CN101762639A - Mixed state ultrasound on-line monitoring method in polymer production process - Google Patents

Mixed state ultrasound on-line monitoring method in polymer production process Download PDF

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CN101762639A
CN101762639A CN201010000080A CN201010000080A CN101762639A CN 101762639 A CN101762639 A CN 101762639A CN 201010000080 A CN201010000080 A CN 201010000080A CN 201010000080 A CN201010000080 A CN 201010000080A CN 101762639 A CN101762639 A CN 101762639A
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polymer
amplitude
ultrasonic
temperature
mixed state
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王召巴
陈友兴
赵霞
邢巍
金永
肖凯生
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North University of China
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Abstract

本发明公开了一种聚合物生产过程中混合状态超声在线监测方法,属于工业检测技术领域。本发明通过安装在单螺杆或双螺杆挤出机上的超声传感器实时获取反映聚合物混合状态的超声回波信号的振幅;使用对应位置的温度压力传感器获取的机筒内熔态聚合物的温度和压力作为参考量,采用秩滤波和低通滤波方法校正并归一化回波振幅;运用相关系数匹配方法完成振幅曲线不同周期间的位置匹配;计算不同周期间对应位置的超声回波振幅偏差,通过振幅与聚合物含量的关系,识别聚合物的混合状态;该方法能够实时在线监测聚合物挤出过程中的混合状态,为聚合物的产品质量和工艺调整提供状态参数。The invention discloses an ultrasonic on-line monitoring method for a mixed state in a polymer production process, belonging to the technical field of industrial detection. The present invention obtains the amplitude of the ultrasonic echo signal reflecting the mixing state of the polymer in real time through the ultrasonic sensor installed on the single-screw or twin-screw extruder; the temperature and temperature of the molten polymer in the barrel obtained by using the temperature and pressure sensor at the corresponding position Pressure is used as a reference quantity, and the echo amplitude is corrected and normalized by rank filtering and low-pass filtering methods; the correlation coefficient matching method is used to complete the position matching of the amplitude curve in different periods; the ultrasonic echo amplitude deviation of the corresponding position in different periods is calculated, Through the relationship between the amplitude and the polymer content, the mixing state of the polymer can be identified; this method can monitor the mixing state of the polymer in the process of extrusion in real time, and provide state parameters for the product quality and process adjustment of the polymer.

Description

聚合物生产过程中混合状态超声在线监测方法 Ultrasonic on-line monitoring method of mixing state in polymer production process

技术领域:本发明属于工业检测技术领域,具体涉及一种聚合物生产过程中混合状态超声在线监测方法。Technical field: the invention belongs to the technical field of industrial detection, and specifically relates to an ultrasonic on-line monitoring method of the mixing state in the polymer production process.

背景技术:Background technique:

聚合物共混物是由两种或两种以上的均聚物或共聚物的混合而成,由于其性能优越,已成为国民经济及国防领域不可缺少的一类重要材料。聚合物的共混加工方法主要是通过单(双)螺杆挤出机进行混合。固态聚合物由进料口进入,在螺杆挤出机机筒内由固态变成熔融态,由挤出机出料口挤出进入成型磨具。最终挤出产品的质量与原材料的性能配比、机筒内温度压力、挤出机螺杆转速、螺杆结构等因素有关,同时在生产过程中也体现为混合物在螺杆挤出机机筒中不同部位的混合状态。因此在生产过程中对聚合物混合过程状态的在线检测具有重要意义,可以利用检测结果及时调整生产工艺,减少产品浪费和废品污染,加快产品生产周期。Polymer blends are a mixture of two or more homopolymers or copolymers. Due to their superior performance, they have become an indispensable class of important materials in the fields of national economy and national defense. The blending processing method of the polymer is mainly to mix through a single (twin) screw extruder. The solid polymer enters from the feed port, changes from solid to molten state in the barrel of the screw extruder, and is extruded from the discharge port of the extruder into the molding tool. The quality of the final extruded product is related to the performance ratio of raw materials, the temperature and pressure in the barrel, the screw speed of the extruder, the screw structure and other factors, and it is also reflected in the different parts of the mixture in the screw extruder barrel during the production process mixed state. Therefore, in the production process, the online detection of the state of the polymer mixing process is of great significance. The detection results can be used to adjust the production process in time, reduce product waste and waste pollution, and speed up the product production cycle.

目前聚合物生产线上主要通过监测机筒内的温度和压力来指导生产,而获取混合状态信息的方法都是离线的,如对通过安装在不同部位的特殊的样品采集器获得的混合样品进行理化分析、通过安装在挤出机上的玻璃窗观察混合过程等。这些方法均不能实时、准确的给出混合信息,不能满足生产的需要,严重制约了我国聚合物加工产业的发展。At present, the polymer production line mainly guides the production by monitoring the temperature and pressure in the barrel, and the methods of obtaining the mixing state information are offline, such as performing physical and chemical analysis on the mixed samples obtained through special sample collectors installed in different parts. analysis, observation of the mixing process through glass windows installed on the extruder, etc. None of these methods can give real-time and accurate mixing information, and cannot meet the needs of production, which seriously restricts the development of my country's polymer processing industry.

超声检测技术采用超声波在穿透共混聚合物熔体时,其回波振幅、声速、衰减系数和声阻抗将随共混物的熔融状态而变化,这一原理可用于聚合物在螺杆挤压过程中不同位置处的混合状态检测。聚合物混合时,其在挤出机中的熔融态温度一般在100℃以上,而一般超声探头只能在常温下工作,影响超声技术在这方面的应用。Ultrasonic testing technology uses ultrasonic waves to penetrate the blended polymer melt, and its echo amplitude, sound velocity, attenuation coefficient and acoustic impedance will change with the melting state of the blend. This principle can be used for polymers in screw extrusion. Mixed state detection at different locations in the process. When polymers are mixed, their molten state temperature in the extruder is generally above 100°C, while general ultrasonic probes can only work at room temperature, which affects the application of ultrasonic technology in this area.

发明内容:Invention content:

本发明目的在于提供一种聚合物生产过程中混合状态超声在线监测方法,采用该方法能够在聚合物挤出生产线上实现对聚合物在挤出机中不同部位的混合状态进行实时监测、状态识别和生产分析等功能。The purpose of the present invention is to provide an ultrasonic on-line monitoring method of the mixing state in the polymer production process, which can realize real-time monitoring and state identification of the mixing state of the polymer in different parts of the extruder on the polymer extrusion production line and production analysis.

本发明提供的聚合物生产过程中混合状态超声在线监测方法,其特征在于:通过安装在单螺杆或双螺杆挤出机上的超声传感器实时获取反映聚合物混合状态的超声回波信号的振幅;使用对应位置的温度压力传感器获取的机筒内熔态聚合物的温度和压力作为参考量,采用秩滤波和低通滤波方法校正并归一化回波振幅;运用相关系数匹配方法完成振幅曲线不同周期间的位置匹配;计算不同周期间对应位置的超声回波振幅偏差,通过振幅与聚合物含量的关系,识别聚合物的混合状态。The ultrasonic on-line monitoring method of the mixing state in the polymer production process provided by the present invention is characterized in that: the amplitude of the ultrasonic echo signal reflecting the mixing state of the polymer is obtained in real time through an ultrasonic sensor installed on a single-screw or twin-screw extruder; The temperature and pressure of the molten polymer in the barrel obtained by the temperature and pressure sensor at the corresponding position are taken as a reference, and the echo amplitude is corrected and normalized by using the rank filtering and low-pass filtering methods; Position matching during the period; calculate the amplitude deviation of the ultrasonic echo at the corresponding position during different periods, and identify the mixing state of the polymer through the relationship between the amplitude and the polymer content.

可以根据现场的监测需求,分别在螺杆挤出机上不同部位安装温度压力传感器和超声传感器,同时监测多个部位的聚合物混合状态,实现聚合物混合过程的监测。According to on-site monitoring requirements, temperature and pressure sensors and ultrasonic sensors can be installed on different parts of the screw extruder to monitor the polymer mixing status of multiple parts at the same time, so as to realize the monitoring of the polymer mixing process.

所说的超声传感器由超声探头、声波耦合杆和水冷装置组成;超声探头的中心频率为2.5MHz,激励脉冲宽度为1μs;声波耦合杆以聚醚醚酮为材料,主体部分为圆柱结构,采用螺纹结构与螺杆挤出机机筒紧密连接,顶端与超声探头粘接接触,底端与挤出机机筒内壁相切;水冷装置中的恒温水与声波耦合杆充分接触。The ultrasonic sensor is composed of an ultrasonic probe, an acoustic coupling rod and a water cooling device; the center frequency of the ultrasonic probe is 2.5 MHz, and the excitation pulse width is 1 μs; the acoustic coupling rod is made of polyether ether ketone, and the main part is a cylindrical structure. The thread structure is closely connected with the screw extruder barrel, the top end is in adhesive contact with the ultrasonic probe, and the bottom end is tangent to the inner wall of the extruder barrel; the constant temperature water in the water cooling device is fully in contact with the acoustic wave coupling rod.

本发明的有益效果:Beneficial effects of the present invention:

(1)利用超声回波幅值、机筒内聚合物的压力和温度,在线监测机筒内不同部位聚合物的混合状态,不受人主观因素的影响,起到及时指导和调整生产工艺的作用,有效地提高生产效率,缩短新产品的研发周期。(1) Use the ultrasonic echo amplitude, the pressure and temperature of the polymer in the barrel to monitor the mixing state of the polymer in different parts of the barrel online, without being affected by human subjective factors, and play a role in timely guiding and adjusting the production process It can effectively improve production efficiency and shorten the research and development cycle of new products.

(2)超声传感器带有水冷装置和螺纹安装结构,适用于聚合物在生产挤出过程中的高温高压环境下工作;(2) The ultrasonic sensor has a water cooling device and a threaded installation structure, which is suitable for working in a high temperature and high pressure environment during the production and extrusion of polymers;

(3)声波耦合杆采用聚醚醚酮为材料,提高了声波在耦合杆与聚合物界面的透射率,有效地抑制了超声波在圆柱杆中传播的尾随噪声,提高了特征回波的信噪比;(3) The acoustic wave coupling rod is made of polyether ether ketone, which improves the transmittance of the sound wave at the interface between the coupling rod and the polymer, effectively suppresses the trailing noise of the ultrasonic wave propagating in the cylindrical rod, and improves the signal-to-noise of the characteristic echo Compare;

(4)声波耦合杆底端与机筒内壁相切,可在不影响聚合物挤出机正常工作情况下,准确监测聚合物的混合状态;(4) The bottom end of the acoustic wave coupling rod is tangent to the inner wall of the barrel, which can accurately monitor the mixing state of the polymer without affecting the normal operation of the polymer extruder;

(5)采用不同周期间同一位置的超声回波偏差作为特征量,有效的避免了由于螺杆结构造成的影响;(5) Using the ultrasonic echo deviation at the same position in different cycles as the characteristic quantity, effectively avoiding the influence caused by the screw structure;

(6)使用熔态聚合物的温度和压力为参考量,采用秩滤波和低通滤波方法校正并归一化超声回波振幅,避免由于熔态聚合物的温度和压力对超声回波信号的影响;(6) Using the temperature and pressure of the molten polymer as a reference, the rank filtering and low-pass filtering methods are used to correct and normalize the ultrasonic echo amplitude, so as to avoid the influence of the temperature and pressure of the molten polymer on the ultrasonic echo signal. Influence;

(7)使用相关系数匹配方法完成振幅曲线不同周期间的位置匹配,避免了由于螺杆转速不匀造成采样点与螺杆位置的偏差影响对应位置的准确比较;(7) Use the correlation coefficient matching method to complete the position matching during different periods of the amplitude curve, avoiding the accurate comparison of the corresponding position due to the deviation of the sampling point and the screw position caused by the uneven screw speed;

(8)结合信号处理技术和工业控制技术,可以达到实时监测聚合物混合过程多个不同部位的混合状态,易于扩展;可以对监测数据进行保存、显示和分析,适用于聚合物新产品研发的应用。(8) Combined with signal processing technology and industrial control technology, it can achieve real-time monitoring of the mixing state of multiple different parts of the polymer mixing process, which is easy to expand; it can save, display and analyze the monitoring data, which is suitable for the development of new polymer products. application.

附图说明:Description of drawings:

图1为传感器安装位置图;Figure 1 is a diagram of the sensor installation location;

图1中,(1a)传感器安装正视图,(1b)传感器安装处的周向截面图;In Fig. 1, (1a) sensor installation front view, (1b) circumferential sectional view of sensor installation place;

图2为超声波在聚合物中的传播和回波示意图;Fig. 2 is the propagation and echo schematic diagram of ultrasonic wave in polymer;

图2中,(2a)传播原理示意图,(2b)超声回波示意图;In Fig. 2, (2a) schematic diagram of propagation principle, (2b) schematic diagram of ultrasonic echo;

图3为超声传感器特征回波信号的B扫描图;Fig. 3 is the B-scan diagram of ultrasonic sensor characteristic echo signal;

图3中,(3a)位置I,(3b)位置II,(3c)位置III,(3d)位置IV;In Fig. 3, (3a) position I, (3b) position II, (3c) position III, (3d) position IV;

图4为特征信号幅值偏差柱状图;Fig. 4 is a histogram of characteristic signal amplitude deviation;

具体实现方式:The specific implementation method:

本发明以超声回波特征量来表征聚合物混合状态信息,结合挤出机机筒内的温度、压力,通过信号处理方法,采用计算机的处理技术,实现实时在线监测聚合物在生产挤出过程中的混合状态。The present invention uses ultrasonic echo feature quantity to characterize polymer mixing state information, combined with temperature and pressure in extruder barrel, through signal processing method, adopts computer processing technology, realizes real-time on-line monitoring of polymer in production extrusion process mixed state in .

聚合物生产过程中混合状态超声在线监测方法,通过安装在单螺杆或双螺杆挤出机上的超声传感器实时获取反映聚合物混合状态的超声回波信号的振幅;使用对应位置的温度压力传感器获取的机筒内熔态聚合物的温度和压力作为参考量,采用秩滤波和低通滤波方法校正并归一化回波振幅;运用相关系数匹配方法完成振幅曲线不同周期间的位置匹配;计算不同周期间对应位置的超声回波振幅偏差,通过振幅与聚合物含量的关系,识别聚合物的混合状态。The ultrasonic on-line monitoring method of the mixing state in the polymer production process obtains the amplitude of the ultrasonic echo signal reflecting the mixing state of the polymer in real time through the ultrasonic sensor installed on the single-screw or twin-screw extruder; the temperature and pressure sensor obtained by using the corresponding position The temperature and pressure of the molten polymer in the barrel are used as reference quantities, and the echo amplitude is corrected and normalized by rank filtering and low-pass filtering methods; the correlation coefficient matching method is used to complete the position matching of the amplitude curve in different periods; During the period, the ultrasonic echo amplitude deviation at the corresponding position can be used to identify the mixing state of the polymer through the relationship between the amplitude and the polymer content.

根据现场的监测需求,分别在螺杆挤出机上不同部位安装温度压力传感器和超声传感器,同时监测多个部位的聚合物混合状态,实现聚合物混合过程的监测。According to on-site monitoring requirements, temperature and pressure sensors and ultrasonic sensors are installed on different parts of the screw extruder to monitor the polymer mixing status of multiple parts at the same time, so as to realize the monitoring of the polymer mixing process.

所说的超声传感器由超声探头、声波耦合杆和水冷装置组成;超声探头的中心频率为2.5MHz,激励脉冲宽度为1μs;声波耦合杆以聚醚醚酮为材料,主体部分为圆柱结构,采用螺纹结构与螺杆挤出机机筒紧密连接,顶端与超声探头粘接接触,底端与挤出机机筒内壁相切;水冷装置中的恒温水与声波耦合杆充分接触。The ultrasonic sensor is composed of an ultrasonic probe, an acoustic coupling rod and a water cooling device; the center frequency of the ultrasonic probe is 2.5 MHz, and the excitation pulse width is 1 μs; the acoustic coupling rod is made of polyether ether ketone, and the main part is a cylindrical structure. The thread structure is closely connected with the screw extruder barrel, the top end is in adhesive contact with the ultrasonic probe, and the bottom end is tangent to the inner wall of the extruder barrel; the constant temperature water in the water cooling device is fully in contact with the acoustic wave coupling rod.

如图1a所示,螺杆挤出机机筒上的不同部位安装有温度压力传感器和超声传感器,温度压力传感器和超声传感器在圆周方向的相对位置如图1b所示,图1b中TPT和UT分别表示温度压力传感器和超声传感器。计算机控制系统同时同步采集多路温度压力传感器的温度、压力和超声传感器的超声信号,并提取反映聚合物混合状态的特征回波振幅;对于任一部位,先以温度和压力为参考量校正当前一段时间内的超声回波振幅,再进行秩滤波,滤除由于螺杆结构变化而影响的振幅跳变,接着采用低通滤波方法提取振幅变化趋势向,归一化回波振幅,将这段时间内多个周期的振幅曲线采用运用相关系数匹配方法进行位置匹配;根据位置匹配的结果,计算所有同一位置的超声回波振幅偏差,并得出综合偏差;最后通过振幅与聚合物含量的关系,采用综合偏差识别聚合物的混合状态,并显示。在实际应用中,可以根据需要,增加控制模块实现聚合物挤出过程的反馈控制。As shown in Figure 1a, temperature and pressure sensors and ultrasonic sensors are installed on different parts of the barrel of the screw extruder, and the relative positions of the temperature, pressure sensor and ultrasonic sensor in the circumferential direction are shown in Figure 1b. In Figure 1b, TPT and UT are respectively Indicates temperature pressure sensor and ultrasonic sensor. The computer control system simultaneously collects the temperature and pressure of multiple temperature and pressure sensors and the ultrasonic signals of ultrasonic sensors, and extracts the characteristic echo amplitude reflecting the mixing state of the polymer; The ultrasonic echo amplitude within a period of time, and then perform rank filtering to filter out the amplitude jump due to the change of the screw structure, and then use the low-pass filtering method to extract the trend of the amplitude change, normalize the echo amplitude, and convert this period of time The amplitude curves of multiple periods within the cycle are matched by using the correlation coefficient matching method; according to the results of the position matching, the amplitude deviation of the ultrasonic echo at the same position is calculated, and the comprehensive deviation is obtained; finally, through the relationship between the amplitude and the polymer content, The mixed state of the polymer is identified using the integrated deviation and displayed. In practical applications, a control module can be added to realize feedback control of the polymer extrusion process as required.

超声特征回波的提取是依据图2的超声传播原理,声波经声波耦合杆、熔态聚合物传播,在耦合杆/聚合物界面和聚合物/螺杆界面产生回波L1和L2,最后由超声探头接收,得到的典型回波信号如图3所示,图3中的A2为超声特征回波振幅。The extraction of ultrasonic characteristic echoes is based on the principle of ultrasonic propagation in Figure 2. The sound wave propagates through the acoustic coupling rod and molten polymer, and generates echoes L1 and L2 at the coupling rod/polymer interface and polymer/screw interface. The typical echo signal received by the probe is shown in Figure 3, and A2 in Figure 3 is the ultrasonic characteristic echo amplitude.

应用实例:Applications:

在单螺杆挤出机进行90%低密度聚乙烯(LDPE)和10%碳酸钙的混合试验。机筒内径为φ90mm,螺杆长1600mm,螺杆转速为10r/min;压力温度传感器采用PT124B/PT124G;在图1中的四个部位安装相同的超声传感器进行检测,图4为四个位置的特征回波信号B扫描图,从图中可以看出在位置I处检测的特征回波幅值起伏较大,而在位置IV处的特征回波信号最稳定,图5列出了四个位置检测特征回波幅值的相对方差(方差与均值之比,表示相对偏差量)的对比情况,说明随着混合的进行特征回波信号越稳定、幅值方差越小,根据这一特点可以检测两种聚合物的混合状态。Mixing trials of 90% low density polyethylene (LDPE) and 10% calcium carbonate were performed in a single screw extruder. The inner diameter of the barrel is φ90mm, the screw length is 1600mm, and the screw speed is 10r/min; the pressure and temperature sensors are PT124B/PT124G; the same ultrasonic sensors are installed at the four positions in Figure 1 for detection, and Figure 4 shows the characteristic cycles of the four positions Wave signal B scan diagram, it can be seen from the figure that the amplitude of the characteristic echo detected at position I fluctuates greatly, while the characteristic echo signal at position IV is the most stable. Figure 5 lists the four position detection features The comparison of the relative variance of the echo amplitude (the ratio of the variance to the mean value, indicating the relative deviation) shows that the more stable the characteristic echo signal is, the smaller the amplitude variance will be as the mixing progresses. According to this feature, two kinds of Mixed state of the polymer.

Claims (3)

1. mixed state ultrasound on-line monitoring method in the production processes of polyalcohol is characterized in that: by being installed in the amplitude that sonac on single screw rod or the double screw extrusion machine obtains the ultrasound echo signal of reflection polymer mixed state in real time; The temperature and pressure of melt polymkeric substance adopts correction of order filtering and low-pass filtering method and normalization echo amplitude as with reference to amount in the machine barrel that the temperature and pressure transmitter of use correspondence position obtains; Utilization related coefficient matching process is finished the location matches between the amplitude curve different cycles; Calculate the ultrasonic echo amplitude deviation of correspondence position between different cycles, by the relation of amplitude and polymer content, the admixture of identification polymkeric substance.
2. mixed state ultrasound on-line monitoring method in the production processes of polyalcohol according to claim 1, it is characterized in that: according to the monitoring requirements at scene, different parts is installed temperature and pressure transmitter and sonac on screw extruder respectively, monitor the polymer mixed state at a plurality of positions simultaneously, realize the monitoring of polymer mixed process.
3. mixed state ultrasound on-line monitoring method in the production processes of polyalcohol according to claim 1 is characterized in that: said sonac is made up of ultrasonic probe, sound wave coupling bar and water cooling plant; The centre frequency of ultrasonic probe is 2.5MHz, and excitation pulse is 1 μ s; The sound wave coupling bar is material with the polyetheretherketone, and main part is a column structure, adopts helicitic texture closely to be connected with screw extruder barrel, and the top contacts with ultrasonic probe is bonding, and bottom and extruder barrel inwall are tangent; Thermostatted water in the water cooling plant fully contacts with the sound wave coupling bar.
CN201010000080A 2010-01-07 2010-01-07 Mixed state ultrasound on-line monitoring method in polymer production process Pending CN101762639A (en)

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CN109196350A (en) * 2016-05-25 2019-01-11 法国电力公司 Pass through the method for the defects of ultrasound detection material
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CN111855491B (en) * 2019-04-28 2023-08-22 中国石油化工股份有限公司 Method and device for detecting flow state of polymer melt
CN112743795A (en) * 2020-12-22 2021-05-04 中国兵器装备集团自动化研究所 Prevent remaining extruder
CN114957663A (en) * 2022-05-27 2022-08-30 成都新晨新材科技有限公司 Continuous polymerization control process, device and system of PBO polymer and computer readable storage medium
CN114957663B (en) * 2022-05-27 2023-08-25 成都新晨新材科技有限公司 PBO polymer continuous polymerization control process, device and system thereof and computer readable storage medium

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