CN105181526A - Viscosity detection method in sizing agent production process - Google Patents
Viscosity detection method in sizing agent production process Download PDFInfo
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Abstract
The invention provides a viscosity detection method in a sizing agent production process. The method comprises the following steps: measuring the torque through a torque sensor arranged in a reaction kettle, testing the viscosity of a material obtained in the period, carrying out nonlinear fitting to make a corresponding relation curve, and deriving an equation in order to monitor the viscosity of the material in any period. The method allows the viscosity of the material in the reaction kettle in the sizing agent production process to be continuously, rapidly, economically and conveniently determined, overcomes the problems of tedious process, time consumption and low efficiency of traditional test methods, and saves the cost for purchasing an expensive imported online viscometer. The method has the advantages of rapid and continuous determination of the viscosity of the material in the reaction kettle in the sizing agent production process, timely monitoring of the reaction process of the material in the reaction kettle and determination of a reaction end point, facilitation of the improvement of the stability among products in batches, and reduction of the total production cost.
Description
Technical field
The present invention relates to a kind of detection method of sizing agent production run medium viscosity.
Background technology
Carbon fiber is the important component part of advanced composite material, enjoys great prestige in the world with the outstanding advantages of its " height ", " by force ", " light weight ", becomes the preferred material of the industries such as Aero-Space, high-end automobile, high-grade sports goods.Sizing agent is the important component part of carbon fiber, the convergence, wearing quality, pliability, antistatic behaviour etc. of carbon fiber can be improved on the one hand, meet the performance requirement of carbon fiber at composite material manufacturing technologies such as follow-up braiding, preimpregnation, laying, winding, pultrusions.On the other hand, sizing agent is conducive to the wellability strengthening carbon fiber and matrix resin, improves the interfacial adhesion between carbon fiber and matrix resin, improves compound substance interlayer shear resistance.
In the production run of sizing agent, often monitoring method is not fast and accurately had to reaction process.In general two kinds of methods are mainly contained:
A kind of is estimate judgement by the technician with certain working experience according to the time etc. of the material state in reaction vessel and reaction.The maximum advantage of this kind of method is the speed of " monitoring ", also obviously can not affect the process of material change in reaction vessel.But the shortcoming of this method is also apparent, the judgement of different technician to reaction process there are differences, and subjective consciousness is comparatively strong, runs counter to the regulation of quality system management, affects the quality of final products to a certain extent.
Another kind method is in the production run of sizing agent, is taken out by material in reaction vessel, tests the performance of its key, such as viscosity and epoxide equivalent etc.The advantage of this kind of method is can quantitative test These parameters, as the foundation judging reaction process.But its shortcoming be have ignored sizing agent produce be a continuous print process, and test needs the time, therefore can not the instantaneous state of reaction mass really, particularly in mass production process, the method receives the restriction of all many condition, is of limited application.
So, need the effective monitoring method setting up a kind of sizing agent reaction process badly, thus ensure the stable of end product quality, also can reduce production cost simultaneously, improve productivity effect.
Viscosity weighs the important physical parameter of liquid opposing fluid ability.In the field such as physical chemistry and fluid mechanics, viscosity measurement is the means of the relative efficiency of industrial stokehold.Same viscosity also can reflect the reaction process of material in the production run of sizing agent.Mentioned the method for testing of viscosity in above-mentioned, obviously in actual production, feasibility is strong, and the method for more enterprise or choice for use range estimation judges reaction process.
Summary of the invention
The object of the invention is to propose a kind of continuous, quick, economical, detection method easily of sizing agent production run medium viscosity, overcome the loaded down with trivial details, time-consuming and inefficient of conventional test methodologies, save the funds buying expensive import in-line viscometer simultaneously.
Method provided by the invention can reflect the material viscosity in sizing agent production run, thus monitor the reaction process of material in reactor and determine reaction end, to carry out quality control more accurately, improve the stability of the product quality of sizing agent, reduce production cost.
Technical solution of the present invention is:
A kind of detection method of sizing agent production run medium viscosity, moment of torsion measured by the torque sensor built-in by reactor, test the viscosity of this period material simultaneously, corresponding relation curve is made by nonlinear fitting, and derive equation, and then the viscosity of monitoring material when section in office, detecting step is as follows:
Step one, measures the torque value sampling period sample in sizing agent production run;
Step 2, measures the sample viscosity value of sampling period, after sampling, uses the viscosity number y of viscometer determining sampling period sample;
Step 3, inputs computing machine respectively accordingly by the moment of torsion of the sampling period sample of mensuration and viscosity number, and mapping obtains the relation curve of moment of torsion and viscosity;
Step 4, samples the moment of torsion of sample and the relation curve of viscosity in matching above-mentioned steps, can be obtained by the mechanism of emulsion polymerization, viscosity during material phase inversion reaches maximum; Observe above-mentioned relation curve known, in the production run of sizing agent, there are two kinds of variation tendencies in the relation curve of viscosity and moment of torsion: before material generation phase inversion, viscosity is tending towards phenomenon slowly after first increasing fast along with the increase of torque value presents, after phase inversion adds water, but viscosity reduces along with the reduction of torque value; By nonlinear fitting, the relation curve equation of the moment of torsion and viscosity that obtain material is:
Before phase inversion: y=a*x
2+ 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 difference verification expression (1) and formula (2); Known by the nonlinear fitting of origin, if the R>0.9 of formula (1) and formula (2), this fit equation can directly use; If the R<0.9 of formula (1) and formula (2), repeat step, the torque value quantity increasing sampling period sample and the sample interval of reducing between adjacent two torque values, again after obtaining the relation curve of moment of torsion and viscosity, according to step 4, step 5, matching and optimization are carried out, till meeting above-mentioned requirements to curve again; The moment of torsion of the material after being optimized and the relation curve equation of viscosity;
Step 6, the test of online viscosity; When sizing agent is produced, the moment of torsion of this period material in reactor is measured by the torque sensor that reactor is built-in, according to the moment of torsion after optimizing in step 5 and the relation curve equation of viscosity, torque value is inputted, the viscosity number converting same period reactor material to exports, and monitors the reaction process of this period.
Further, step one is specially: adopt homogeneous raw material, same formula, same production technology to produce sizing agent, the torque sensor using sizing agent reactor built-in measures the moment of torsion of sampling period sample, if the sample torque value x sampling the period in sizing agent production run represents, the torque value quantity then sampling sample has 6 at least, wherein phase inversion stage sampling at least two, the sample interval between adjacent two torque values is 10-60min.
Further, through hole is offered in the upper end, still top of reactor, at the built-in major axis paddle of through hole, major axis paddle comprises transmission shaft and is located at the blade on transmission shaft, the upper end of major axis paddle is connected with the motor be supported on outside kettle by magnetic machine envelope, the through hole of reactor arranges ball valve, and torque sensor is supported on the upper end of ball valve by magnetic machine envelope.
Further, viscosity meter adopts rotational viscosimeter or cone-and-plate viscometer.
The invention has the beneficial effects as follows:
One, this method of testing is simple and convenient, and do not have complicated parts, cost can be ignored substantially;
Two, the viscosity of material in reactor in sizing agent production run can be determined rapidly, continuously, in time monitoring material in reactor reaction process and determine reaction end, be conducive to the stability between improving product batch;
Three, improve the product quality of sizing agent, ensure the stable of product quality, indirectly reduce total production cost simultaneously.
Accompanying drawing explanation
Fig. 1 is the moment of torsion of material and the graph of relation of viscosity in embodiment one.
Fig. 2 is the moment of torsion of material and the relation curve of viscosity in embodiment two.
Fig. 3 is the moment of torsion of material and the relation curve of viscosity in embodiment three.
Fig. 4 is the moment of torsion of material and the relation curve of viscosity in embodiment four.
Fig. 5 is the structural representation of reactor in embodiment.
Wherein: 1-kettle, 2-blade, 3-transmission shaft, 4-torque sensor, 5-motor, 6-wire, 7-display.
Embodiment
The preferred embodiments of the present invention are described in detail below in conjunction with accompanying drawing.
The method for quick of a kind of sizing agent production run medium viscosity of embodiment, this method propose the corresponding relation between moment of torsion and viscosity, the change of viscosity is reflected by the change of damping torque, and the curvilinear motion through between series of experiments determination moment of torsion and viscosity, thus determine the viscosity B coefficent in current arrangements, then determine the material state in current reaction vessel, the monitoring for production process provides a comparatively effective method of testing.
In embodiment, reactor adopts structure as shown in Figure 5, through hole is offered in the upper end, still top of reactor, at the built-in major axis paddle of through hole, the blade 2 that major axis paddle comprises transmission shaft 3 and is located on transmission shaft 3, the upper end of major axis paddle is connected with the motor 5 be supported on outside kettle 1 by magnetic machine envelope, the through hole of reactor arranges ball valve, and torque sensor 4 is supported on the upper end of ball valve by magnetic machine envelope.Torque sensor 4 is connected with display 7 by wire 6.
The principle of embodiment is: in same reactor, adopt same sizing agent factory formula, by certain rotation speed operation reactor stirrer suffered by moment of torsion and the viscosity of material in reactor have direct corresponding relation, material viscosity is larger, and suffered moment of torsion is larger.In sizing agent production technology, the sizing agent of same formula is fixing according to the addition of technical recipe in reactor, and namely the production capacity of same sizing agent is determined by the volume size of reactor.The limiting viscosity in the differential responses stage that same formula its time in same reactor is suitable is close, similar.Based on above reason, the change of viscosity is set as the leading indicator judging reaction end by the present invention.
Embodiment can utilize the principle of analysing fluid mechanics, and reactor stirrer of deriving is as the relation formula between parameters different in this method of surveying work head.Embodiment will be adopted experimentally, in sizing agent production run not in the same time, according to the one_to_one corresponding data of the practical viscosity numerical value of surveyed torque value and laboratory measurement, thus find out its corresponding relation curve.
The quick detection of embodiment 1HS-1 sizing agent production run medium viscosity
Measure the torque value sampling period sample in sizing agent production run.Homogeneous raw material, same formula, same production technology is adopted to produce sizing agent, the torque sensor using sizing agent reactor built-in measures the moment of torsion of sampling period sample, if the sample torque value x sampling the period in sizing agent production run represents, the torque value quantity then sampling sample has 6 at least, wherein phase inversion stage sampling at least two, at least 10 minutes, sample interval between adjacent two torque values, 60 minutes at the most.Choose 10 points in this example, the interval time between adjacent two sampling spots is 30 minutes, and particular content is in table 1.
Table 1 samples the torque value of period reactor operation interface display
| 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 |
Measure the sample viscosity value of sampling period.After sampling, use the viscosity number y of viscometer determining sampling period sample.Measurement result is 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 of the sampling period sample of mensuration and viscosity number are inputted computing machine respectively accordingly, and mapping obtains the relation curve of moment of torsion and viscosity.
The above-mentioned moment of torsion of sampling sample of matching and the relation curve of viscosity.Can be obtained by the mechanism of emulsion polymerization, viscosity during material phase inversion reaches maximum.Observe above-mentioned relation curve known, in the production run of sizing agent, there are two kinds of variation tendencies in the relation curve of viscosity and moment of torsion.Before material generation phase inversion, viscosity is tending towards phenomenon slowly after first increasing fast along with the increase of torque value presents, and after phase inversion adds water, but viscosity reduces along with the reduction of torque value.By nonlinear fitting, the relation curve of the moment of torsion and viscosity that obtain material is as Fig. 1.
The relation curve equation of the moment of torsion and viscosity that obtain material is:
Before phase inversion: y=-0.3209*x
2+ 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, the coefficient R of verification expression (1) and formula (2) respectively, known by the nonlinear fitting of origin, the R value of formula (1) and formula (2) is respectively 0.9924,0.9919, meet accuracy requirement, this fit equation can directly use.By the relation curve equation that obtains after optimizing stored in computing machine.
The test of online viscosity.In sizing agent production run, the moment of torsion of this period material in reactor is measured by the torque sensor that reactor is built-in, according to the moment of torsion after optimizing and the relation curve equation of viscosity, torque value is inputted computing machine, the viscosity number converting same period reactor material to exports, thus monitors the reaction process of this period.Following table 3 is that the sample on-line checkingi result of one group of different sampling period in sizing agent production run gathers.
Table 3 measurement result is illustrated
| Time numbers | 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 embodiment 2HS-2 sizing agent production run medium viscosity
Measure the torque value sampling period sample in sizing agent production run.Homogeneous raw material, same formula, same production technology is adopted to produce sizing agent, the torque sensor using sizing agent reactor built-in measures the moment of torsion of sampling period sample, if the sample torque value x sampling the period in sizing agent production run represents, the torque value quantity then sampling sample has 6 at least, wherein phase inversion stage sampling at least two, at least 10 minutes, sample interval between adjacent two torque values, 60 minutes at the most.Choose 15 points in this example, the interval time between adjacent two sampling spots is 20 minutes, and particular content is in table 4.
Table 4 samples the torque value of period reactor operation interface display
| 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 |
Measure the sample viscosity value of sampling period.After sampling, use the viscosity number y of viscometer determining sampling period sample.Measurement result is 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 of the sampling period sample of mensuration and viscosity number are inputted computing machine respectively accordingly, and mapping obtains the relation curve of moment of torsion and viscosity.
The above-mentioned moment of torsion of sampling sample of matching and the relation curve of viscosity.Can be obtained by the mechanism of emulsion polymerization, viscosity during material phase inversion reaches maximum.Observe above-mentioned relation curve known, in the production run of sizing agent, there are two kinds of variation tendencies in the relation curve of viscosity and moment of torsion.Before material generation phase inversion, viscosity is tending towards phenomenon slowly after first greatly increasing along with the increase of torque value presents, and after phase inversion adds water, but viscosity reduces along with the reduction of torque value.By nonlinear fitting, the relation curve of the moment of torsion and viscosity that obtain material is as Fig. 2.
The relation curve equation of the moment of torsion and viscosity that obtain material is:
Before phase inversion: y=-0.1633*x
2+ 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, the coefficient R of verification expression (1) and formula (2) respectively, known by the nonlinear fitting of origin, the R value of formula (1) and formula (2) is respectively 0.9988,0.9929, meet accuracy requirement, this fit equation can directly use.By the relation curve equation that obtains after optimizing stored in computing machine.
The test of online viscosity.In sizing agent production run, the moment of torsion of this period material in reactor is measured by the torque sensor that reactor is built-in, according to the moment of torsion after optimizing and the relation curve equation of viscosity, torque value is inputted computing machine, the viscosity number converting same period reactor material to exports, thus monitors the reaction process of this period.Following table 6 is that the sample on-line checkingi result of one group of different sampling period in sizing agent production run gathers.
Table 6 measurement result is illustrated
| Time numbers | 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 embodiment 3HS-3 sizing agent production run medium viscosity
Measure the torque value sampling period sample in sizing agent production run.Homogeneous raw material, same formula, same production technology is adopted to produce sizing agent, the torque sensor using sizing agent reactor built-in measures the moment of torsion of sampling period sample, if the sample torque value x sampling the period in sizing agent production run represents, the torque value quantity then sampling sample has 6 at least, wherein phase inversion stage sampling at least two, at least 10 minutes, sample interval between adjacent two torque values, 60 minutes at the most.Choose 7 points in this example, the interval time between adjacent two sampling spots is 50 minutes, and particular content is in table 7.
Table 7 samples the torque value of period reactor operation interface display
| 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 |
Measure the sample viscosity value of sampling period.After sampling, use the viscosity number y of viscometer determining sampling period sample.Measurement result is 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 of the sampling period sample of mensuration and viscosity number are inputted computing machine respectively accordingly, and mapping obtains the relation curve of moment of torsion and viscosity.
The above-mentioned moment of torsion of sampling sample of matching and the relation curve of viscosity.Can be obtained by the mechanism of emulsion polymerization, viscosity during material phase inversion reaches maximum.Observe above-mentioned relation curve known, in the production run of sizing agent, there are two kinds of variation tendencies in the relation curve of viscosity and moment of torsion.Before material generation phase inversion, viscosity is tending towards phenomenon slowly after first greatly increasing along with the increase of torque value presents, and after phase inversion adds water, but viscosity reduces along with the reduction of torque value.By nonlinear fitting, the relation curve of the moment of torsion and viscosity that obtain material is as Fig. 3.
The relation curve equation of the moment of torsion and viscosity that obtain material is:
Before phase inversion: y=-0.2148*x
2+ 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, the coefficient R of verification expression (1) and formula (2) respectively, known by the nonlinear fitting of origin, the R value of formula (1) and formula (2) is respectively 0.8897,0.9685, the R value of its Chinese style (1) is less than 0.9, do not meet accuracy requirement, this fit equation not directly uses.
Repeat above-mentioned torque value determination step, increase the torque value quantity to 13 of sampling period sample in this example, the sample interval between adjacent two torque values is reduced to 25 minutes, and particular content is in table 9.
Table 9 samples the torque value of period reactor operation interface display
| 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 |
Repeat above-mentioned viscosity number determination step, measurement result is 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 the relation curve of moment of torsion and viscosity and matching samples the moment of torsion of sample and the relation curve step of viscosity.By nonlinear fitting, the relation curve of the moment of torsion and viscosity that obtain material is as Fig. 4.
The relation curve equation of the moment of torsion and viscosity that obtain material is:
Before phase inversion: y=-0.1828*x
2+ 166.3129*x-22478.7049 (1)
After phase inversion: y=56.6970*x-7758.7879 (2)
Repeat the moment of torsion of above-mentioned optimization material and the relation curve equation step of viscosity.First, the coefficient R of verification expression (1) and formula (2) respectively, known by the nonlinear fitting of origin, the R value of formula (1) and formula (2) is respectively 0.9984,0.9805, meet accuracy requirement, this fit equation can directly use.By the relation curve equation that obtains after optimizing stored in computing machine.
10, the test of online viscosity.In sizing agent production run, the moment of torsion of this period material in reactor is measured by the torque sensor that reactor is built-in, according to the moment of torsion after optimizing and the relation curve equation of viscosity, torque value is inputted computing machine, the viscosity number converting same period reactor material to exports, thus monitors the reaction process of this period.Following table 11 is that the sample on-line checkingi result of one group of different sampling period in sizing agent production run gathers.
Table 11 measurement result is illustrated
| Time numbers | 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 a sizing agent production run medium viscosity, it is characterized in that, moment of torsion measured by the torque sensor built-in by reactor, test the viscosity of this period material simultaneously, corresponding relation curve is made by nonlinear fitting, and derive equation, and then the viscosity of monitoring material when section in office, detecting step is as follows:
Step one, measures the torque value sampling period sample in sizing agent production run;
Step 2, measures the sample viscosity value of sampling period, after sampling, uses the viscosity number y of viscometer determining sampling period sample;
Step 3, inputs computing machine respectively accordingly by the moment of torsion of the sampling period sample of mensuration and viscosity number, and mapping obtains the relation curve of moment of torsion and viscosity;
Step 4, samples the moment of torsion of sample and the relation curve of viscosity in matching above-mentioned steps, can be obtained by the mechanism of emulsion polymerization, viscosity during material phase inversion reaches maximum; Observe above-mentioned relation curve known, in the production run of sizing agent, there are two kinds of variation tendencies in the relation curve of viscosity and moment of torsion: before material generation phase inversion, viscosity is tending towards phenomenon slowly after first increasing fast along with the increase of torque value presents, after phase inversion adds water, but viscosity reduces along with the reduction of torque value; By nonlinear fitting, the relation curve equation of the moment of torsion and viscosity that obtain material is:
Before phase inversion: y=a*x
2+ 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 difference verification expression (1) and formula (2); Known by the nonlinear fitting of origin, if the R>0.9 of formula (1) and formula (2), this fit equation can directly use; If the R<0.9 of formula (1) and formula (2), repeat step, the torque value quantity increasing sampling period sample and the sample interval of reducing between adjacent two torque values, again after obtaining the relation curve of moment of torsion and viscosity, according to step 4, step 5, matching and optimization are carried out, till meeting above-mentioned requirements to curve again; The moment of torsion of the material after being optimized and the relation curve equation of viscosity;
Step 6, the test of online viscosity; When sizing agent is produced, the moment of torsion of this period material in reactor is measured by the torque sensor that reactor is built-in, according to the moment of torsion after optimizing in step 5 and the relation curve equation of viscosity, torque value is inputted, the viscosity number converting same period reactor material to exports, and monitors the reaction process of this period.
2. the detection method of sizing agent production run medium viscosity as claimed in claim 1, it is characterized in that, step one is specially: adopt homogeneous raw material, same formula, same production technology to produce sizing agent, the torque sensor using sizing agent reactor built-in measures the moment of torsion of sampling period sample, if the sample torque value x sampling the period in sizing agent production run represents, the torque value quantity then sampling sample has 6 at least, wherein phase inversion stage sampling at least two, the sample interval between adjacent two torque values is 10-60min.
3. the detection method of sizing agent production run medium viscosity as claimed in claim 1 or 2, it is characterized in that: through hole is offered in the upper end, still top of reactor, at the built-in major axis paddle of through hole, major axis paddle comprises transmission shaft and is located at the blade on transmission shaft, the upper end of major axis paddle is connected with the motor be supported on outside kettle by magnetic machine envelope, the through hole of reactor arranges ball valve, and torque sensor is supported on the upper end of ball valve by magnetic machine envelope.
4. the detection method of sizing agent production run medium viscosity as claimed in claim 1 or 2, is characterized in that: viscosity meter adopts rotational viscosimeter or cone-and-plate viscometer.
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