CN106596340A - On-line detection method of viscosity of poly(p-phenylene terephthalamide) resin - Google Patents
On-line detection method of viscosity of poly(p-phenylene terephthalamide) resin Download PDFInfo
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- CN106596340A CN106596340A CN201611234958.2A CN201611234958A CN106596340A CN 106596340 A CN106596340 A CN 106596340A CN 201611234958 A CN201611234958 A CN 201611234958A CN 106596340 A CN106596340 A CN 106596340A
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- 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
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Abstract
The invention relates to the field of aramid resin viscosity detection and especially relates to an on-line detection method of viscosity of poly(p-phenylene terephthalamide) (PPTA) resin. The method realizes measurement of aramid resin viscosity through aramid resin extruder motor torque and a rotation rate. The method has the advantages of simple processes, fast measurement rate, good measurement repeatability and low cost.
Description
Technical field
The present invention relates to aramid fiber resin viscosity detection field, more particularly to a kind of PPTA (PPTA)
The online test method of resin viscosity.
Background technology
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 lightweight
Performance materials, are all widely used in civilian and national defence.The PPTA of production molecular weight stabilizers
(PPTA) resin is precondition and the basis for producing para-aramid fiber.During production PPTA resins, PPTA molecules
The quick detection of amount is one of crucial problem.
PPTA molecular weight distribution directly influences the quality of spinning moulding, current PPTA molecular weight detections it is conventional
Method is sulfuric acid process.Will PPTA be slowly dissolve in concentrated sulphuric acid, then with the stream of determination of ubbelohde viscometer PPTA sulfuric acid solutions
Go out the time, be then compared with the concentrated sulphuric acid delivery time, finally draw logarithmic viscosity number η.But in the method due to
The rigid structure of PPTA macromole, causes to dissolve flow velocity slowly, takes very long.The PPTA resins for being such as used for spinning are general
η will generally dissolve more than 48h in 6.0-6.5dL/g, in 98% concentrated sulphuric acid, and this is for the quality prison of PPTA continuous polymerizations production
Survey is a huge challenge.
The content of the invention
Being difficult to dissolving for PPTA resins causes viscosity to be difficult to quick detection, and can not be online in continuous polymerization production
Viscosimetric problem is examined, the present invention proposes a kind of quick, method of on-line checking PPTA viscosity.
The online test method of a kind of PPTA resin viscosity of the present invention, comprising following step
Suddenly：
(1) in PPTA resin polymerization factory formula, hydrotropy salt and water content are adjusted, is gathered
Poly P phenylene diamine terephthalamide resin polymerization；
(2) control temperature T of screw extruder is set according to technological requirement；
(3) on the premise of keeping temperature T is constant, rotational speed omega is controlled respectively 80r/min, 85r/min, 90r/min,
95r/min and 100r/min, takes respectively 20 PPTA resin-likes for obtaining that are polymerized under each rotating speed
Product, at the same when recording the sampling of each sample extruder torque M；
(4) above-mentioned each PPTA resin sample is used respectively concentrated sulfuric acid dissolution, it is viscous with Ubbelohde
Degree meter method detects its logarithmic viscosity number η；
(5) data input that step (3) and step (4) are obtained is analyzed to Matlab softwares, using curve matching
The method founding mathematical models K that obtains under formula 1, and the process conditions1、K2Concrete numerical value.
η=K1M/ω+K2T formula 1
Wherein：
η is logarithmic viscosity number；
M for extruder motor torque M, unit NM；
ω is rotating speed, unit r/min；
T is temperature, unit DEG C.
(6) when carrying out the online viscosity measurements of PPTA resin, screw rod is kept to squeeze according to technological requirement
Temperature T for going out machine is constant, workshop DCS monitoring systems can Real-time Collection extruder motor torque M and rotational speed omega parameter, profit
With the computation model in step (5), the logarithmic viscosity number of PPTA resin is calculated.
In the present invention, the concrete production technology reference Chinese patent ZL201210485817.3 of PPTA resins, in PPTA trees
In fat polymerization formula, hydrotropy salt and water content are adjusted, while other technological parameters are constant (including monomer ratio, polymerization temperature
Degree, washing drying condition etc.) obtain the different PPTA resins of molecular weight.
Motor driver used in the present invention controls converter using the ACS550 high performance vectors of ABB AB's production,
Current motor parameter can in real time be read by ModBus interfaces.
In formula 1, K1And K2For constant, in concrete production process, due to K1With the length of screw rod in extruder, radius,
Screw rod inner chamber radius and screw rod internal gear relevant, the K of arrangement2It is related to the temperature of charge in current extruder, if in production technology
Temperature-resistant, extrusion machine equipment does not change, then K1、K2For determination value, without the need for being fitted again, but when polymerization technique temperature
Or extrusion machine equipment should be fitted according to method described in the invention to the parameter in formula 1 again when changing.
The present invention and prior art contrast, with following technique effect：
1. detection speed is fast, can be detected with on-line continuous, and effectively solving PPTA resin is difficult to a difficult problem for quick detection viscosity.
2. testing cost is cheap.
Description of the drawings
Fig. 1 is the PPTA sample datas that obtain under different rotating speeds, the torque of extruder when abscissa is each sample
M, vertical coordinate is its logarithmic viscosity number η of Ubbelohde viscometer method detection；
Fig. 2 is the structural representation of the present invention.
Specific embodiment
Described below is only the specific embodiment of the present invention, is not limited to the present invention.It is all the present invention
Any modification, equivalent and the improvement made within spirit and principle, should be included in protection scope of the present invention.
In the present invention, the concrete production technology reference Chinese patent ZL201210485817.3 of PPTA resins, in PPTA trees
In fat polymerization formula, hydrotropy salt and water content are adjusted, while other technological parameters are constant (including monomer ratio, polymerization temperature
Degree, washing drying condition etc.) obtain the different PPTA resins of molecular weight；
Technical scheme is described further with reference to Fig. 1：
The screw rod is extruder screw device.
The motor is direct current generator.
The motor driver controls converter, the converter reality using the ACS550 high performance vectors of ABB AB's production
When read current of electric, torque, the parameter such as rotating speed, it is possible to DCS controllers are transferred data to by ModBus interfaces.
The temperature transmitter is used to measure temperature of charge in extruder.
The DCS controllers are Hollysys's MACS5 control systems, for gathering motor torque, rotating speed and temperature signal, root
The PPTA resin viscosities of current production are calculated according to these parameters, and the viscosity number for calculating is shown on the monitoring page.
The display is used to show the PPTA resin viscosities that DCS is calculated.
Embodiment 1
PPTA resin viscosities online test method disclosed by the invention is concretely comprised the following steps：
(1) with reference to Chinese patent ZL201210485817.3, in PPTA resin polymerization factory formulas, adjustment hydrotropy salt and
Water content, carries out PPTA resin polymerization；
(2) control temperature T=52 DEG C of screw rod is set according to technological requirement；
(3) on the premise of keeping temperature T is constant, screw speed is controlled respectively 80r/min, 85r/min, 90r/min,
95r/min and 100r/min, takes respectively 20 PPTA samples for obtaining that are polymerized, while recording each sample under each rotating speed
The torque M of extruder during sampling；
(4) above-mentioned each PPTA resin sample is used respectively concentrated sulfuric acid dissolution, 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 input that step (3) and step (4) are obtained is analyzed to Matlab softwares, using curve matching
Method founding mathematical models formula 1 and the process conditions under K1、K2Concrete numerical value, obtains practical viscosity computing formula 2,
η=K1M/ω+K2T formula 1
η=0.6996M/ ω+0.0154T formula 2
Wherein：
η is logarithmic viscosity number；
M for extruder motor torque M, unit NM；
ω is rotating speed, unit r/min；
T is temperature, unit DEG C.
(6) when carrying out the online viscosity measurements of PPTA resin, screw rod is kept to squeeze according to technological requirement
Temperature T for going out machine is constant, workshop DCS monitoring systems can Real-time Collection extruder motor torque M and rotational speed omega parameter, profit
With the computation model in step (5), the viscosity of PPTA resin is calculated.
DCS system used in the present invention is the MACS5 systems of company of Hollysys.
The method of the invention compared with traditional sulfuric acid process, sulfuric acid process time of measuring more than 48 hours, institute of the present invention
Method is stated to measure in real time, time of measuring is very short.
A kind of online test method of PPTA (PPTA) resin viscosity that the present embodiment is proposed, tool
There is detection speed fast, measurement range width, reproducible, low cost and other advantages.
Comparative example
Under the process conditions described in embodiment 1, the practical viscosity computing formula 2 obtained using embodiment 1, to poly- to benzene
The online viscosity of two formyl p-phenylenediamine resins is detected, and the viscosity for being obtained is viscous with what is obtained using traditional detection method
Degree is contrasted, concrete as shown in table 2：
The present invention of table 2 and traditional detection method Comparative result
Claims (3)
1. a kind of online test method of PPTA resin viscosity, it is characterised in that：Comprise the steps of：
(1) in PPTA resin polymerization factory formula, hydrotropy salt and water content are adjusted, is carried out poly- to benzene
Two formyl p-phenylenediamine resin polymerizations；
(2) control temperature T of screw extruder is set according to technological requirement；
(3) on the premise of keeping temperature T is constant, rotational speed omega is controlled respectively in 80r/min, 85r/min, 90r/min, 95r/
Min and 100r/min, takes respectively 20 PPTA resin sample for obtaining that are polymerized, together under each rotating speed
The torque M of extruder during the sampling of Shi Jilu each sample；
(4) above-mentioned each PPTA resin sample is used respectively concentrated sulfuric acid dissolution, Ubbelohde viscometer is used
Method detects its logarithmic viscosity number η；
(5) data input that step (3) and step (4) are obtained is analyzed to Matlab softwares, using the side of curve matching
Method founding mathematical models obtain the K under formula 1, and the process conditions1、K2Concrete numerical value.
η=K1M/ω+K2T formula 1
Wherein：
η is logarithmic viscosity number；
M for extruder motor torque M, unit NM；
ω is rotating speed, unit r/min；
T is temperature, unit DEG C.
(6) when carrying out the online viscosity measurements of PPTA resin, according to technological requirement screw extruder is kept
Temperature T it is constant, workshop DCS monitoring systems can Real-time Collection extruder motor torque M and rotational speed omega parameter, using step
Suddenly the computation model in (5), calculates the logarithmic viscosity number of PPTA resin.
2. the online test method of a kind of PPTA resin viscosity according to claim 1, it is special
Levy and be：Motor driver used in the present invention is somebody's turn to do using the ACS550 high performance vectors control converter of ABB AB's production
Converter reads in real time the parameters such as current of electric, torque, rotating speed, it is possible to transfer data to DCS prisons by ModBus interfaces
Control system.
3. the online test method of a kind of PPTA resin viscosity according to claim 1, it is special
Levy and be：Described DCS monitoring systems are the MACS5 of company of Hollysys.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| CN106596340A true CN106596340A (en) | 2017-04-26 |
| CN106596340B CN106596340B (en) | 2019-04-23 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018121597A1 (en) * | 2016-12-28 | 2018-07-05 | 中芳特纤股份有限公司 | On-line detection method for viscosity of poly(p-phenylene terephthalamide) resin |
| 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 |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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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| 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 |
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| WO2018121597A1 (en) | 2018-07-05 |
| CN106596340B (en) | 2019-04-23 |
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