) * | 2018-06-01 | 2020-11-17 | 江西华圆机电有限公司 | Post-spinning equipment for producing high-performance fibers based on melt spinning method |
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| CN200972474Y (en) * | 2006-11-22 | 2007-11-07 | 王健 | Continuosu monitoring system for smoke discharge |
| CN101288820B (en) * | 2008-06-13 | 2011-06-15 | 北京云辰天环保科技有限公司 | Active carbon fiber organic gas recovery method and system using nitrogen as desorption medium |
| CN201442996U (en) * | 2009-07-31 | 2010-04-28 | 山东爱地高分子材料有限公司 | Device for recovering and processing UHMWPE fiber spinning solvent |
| CN102302888A (en) * | 2011-07-22 | 2012-01-04 | 邹希坚 | Organic waste gas recycling device with functions of saving energy and prolonging service life of absorbing agent |
| CN202490561U (en) * | 2011-12-31 | 2012-10-17 | 浙江雅迪纤维有限公司 | Tail gas recovery device generating spandex |
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| CN202666652U (en) * | 2012-06-25 | 2013-01-16 | 临安创亿机械设备有限公司 | Nitrogen-desorbing organic waste gas recycling device |
| CN103801104B (en) * | 2012-11-08 | 2015-10-14 | 中国石油化工股份有限公司 | The power-economizing method of high-performance polyethylene fibres dry spinning solvent recovery |
| CN202974730U (en) * | 2012-12-27 | 2013-06-05 | 铜陵蓝光电子科技有限公司 | Flue gas sampler with heating and back-blowing functions |
| CN103611418B (en) * | 2013-11-26 | 2015-07-22 | 中国化学工业桂林工程有限公司 | Joint treatment device and method for organic waste gas |
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Address after: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee after: China Petroleum & Chemical Corp. Patentee after: SINOPEC NANJING CHEMICAL RESEARCH INSTITUTE Co.,Ltd. Address before: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee before: China Petroleum & Chemical Corp. Patentee before: Nanhua Group Research Institute |