CN105181526B - The detection method of viscosity in sizing agent production process - Google Patents
The detection method of viscosity in sizing agent production process Download PDFInfo
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Abstract
The present invention provides a kind of detection method of viscosity in sizing agent production process, moment of torsion is measured by the torque sensor built in reactor, while testing the viscosity of the period material, corresponding relation curve is made by nonlinear fitting, and equation is derived, and then monitor the viscosity of material at any period.The present invention can continuously, viscosity that is quick, economic, easily determining material in reactor in sizing agent production process, cumbersome, the time-consuming and poor efficiency of conventional test methodologies is overcome, while saving the funds of the expensive import in-line viscometer of purchase.The present invention can rapidly, continuously determine the viscosity of material in reactor in sizing agent production process, and the reaction process of monitoring material in reactor and determination reaction end, are conducive to lifting the stability between product batches in time, while reducing total production cost.
Description
Technical field
The present invention relates to a kind of detection method of viscosity in sizing agent production process.
Background technology
Carbon fiber is the important component of advanced composite material, is enjoyed great prestige with the outstanding advantages of its " height ", " strong ", " light weight "
The world, the preferred material as industries such as Aero-Space, high-end automobile, high-grade sports goods.Sizing agent is the important of carbon fiber
Part, on the one hand can improve convergence, wearability, pliability, antistatic behaviour of carbon fiber etc., meet carbon fiber rear
Sequel knit, presoak, laying, winding, the performance requirement of the composite material manufacturing technology such as pultrusion.On the other hand, sizing agent is conducive to
Strengthen the wellability of carbon fiber and matrix resin, improve the interfacial adhesion between carbon fiber and matrix resin, improve composite
Interlaminar shear strength.
In the production process of sizing agent, to reaction process often without fast and accurately monitoring method.In general lead
There are two methods：
A kind of is according to the material state in reaction vessel and reaction by the technical staff with certain working experience
The range estimation such as time judges.Such a method biggest advantage is the speed of " monitoring ", will not also be significantly affected in reaction vessel
The process of material change.But the shortcoming of this method is also evident from, the judgement of different technical staff to reaction process is deposited
In difference, subjective consciousness is stronger, runs counter to the regulation of quality system management, and the quality of final products is influenceed to a certain extent.
Another method is that in the production process of sizing agent, material is taken out out of reaction vessel, tests its key
Performance, such as viscosity and epoxide equivalent etc..The advantage of such a method be can with quantitative test These parameters, as judge to react into
The foundation of journey.But it has the disadvantage that have ignored sizing agent production is a continuous process, and testing needs the time, therefore simultaneously
Can not real reaction mass instantaneous state, particularly during mass production, this method receives all many conditions
Limitation, is of limited application.
So, need badly and set up a kind of effective monitoring method of sizing agent reaction process, so as to ensure end product quality
It is stable, while can also reduce production cost, improve productivity effect.
Viscosity is to weigh the important physical parameter that liquid resists fluid ability.In the field such as physical chemistry and hydrodynamics,
Viscosity measurement is the means of the relative efficiency of industrial stokehold.Same viscosity can also reflect thing in the production process of sizing agent
The reaction process of material.It has been mentioned that the method for testing of viscosity in above-mentioned, it is clear that feasibility is not strong in actual production, more
Enterprise still select to judge reaction process using the method for range estimation.
The content of the invention
It is an object of the invention to propose a kind of the continuous, quick, economic, easily of viscosity in sizing agent production process
Detection method, overcomes cumbersome, the time-consuming and poor efficiency of conventional test methodologies, while saving the expensive import in-line viscometer of purchase
Funds.
The material viscosity that the method that the present invention is provided can reflect in sizing agent production process, so as to monitor thing in reactor
The reaction process and determination reaction end of material, more accurately to carry out quality control, improve the product quality of sizing agent
Stability, reduces production cost.
The present invention technical solution be：
The detection method of viscosity in a kind of sizing agent production process, is measured by the torque sensor built in reactor and turned round
Square, while testing the viscosity of the period material, corresponding relation curve is made by nonlinear fitting, and derives equation, is entered
And the viscosity of material at any period is monitored, detecting step is as follows：
Step one, the torque value that period sample is sampled in sizing agent production process is determined；
Step 2, determines the sample viscosity value of sampling period, after sampling, is determined using viscosimeter and samples the viscous of period sample
Angle value y；
Step 3, respectively correspondingly inputs computer by the moment of torsion and viscosity number of the sampling period sample of measure, maps
To moment of torsion and the relation curve of viscosity；
The moment of torsion and the relation curve of viscosity of sampling sample, pass through the machine of emulsion polymerization in step 4, fitting above-mentioned steps
Li Ke get, viscosity during material phase inversion reaches maximum；Observe above-mentioned relation curve to understand, in the production process of sizing agent, glue
There are two kinds of variation tendencies in the relation curve of degree and moment of torsion：Material occurs before phase inversion, and viscosity is presented first with the increase of torque value
Tend to slow phenomenon, after phase inversion adds water, viscosity after quick increase but reduce with the reduction of torque value；Pass through non-thread
Property fitting, obtain the moment of torsion of material and the relation curve equation of viscosity be：
Before phase inversion：Y=a*x2+b*x+c (1)
After phase inversion：Y=d*x+e (2)
Step 5, optimizes the moment of torsion of material and the relation curve equation of viscosity；
First, the coefficient R of formula (1) and formula (2) is separately verified；By origin nonlinear fitting, if formula
(1) and formula (2) R>0.9, the fit equation can be used directly；If the R of formula (1) and formula (2)<0.9, repeat step one, increase
Sample the torque value quantity of period sample and reduce the sample interval between two neighboring torque value, retrieve moment of torsion and
After the relation curve of viscosity, according still further to Step 4: step 5 is fitted and optimized to curve, until meeting above-mentioned requirements and being
Only；The moment of torsion of material after being optimized and the relation curve equation of viscosity；
Step 6, the test of online viscosity；When sizing agent is produced, this is determined by the torque sensor built in reactor
The moment of torsion of one period material in reactor, according to the moment of torsion and the relation curve equation of viscosity after optimization in step 5, by moment of torsion
Value input, is converted into the viscosity number output of same period reactor material, to monitor the reaction process of the period.
Further, step one is specially：Sizing agent is produced using homogeneous raw material, same formula, same production technology,
The moment of torsion of sampling period sample is determined using the torque sensor built in sizing agent reactor, if being sampled in sizing agent production process
The sample torque value of period is represented with x, then samples the torque value quantity at least 6 of sample, the wherein sampling of phase inversion stage at least
Two, the sample interval between two neighboring torque value is 10-60min.
Further, the kettle top upper end of reactor opens up through hole, in a major axis agitating paddle built in through hole, major axis agitating paddle bag
Power transmission shaft and the blade on power transmission shaft are included, the upper end of major axis agitating paddle seals the motor with being supported on outside kettle by magnetic machine
Ball valve is set on connection, the through hole of reactor, and torque sensor seals the upper end for being supported on ball valve by magnetic machine.
Further, viscosimeter uses rotation viscometer or cone and plate viscometer.
The beneficial effects of the invention are as follows：
First, the method for testing is simple and convenient, and without complicated part, cost can be ignored substantially；
2nd, the viscosity of material in reactor in sizing agent production process can rapidly, continuously be determined, in time monitoring reaction
The reaction process of material and determination reaction end, are conducive to lifting the stability between product batches in kettle；
3rd, the product quality of sizing agent is improved, it is ensured that the stabilization of product quality, while indirectly reducing production assembly
This.
Brief description of the drawings
Fig. 1 is the moment of torsion of material in embodiment one and the graph of relation of viscosity.
Fig. 2 is the moment of torsion of material in embodiment two and the relation curve of viscosity.
Fig. 3 is the moment of torsion of material in embodiment three and the relation curve of viscosity.
Fig. 4 is the moment of torsion of material in example IV and the relation curve of viscosity.
Fig. 5 is the structural representation of reactor in embodiment.
Wherein：1- kettlies, 2- blades, 3- power transmission shafts, 4- torque sensors, 5- motors, 6- wires, 7- displays.
Embodiment
The preferred embodiment that the invention will now be described in detail with reference to the accompanying drawings.
The quick determination method of viscosity, this method propose moment of torsion and viscosity in a kind of sizing agent production process of embodiment
Between corresponding relation, reflect the change of viscosity by the change of damping torque, and by a series of experiments determine moment of torsion with
Curvilinear motion between viscosity, so that it is determined that the viscosity B coefficent in current arrangements, then determines the material shape in current reaction vessel
State, a more effective method of testing is provided for the monitoring of production process.
Reactor uses structure as shown in Figure 5 in embodiment, and the kettle top upper end of reactor opens up through hole, built in through hole one
Major axis agitating paddle, major axis agitating paddle includes power transmission shaft 3 and the blade 2 on power transmission shaft 3, and the upper end of major axis agitating paddle passes through magnetic
Property machine envelope be connected with the motor 5 being supported on outside kettle 1, ball valve is set on the through hole of reactor, and torque sensor 4 passes through magnetic machine
Envelope is supported on the upper end of ball valve.Torque sensor 4 is connected with display 7 by wire 6.
The principle of embodiment is：In same reactor, using same sizing agent factory formula, by certain rotation speed operation
Reactor agitator suffered by moment of torsion and the viscosity of material in reactor have direct corresponding relation, material viscosity is bigger,
Suffered moment of torsion is bigger.In starching agent producing process, the sizing agent of same formula is in reactor according to technical recipe
Addition be fixed, i.e., the production capacity of same sizing agent is determined by the volume size of reactor.Same formula is same anti-
The inherent viscosity for answering suitable differential responses stage its time in kettle is close, similar.Based on above reason, the present invention will be viscous
The change of degree is set as judging the leading indicator of reaction end.
Embodiment may not necessarily be using hydromechanical principle be analyzed, to derive reactor agitator as measurement work head
This method in relation formula between different parameter.Embodiment will be adopted experimentally, in sizing agent production process
In not in the same time, according to the one-to-one corresponding data of the practical viscosity numerical value for the torque value and laboratory measurement surveyed so that
Find out its corresponding relation curve.
The quick detection of viscosity in the HS-1 sizing agent production processes of embodiment 1
Determine the torque value that period sample is sampled in sizing agent production process.Using homogeneous raw material, same formula, with all one's life
Production. art produces sizing agent, and the moment of torsion for sampling period sample is determined using the torque sensor built in sizing agent reactor, if
The sample torque value of period is sampled in sizing agent production process to be represented with x, then samples the torque value quantity at least 6 of sample,
Sample interval at least 10 minutes, at most 60 points between wherein phase inversion stage sampling at least two, two neighboring torque value
Clock.The interval time chosen in this example between 10 points, two neighboring sample point is 30 minutes, and particular content is shown in Table 1.
The torque value that the sampling of table 1 period reactor operation interface is shown
| Sample number into spectrum | Torque value/Nm |
| 1 | 175.2 |
| 2 | 191.1 |
| 3 | 246.3 |
| 4 | 312.4 |
| 5 | 365.9 |
| 6 | 376.7 |
| 7 | 318.6 |
| 8 | 251.3 |
| 9 | 213.4 |
| 10 | 142.2 |
Determine the sample viscosity value of sampling period.After sampling, the viscosity number y for sampling period sample is determined using viscosimeter.
Measurement result is shown in Table 2.
Table 2 samples period moment of torsion and sample viscosity
| Sample number into spectrum | Torque value/Nm | Viscosity number/mPas |
| 1 | 175.2 | 2185.2 |
| 2 | 191.1 | 4651.5 |
| 3 | 246.3 | 9665.6 |
| 4 | 312.4 | 12374.7 |
| 5 | 365.9 | 13430.4 |
| 6 | 376.7 | 13652.2 |
| 7 | 318.6 | 10775.4 |
| 8 | 251.3 | 7554.2 |
| 9 | 213.4 | 4675.4 |
| 10 | 142.2 | 421.3 |
The moment of torsion and viscosity number of the sampling period sample of measure are respectively correspondingly inputted into computer, mapping obtain moment of torsion with
The relation curve of viscosity.
It is fitted the moment of torsion of above-mentioned sampling sample and the relation curve of viscosity.It can be obtained by the mechanism of emulsion polymerization, material turns
Viscosity during phase reaches maximum.Above-mentioned relation curve is observed to understand, in the production process of sizing agent, the relation of viscosity and moment of torsion
There are two kinds of variation tendencies in curve.Material occurs before phase inversion, and viscosity tends to after first quick increase is presented with the increase of torque value
Slow phenomenon, after phase inversion adds water, viscosity but reduce with the reduction of torque value.By nonlinear fitting, thing is obtained
The moment of torsion of material and the relation curve of viscosity such as Fig. 1.
Obtain the moment of torsion of material and the relation curve equation of viscosity is：
Before phase inversion：Y=-0.3209*x2+231.1829*x-28117.7594 (1)
After phase inversion：Y=56.5202*x-7304.4111 (2)
Optimize the moment of torsion of material and the relation curve equation of viscosity.First, formula (1) is separately verified related to formula (2)
Coefficients R, by origin nonlinear fitting, the R values of formula (1) and formula (2) are respectively 0.9924,0.9919, meet essence
Degree requires that the fit equation can be used directly.The relation curve equation obtained after optimization is stored in computer.
The test of online viscosity.In sizing agent production process, this is determined by the torque sensor built in reactor
The moment of torsion of period material in reactor, according to the moment of torsion after optimization and the relation curve equation of viscosity, torque value is inputted and calculated
Machine, is converted into the viscosity number output of same period reactor material, so as to monitor the reaction process of the period.Table 3 below is sizing agent
The sample on-line checking result of one group of different sampling period collects in production process.
The measurement result of table 3 is illustrated
| Time domain | Torque value/Nm | Viscosity number/mPas |
| Moment 1 | 180.1 | 3109.5653 |
| Moment 2 | 235.4 | 8520.6122 |
| Moment 3 | 294.6 | 12138.0815 |
| Moment 4 | 327.3 | 13171.8982 |
| Moment 5 | 343.2 | 13426.6075 |
| Moment 6 | 370.9 | 13482.7889 |
| Moment 7 | 381.0 | 13380.7606 |
| Moment 8 | 326.5 | 11149.4342 |
| Moment 9 | 298.4 | 9561.2166 |
| Moment 10 | 214.7 | 4830.4758 |
| Moment 11 | 165.1 | 2027.0739 |
| Moment 12 | 141.0 | 664.9371 |
The quick detection of viscosity in the HS-2 sizing agent production processes of embodiment 2
Determine the torque value that period sample is sampled in sizing agent production process.Using homogeneous raw material, same formula, with all one's life
Production. art produces sizing agent, and the moment of torsion for sampling period sample is determined using the torque sensor built in sizing agent reactor, if
The sample torque value of period is sampled in sizing agent production process to be represented with x, then samples the torque value quantity at least 6 of sample,
Sample interval at least 10 minutes, at most 60 points between wherein phase inversion stage sampling at least two, two neighboring torque value
Clock.The interval time chosen in this example between 15 points, two neighboring sample point is 20 minutes, and particular content is shown in Table 4.
The torque value that the sampling of table 4 period reactor operation interface is shown
| Sample number into spectrum | Torque value/Nm |
| 1 | 123.1 |
| 2 | 134.2 |
| 3 | 172.5 |
| 4 | 217.6 |
| 5 | 261.3 |
| 6 | 303.4 |
| 7 | 337.8 |
| 8 | 359.6 |
| 9 | 379.2 |
| 10 | 357.5 |
| 11 | 321.7 |
| 12 | 247.2 |
| 13 | 203.1 |
| 14 | 174.3 |
| 15 | 119.2 |
Determine the sample viscosity value of sampling period.After sampling, the viscosity number y for sampling period sample is determined using viscosimeter.
Measurement result is shown in Table 5.
Table 5 samples period moment of torsion and sample viscosity
| Sample number into spectrum | Torque value/Nm | Viscosity number/mPas |
| 1 | 123.1 | 513.2 |
| 2 | 134.2 | 1854.9 |
| 3 | 172.5 | 4782.6 |
| 4 | 217.6 | 8213.8 |
| 5 | 261.3 | 10722.4 |
| 6 | 303.4 | 12141.3 |
| 7 | 337.8 | 13167.5 |
| 8 | 359.6 | 13945.2 |
| 9 | 379.2 | 14122.8 |
| 10 | 357.5 | 513.2 |
| 11 | 321.7 | 12930.4 |
| 12 | 247.2 | 11342.6 |
| 13 | 203.1 | 8185.7 |
| 14 | 174.3 | 5268.1 |
| 15 | 119.2 | 3203.5 |
The moment of torsion and viscosity number of the sampling period sample of measure are respectively correspondingly inputted into computer, mapping obtain moment of torsion with
The relation curve of viscosity.
It is fitted the moment of torsion of above-mentioned sampling sample and the relation curve of viscosity.It can be obtained by the mechanism of emulsion polymerization, material turns
Viscosity during phase reaches maximum.Above-mentioned relation curve is observed to understand, in the production process of sizing agent, the relation of viscosity and moment of torsion
There are two kinds of variation tendencies in curve.Material occurs before phase inversion, and viscosity tends to afterwards as the increase of torque value presents first to greatly increase
Slow phenomenon, after phase inversion adds water, viscosity but reduce with the reduction of torque value.By nonlinear fitting, thing is obtained
The moment of torsion of material and the relation curve of viscosity such as Fig. 2.
Obtain the moment of torsion of material and the relation curve equation of viscosity is：
Before phase inversion：Y=-0.1633*x2+134.4311*x-13421.4816 (1)
After phase inversion：Y=52.4013*x-5561.0779 (2)
Optimize the moment of torsion of material and the relation curve equation of viscosity.First, formula (1) is separately verified related to formula (2)
Coefficients R, by origin nonlinear fitting, the R values of formula (1) and formula (2) are respectively 0.9988,0.9929, meet essence
Degree requires that the fit equation can be used directly.The relation curve equation obtained after optimization is stored in computer.
The test of online viscosity.In sizing agent production process, this is determined by the torque sensor built in reactor
The moment of torsion of period material in reactor, according to the moment of torsion after optimization and the relation curve equation of viscosity, torque value is inputted and calculated
Machine, is converted into the viscosity number output of same period reactor material, so as to monitor the reaction process of the period.Table 6 below is sizing agent
The sample on-line checking result of one group of different sampling period collects in production process.
The measurement result of table 6 is illustrated
| Time domain | Torque value/Nm | Viscosity number/mpas |
| Moment 1 | 118.2 | 186.77093 |
| Moment 2 | 192.8 | 6426.67301 |
| Moment 3 | 239.4 | 9402.21535 |
| Moment 4 | 298.1 | 12141.0018 |
| Moment 5 | 324.6 | 13008.72283 |
| Moment 6 | 369.7 | 13958.16397 |
| Moment 7 | 378.2 | 14062.70573 |
| Moment 8 | 384.3 | 14123.18631 |
| Moment 9 | 356.4 | 13114.74542 |
| Moment 10 | 278.5 | 9032.68415 |
| Moment 11 | 211.3 | 5511.31679 |
| Moment 12 | 162.4 | 2948.89322 |
| Moment 13 | 118.9 | 669.43667 |
The quick detection of viscosity in the HS-3 sizing agent production processes of embodiment 3
Determine the torque value that period sample is sampled in sizing agent production process.Using homogeneous raw material, same formula, with all one's life
Production. art produces sizing agent, and the moment of torsion for sampling period sample is determined using the torque sensor built in sizing agent reactor, if
The sample torque value of period is sampled in sizing agent production process to be represented with x, then samples the torque value quantity at least 6 of sample,
Sample interval at least 10 minutes, at most 60 points between wherein phase inversion stage sampling at least two, two neighboring torque value
Clock.The interval time chosen in this example between 7 points, two neighboring sample point is 50 minutes, and particular content is shown in Table 7.
The torque value that the sampling of table 7 period reactor operation interface is shown
| Sample number into spectrum | Torque value/Nm |
| 1 | 211.0 |
| 2 | 256.8 |
| 3 | 323.5 |
| 4 | 381.2 |
| 5 | 308.9 |
| 6 | 231.7 |
| 7 | 122.1 |
Determine the sample viscosity value of sampling period.After sampling, the viscosity number y for sampling period sample is determined using viscosimeter.
Measurement result is shown in Table 8.
Table 8 samples period moment of torsion and sample viscosity
| Sample number into spectrum | Torque value/Nm | Viscosity number/mPas |
| 1 | 211.0 | 4523.5 |
| 2 | 256.8 | 9562.1 |
| 3 | 323.5 | 11499.7 |
| 4 | 381.2 | 14321.6 |
| 5 | 308.9 | 8956.7 |
| 6 | 231.7 | 4624.3 |
| 7 | 122.1 | 256.3 |
The moment of torsion and viscosity number of the sampling period sample of measure are respectively correspondingly inputted into computer, mapping obtain moment of torsion with
The relation curve of viscosity.
It is fitted the moment of torsion of above-mentioned sampling sample and the relation curve of viscosity.It can be obtained by the mechanism of emulsion polymerization, material turns
Viscosity during phase reaches maximum.Above-mentioned relation curve is observed to understand, in the production process of sizing agent, the relation of viscosity and moment of torsion
There are two kinds of variation tendencies in curve.Material occurs before phase inversion, and viscosity tends to afterwards as the increase of torque value presents first to greatly increase
Slow phenomenon, after phase inversion adds water, viscosity but reduce with the reduction of torque value.By nonlinear fitting, thing is obtained
The moment of torsion of material and the relation curve of viscosity such as Fig. 3.
Obtain the moment of torsion of material and the relation curve equation of viscosity is：
Before phase inversion：Y=-0.2148*x2+180.6056*x+23606.2806 (1)
After phase inversion：Y=53.6696*x-6966.6990 (2)
Optimize the moment of torsion of material and the relation curve equation of viscosity.First, formula (1) is separately verified related to formula (2)
Coefficients R, by origin nonlinear fitting, the R values of formula (1) and formula (2) are respectively 0.8897,0.9685, wherein formula
(1) R values are less than 0.9, do not meet required precision, the fit equation is not directly used.
Repeat to increase in above-mentioned torque value determination step, this example the torque value quantity for sampling period sample to 13, phase
Sample interval between adjacent two torque values is reduced to 25 minutes, and particular content is shown in Table 9.
The torque value that the sampling of table 9 period reactor operation interface is shown
| Sample number into spectrum | Torque value/Nm |
| 1 | 211.2 |
| 2 | 237.4 |
| 3 | 265.1 |
| 4 | 295.6 |
| 5 | 337.3 |
| 6 | 371.1 |
| 7 | 381.2 |
| 8 | 369.9 |
| 9 | 321.2 |
| 10 | 275.5 |
| 11 | 224.3 |
| 12 | 176.3 |
| 13 | 122.4 |
Above-mentioned viscosity number determination step is repeated, measurement result is shown in Table 10.
Table 10 samples period moment of torsion and sample viscosity
| Sample number into spectrum | Torque value/Nm | Viscosity number/mPas |
| 1 | 211.2 | 4523.5 |
| 2 | 237.4 | 6968.9 |
| 3 | 265.1 | 8095.6 |
| 4 | 295.6 | 11046.3 |
| 5 | 337.3 | 12996.8 |
| 6 | 371.1 | 13989.5 |
| 7 | 381.2 | 14322.1 |
| 8 | 369.9 | 13656.4 |
| 9 | 321.2 | 10445.8 |
| 10 | 275.5 | 6852.1 |
| 11 | 224.3 | 4486.5 |
| 12 | 176.3 | 1738.4 |
| 13 | 122.4 | 256 |
Repeat above-mentioned mapping and obtain moment of torsion and the relation curve of viscosity and the moment of torsion of fitting sampling sample and the pass of viscosity
It is curve step.By nonlinear fitting, the moment of torsion of material and relation curve such as Fig. 4 of viscosity are obtained.
Obtain the moment of torsion of material and the relation curve equation of viscosity is：
Before phase inversion：Y=-0.1828*x2+166.3129*x-22478.7049 (1)
After phase inversion：Y=56.6970*x-7758.7879 (2)
Repeat the moment of torsion and the relation curve equation step of viscosity of above-mentioned optimization material.First, formula (1) is separately verified
With the coefficient R of formula (2), by origin nonlinear fitting, the R values of formula (1) and formula (2) are respectively 0.9984,
0.9805, meet required precision, the fit equation can be used directly.The relation curve equation obtained after optimization is stored in and calculated
Machine.
10th, the test of online viscosity.In sizing agent production process, this is determined by the torque sensor built in reactor
The moment of torsion of one period material in reactor, according to the moment of torsion after optimization and the relation curve equation of viscosity, torque value is inputted and counted
Calculation machine, is converted into the viscosity number output of same period reactor material, so as to monitor the reaction process of the period.Table 11 below is starching
The sample on-line checking result of one group of different sampling period collects in agent production process.
The measurement result of table 11 is illustrated
| Time domain | Torque value/Nm | Viscosity number/mpas |
| Moment 1 | 210.5 | 4430.2469 |
| Moment 2 | 248.6 | 7569.2838 |
| Moment 3 | 304.1 | 11192.2871 |
| Moment 4 | 356.8 | 13590.1572 |
| Moment 5 | 372.4 | 14105.1933 |
| Moment 6 | 380.1 | 14326.6138 |
| Moment 7 | 364.5 | 12907.2686 |
| Moment 8 | 298.9 | 9187.9454 |
| Moment 9 | 234.3 | 5525.3192 |
| Moment 10 | 187.6 | 2877.5693 |
Claims (4)
1. the detection method of viscosity in a kind of sizing agent production process, it is characterised in that pass through the torque sensing built in reactor
Device measures moment of torsion, while testing the viscosity of the period material, corresponding relation curve, and the side of deriving are made by nonlinear fitting
Formula, and then the viscosity of material at any period is monitored, detecting step is as follows：
Step one, the torque value that period sample is sampled in sizing agent production process is determined；
Step 2, determines the sample viscosity value of sampling period, after sampling, and the viscosity number for sampling period sample is determined using viscosimeter
y；
Step 3, computer is respectively correspondingly inputted by the moment of torsion and viscosity number of the sampling period sample of measure, and mapping is turned round
The relation curve of square and viscosity；
The moment of torsion and the relation curve of viscosity of sampling sample in step 4, fitting above-mentioned steps, can by the mechanism of emulsion polymerization
, viscosity during material phase inversion reaches maximum；Above-mentioned relation curve is observed to understand, in the production process of sizing agent, viscosity with
There are two kinds of variation tendencies in the relation curve of moment of torsion：Material occurs before phase inversion, and viscosity is presented first quick with the increase of torque value
Tend to slow phenomenon, after phase inversion adds water, viscosity after increase but reduce with the reduction of torque value；Pass through Nonlinear Quasi
Close, obtain the moment of torsion of material and the relation curve equation of viscosity is：
Before phase inversion：y=a*x2+b*x+c （1）
After phase inversion：y=d*x+e （2）
Wherein, x represents to sample the sample torque value of period in sizing agent production process；
Step 5, optimizes the moment of torsion of material and the relation curve equation of viscosity；
First, formula is separately verified（1）And formula（2）Coefficient R；By origin nonlinear fitting, if formula（1）With
Formula（2）R>0.9, the fit equation can be used directly；If formula（1）And formula（2）R<0.9, repeat step one, during increase sampling
The torque value quantity of section sample and the sample interval between two neighboring torque value is reduced, retrieve moment of torsion and viscosity
After relation curve, according still further to Step 4: step 5 is fitted and optimized to curve, untill above-mentioned requirements are met；Obtain
The moment of torsion of material after optimization and the relation curve equation of viscosity；
Step 6, the test of online viscosity；When sizing agent is produced, when determining this by the torque sensor built in reactor
The moment of torsion of section material in reactor, it is according to the moment of torsion and the relation curve equation of viscosity after optimization in step 5, torque value is defeated
Enter, the viscosity number output of same period reactor material is converted into, to monitor the reaction process of the period.
2. the detection method of viscosity in sizing agent production process as claimed in claim 1, it is characterised in that step one is specific
For：Sizing agent is produced using homogeneous raw material, same formula, same production technology, the moment of torsion built in sizing agent reactor is used
Sensor determines the moment of torsion of sampling period sample, if the sample torque value that the period is sampled in sizing agent production process is represented with x, then
Sample taking between the torque value quantity at least 6 of sample, wherein phase inversion stage sampling at least two, two neighboring torque value
Sample time interval is 10-60min.
3. the detection method of viscosity in sizing agent production process as claimed in claim 1 or 2, it is characterised in that：Reactor
Kettle top upper end opens up through hole, in a major axis agitating paddle built in through hole, and major axis agitating paddle includes power transmission shaft and on power transmission shaft
Blade, the upper end of major axis agitating paddle is sealed on the motor connection with being supported on outside kettle, the through hole of reactor by magnetic machine and set
Ball valve, torque sensor seals the upper end for being supported on ball valve by magnetic machine.
4. the detection method of viscosity in sizing agent production process as claimed in claim 1 or 2, it is characterised in that：Viscosimeter is adopted
With rotation viscometer or cone and plate viscometer.
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