CN106596340B - A kind of online test method of poly(p-phenylene terephthalamide) resin viscosity - Google Patents
A kind of online test method of poly(p-phenylene terephthalamide) resin viscosity Download PDFInfo
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- CN106596340B CN106596340B CN201611234958.2A CN201611234958A CN106596340B CN 106596340 B CN106596340 B CN 106596340B CN 201611234958 A CN201611234958 A CN 201611234958A CN 106596340 B CN106596340 B CN 106596340B
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- phenylene terephthalamide
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N11/02—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material
- G01N11/04—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture
- G01N11/06—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture by timing the outflow of a known quantity
Abstract
The present invention relates to the online test methods of aramid fiber resin viscosity detection field more particularly to a kind of poly(p-phenylene terephthalamide) (PPTA) resin viscosity.The advantages that this method proposes the method for measuring aramid fiber resin viscosity by the resin extruded machine motor torque of aramid fiber and revolving speed, has method simple, and measuring speed is fast, and measurement reproducibility is good, at low cost.
Description
Technical field
The present invention relates to aramid fiber resin viscosity detection field more particularly to a kind of poly(p-phenylene terephthalamide) (PPTA)
The online test method of resin viscosity.
Background technique
Para-aramid fiber is a kind of height with high-strength and high-modulus, high temperature resistant, acid and alkali-resistance and the excellent properties such as light-weight
Performance materials are all widely used in civilian and national defence.Produce the poly(p-phenylene terephthalamide) of molecular weight stabilizers
(PPTA) resin is precondition and the basis for producing para-aramid fiber.During producing PPTA resin, PPTA molecule
The quick detection of amount is one of crucial problem.
PPTA polymer molecular weight is distributed the quality for directly influencing spinning moulding, and PPTA molecular weight detection is common at present
Method is sulfuric acid process.PPTA is slowly dissolve into the concentrated sulfuric acid, then uses the stream of determination of ubbelohde viscometer PPTA sulfuric acid solution
It time out, is then compared with the concentrated sulfuric acid delivery time, finally obtains logarithmic viscosity number η.But in this method due to
The rigid structure of PPTA macromolecular causes dissolution flow velocity very slow, time-consuming very long.For example the PPTA resin for spinning is general
η will usually dissolve 48h or more in 6.0-6.5dL/g in 98% concentrated sulfuric acid, this supervises the quality of PPTA continuous polymerization production
Survey is a huge challenge.
Summary of the invention
Being difficult to dissolve for PPTA resin causes viscosity to be difficult to quickly detect, and cannot be online in continuous polymerization production
The problem of detecting viscosity, the present invention propose a kind of quick, on-line checking PPTA viscosity method.
A kind of online test method of poly(p-phenylene terephthalamide) resin viscosity of the present invention includes following step
It is rapid:
(1) in poly(p-phenylene terephthalamide) resin polymerization factory formula, hydrotropy salt and water content is adjusted, is gathered
Poly P phenylene diamine terephthalamide resin polymerization；
(2) the control temperature T of setting screw extruder is required according to technique；
(3) keep temperature T it is constant under the premise of, rotational speed omega is controlled respectively 80r/min, 85r/min, 90r/min,
95r/min and 100r/min takes 20 to polymerize obtained poly(p-phenylene terephthalamide) resin-like respectively under each revolving speed
Product, at the same when recording the sampling of each sample extruder torque M；
(4) each above-mentioned poly(p-phenylene terephthalamide) resin sample is used into concentrated sulfuric acid dissolution respectively, it is viscous with Ubbelohde
Degree meter method detects its logarithmic viscosity number η；
(5) data that step (3) and step (4) obtain are input to Matlab software to analyze, utilize curve matching
Method founding mathematical models obtain the K under formula 1 and the process conditions1、K2Specific value.
η=K1M/ω+K2T formula 1
Wherein:
η is logarithmic viscosity number；
M is the torque M of extruder motor, unit NM；
ω is revolving speed, unit r/min；
T is temperature, unit DEG C.
(6) it when carrying out the online viscosity measurements of poly(p-phenylene terephthalamide) resin, requires that screw rod is kept to squeeze according to technique
The temperature T of machine is constant out, and workshop DCS monitoring system can acquire the torque M and rotational speed omega parameter of extruder motor in real time, benefit
With the computation model in step (5), the logarithmic viscosity number of poly(p-phenylene terephthalamide) resin is calculated.
In the present invention, the specific production technology of PPTA resin is referring to Chinese patent ZL201210485817.3, in PPTA tree
In rouge polymerization formula, hydrotropy salt and water content are adjusted, while other technological parameters constant (including monomer ratio, polymerization temperature
Degree, washing drying condition etc.) obtain the different PPTA resin of molecular weight.
Motor driver used in the present invention controls frequency converter using the ACS550 high performance vector of ABB AB's production,
Current motor parameter can be read in real time by ModBus interface.
In formula 1, K1And K2For constant, in specific production process, due to K1With the length of screw rod in extruder, radius,
Screw rod cavity radius and related, the K of screw rod internal gear arrangement2It is related to the temperature of charge in current extruder, if in production technology
It is temperature-resistant, it squeezes out machine equipment and does not change, then K1、K2To determine value, no longer need to be fitted, but work as polymerization technique temperature
Or it squeezes out when machine equipment changes and parameter in formula 1 should be fitted according to method described in the invention again.
The present invention and prior art compare, and have following technical effect that
1. it is fast to detect speed, it can be detected with on-line continuous, effectively solve the problems, such as that PPTA resin is difficult to quickly detect viscosity.
2. testing cost is cheap.
Detailed description of the invention
Fig. 1 is the PPTA sample data obtained under different rotating speeds, the torque of extruder when abscissa is each sample
M, ordinate are its logarithmic viscosity number η of Ubbelohde viscometer method detection；
Fig. 2 is structural schematic diagram of the invention.
Specific embodiment
As described below is only a specific embodiment of the invention, is not intended to restrict the invention.It is all of the invention
Any modifications, equivalent replacements, and improvements done within spirit and principle, should be included within the scope of the present invention.
In the present invention, the specific production technology of PPTA resin is referring to Chinese patent ZL201210485817.3, in PPTA tree
In rouge polymerization formula, hydrotropy salt and water content are adjusted, while other technological parameters constant (including monomer ratio, polymerization temperature
Degree, washing drying condition etc.) obtain the different PPTA resin of molecular weight；
Below with reference to Fig. 1, technical scheme is described further:
The screw rod is extruder screw device.
The motor is direct current generator.
The motor driver controls frequency converter using the ACS550 high performance vector of ABB AB's production, and the frequency converter is real
When read current of electric, torque, the parameters such as revolving speed, and DCS controller can be transferred data to by ModBus interface.
The temperature transmitter is for measuring temperature of charge in extruder.
The DCS controller is Hollysys MACS5 control system, for acquiring motor torque, revolving speed and temperature signal, root
The PPTA resin viscosity currently produced is calculated according to these parameters, and calculated viscosity number is shown on the monitoring page.
The display is for showing the calculated PPTA resin viscosity of DCS.
Embodiment 1
The specific steps of PPTA resin viscosity online test method disclosed by the invention are as follows:
(1) referring to Chinese patent ZL201210485817.3, in PPTA resin polymerization factory formula, adjustment hydrotropy salt and
Water content carries out poly(p-phenylene terephthalamide) resin polymerization；
(2) T=52 DEG C of the control temperature of setting screw rod is required according to technique；
(3) keep temperature T it is constant under the premise of, screw speed is controlled respectively 80r/min, 85r/min, 90r/min,
95r/min and 100r/min takes 20 to polymerize obtained PPTA sample respectively under each revolving speed, while recording each sample
The torque M of extruder when sampling；
(4) each above-mentioned PPTA resin sample is used into concentrated sulfuric acid dissolution respectively, detects it than dense with Ubbelohde viscometer method
Log viscosities η, all PPTA sample viscosities are as shown in table 1 and Fig. 1；
Table 1PPTA sample viscosity
(5) data that step (3) and step (4) obtain are input to Matlab software to analyze, utilize curve matching
Method founding mathematical models formula 1 and the process conditions under K1、K2Specific value obtains practical viscosity calculation formula 2,
η=K1M/ω+K2T formula 1
η=0.6996M/ ω+0.0154T formula 2
Wherein:
η is logarithmic viscosity number；
M is the torque M of extruder motor, unit NM；
ω is revolving speed, unit r/min；
T is temperature, unit DEG C.
(6) it when carrying out the online viscosity measurements of poly(p-phenylene terephthalamide) resin, requires that screw rod is kept to squeeze according to technique
The temperature T of machine is constant out, and workshop DCS monitoring system can acquire the torque M and rotational speed omega parameter of extruder motor in real time, benefit
With the computation model in step (5), the viscosity of poly(p-phenylene terephthalamide) resin is calculated.
DCS system used in the present invention is the MACS5 system of company, Hollysys.
The method of the invention is compared with traditional sulfuric acid process, and sulfuric acid process time of measuring was at 48 hours or more, institute of the present invention
Stating method is real-time measurement, and time of measuring is very short.
A kind of online test method of poly(p-phenylene terephthalamide) (PPTA) resin viscosity that the present embodiment proposes, tool
Have and detects the advantages that speed is fast, and measurement range is wide, reproducible, at low cost.
Comparative example
Under process conditions described in embodiment 1, the practical viscosity calculation formula 2 obtained using embodiment 1, to poly- to benzene
The viscosity and obtained using traditional detection method viscous that the two online viscosity of formyl p-phenylenediamine resin are detected, and obtained
Degree compares, specific as shown in table 2:
2 present invention of table and traditional detection method Comparative result
Claims (3)
1. a kind of online test method of poly(p-phenylene terephthalamide) resin viscosity, it is characterised in that: comprise the steps of:
(1) in poly(p-phenylene terephthalamide) resin polymerization factory formula, hydrotropy salt and water content is adjusted, is gathered to benzene
Two formyl p-phenylenediamine resin polymerizations；
(2) the control temperature T of setting screw extruder is required according to technique；
(3) under the premise of keeping temperature T constant, rotational speed omega is controlled respectively in 80r/min, 85r/min, 90r/min, 95r/
Min and 100r/min takes 20 to polymerize obtained poly(p-phenylene terephthalamide) resin sample, together respectively under each revolving speed
The torque M of extruder when the sampling of each sample of Shi Jilu；
(4) each above-mentioned poly(p-phenylene terephthalamide) resin sample is used into concentrated sulfuric acid dissolution respectively, uses Ubbelohde viscometer
Method detects its logarithmic viscosity number η；
(5) data that step (3) and step (4) obtain are input to Matlab software to analyze, utilize the side of curve matching
Method founding mathematical models obtain the K under formula 1 and the process conditions1、K2Specific value；
η=K1M/ω+K2T formula 1
Wherein:
η is logarithmic viscosity number；
M is the torque M of extruder motor, unit NM；
ω is revolving speed, unit r/min；
T is temperature, unit DEG C；
K1And K2For constant, in specific production process, due to K1With the length of screw rod, radius, screw rod cavity radius in extruder
With related, the K of screw rod internal gear arrangement2It is related to the temperature of charge in current extruder, if temperature-resistant in production technology, squeeze out
Machine equipment does not change, then K1、K2To determine value, no longer need to be fitted；
(6) it when carrying out the online viscosity measurements of poly(p-phenylene terephthalamide) resin, requires to keep screw extruder according to technique
Temperature T it is constant, workshop DCS monitoring system can acquire the torque M and rotational speed omega parameter of extruder motor in real time, utilize
Computation model in step (5), calculates the logarithmic viscosity number of poly(p-phenylene terephthalamide) resin.
2. a kind of online test method of poly(p-phenylene terephthalamide) resin viscosity according to claim 1, special
Sign is: the driver of the motor controls frequency converter using the ACS550 high performance vector of ABB AB's production, and the frequency converter is real
When read current of electric, torque, rotary speed parameter, and DCS monitoring system can be transferred data to by ModBus interface.
3. a kind of online test method of poly(p-phenylene terephthalamide) resin viscosity according to claim 1 or 2,
Be characterized in that: the DCS monitoring system is the MACS5 of company, Hollysys.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611234958.2A CN106596340B (en) | 2016-12-28 | 2016-12-28 | A kind of online test method of poly(p-phenylene terephthalamide) resin viscosity |
| PCT/CN2017/118954 WO2018121597A1 (en) | 2016-12-28 | 2017-12-27 | On-line detection method for viscosity of poly(p-phenylene terephthalamide) resin |
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| CN201611234958.2A CN106596340B (en) | 2016-12-28 | 2016-12-28 | A kind of online test method of poly(p-phenylene terephthalamide) resin viscosity |
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| CN106596340B (en) * | 2016-12-28 | 2019-04-23 | 中芳特纤股份有限公司 | A kind of online test method of poly(p-phenylene terephthalamide) resin viscosity |
| CN108982725A (en) * | 2018-08-27 | 2018-12-11 | 朗析仪器（上海）有限公司 | A kind of in-line analyzer for industrial on-line analysis refrigerant R134a |
| WO2020133313A1 (en) * | 2018-12-29 | 2020-07-02 | 中芳特纤股份有限公司 | Flow control system and control method for para-aramid spinning |
| CN110658036B (en) * | 2019-09-05 | 2022-05-06 | 上海化工研究院有限公司 | Preparation of UHMWPE dilute solution and method for detecting dissolution degree of UHMWPE dilute solution |
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| CN203981538U (en) * | 2014-06-23 | 2014-12-03 | 华南理工大学 | A kind of proving installation of online sign reclaimed rubber mooney viscosity |
| CN204718920U (en) * | 2015-05-03 | 2015-10-21 | 鹤壁百运佳印务有限公司 | A kind of resin viscosity determinator |
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| JP2009292984A (en) * | 2008-06-09 | 2009-12-17 | Du Pont Toray Co Ltd | Method for treating solution of poly paraphenylene terephthalamide in concentrated sulfuric acid |
| JP4883142B2 (en) * | 2008-07-04 | 2012-02-22 | Ｄｉｃ株式会社 | Reaction liquid viscosity measuring apparatus, reaction liquid manufacturing apparatus, and reaction liquid manufacturing method |
| CN101798385B (en) * | 2010-03-15 | 2012-07-11 | 苏州兆达特纤科技有限公司 | Production technology of poly (p-phenytene terephthalamide) resin |
| CN101839838A (en) * | 2010-05-21 | 2010-09-22 | 厦门派鼎自动化设备有限公司 | Resin viscosity on-line measurement system |
| CN101928395A (en) * | 2010-08-16 | 2010-12-29 | 深圳市中晟创新科技股份有限公司 | Preparation method of polyphenylene terephthalamide resin |
| JP5168609B2 (en) * | 2011-06-30 | 2013-03-21 | Ｄｉｃ株式会社 | Method for detecting viscosity of reaction solution, viscosity detection device for reaction solution, method for obtaining reaction product, and production device for obtaining reaction product |
| CN105181526B (en) * | 2015-07-17 | 2017-08-25 | 江苏恒神股份有限公司 | The detection method of viscosity in sizing agent production process |
| CN105699255A (en) * | 2016-03-15 | 2016-06-22 | 山东万圣博科技股份有限公司 | Method for rapidly detecting molecular weight of poly-p-phenylene terephthamide resin |
| CN106596340B (en) * | 2016-12-28 | 2019-04-23 | 中芳特纤股份有限公司 | A kind of online test method of poly(p-phenylene terephthalamide) resin viscosity |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203981538U (en) * | 2014-06-23 | 2014-12-03 | 华南理工大学 | A kind of proving installation of online sign reclaimed rubber mooney viscosity |
| CN204718920U (en) * | 2015-05-03 | 2015-10-21 | 鹤壁百运佳印务有限公司 | A kind of resin viscosity determinator |
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Address after: 257300 Guangrao Binhai New Area in Dongying, Shandong Applicant after: Zhongfang Special Fiber Co., Ltd. Applicant after: Tsinghua University Address before: 257300 Guangrao Binhai New Area in Dongying, Shandong Applicant before: Shandong Wanshengbo Technology Co.,Ltd. Applicant before: Tsinghua University |
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