CN101813932A - Method for component content prediction and optimization operation in wet-process metallurgic extraction process - Google Patents

Method for component content prediction and optimization operation in wet-process metallurgic extraction process Download PDF

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CN101813932A
CN101813932A CN200910010295A CN200910010295A CN101813932A CN 101813932 A CN101813932 A CN 101813932A CN 200910010295 A CN200910010295 A CN 200910010295A CN 200910010295 A CN200910010295 A CN 200910010295A CN 101813932 A CN101813932 A CN 101813932A
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常玉清
王福利
尤富强
贾润达
赵露平
董伟威
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Northeastern University China
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

湿法冶金萃取过程组分含量预测与优化操作方法,采用多级萃取槽的湿法冶金萃取工艺,是通过对湿法冶金萃取过程的混合建模,实现萃余液组分含量的实时预测,并对萃取过程提供在线优化操作指导。包括数据采取、辅助变量的选择以及标准化处理、混合模型的建立、混合模型的校正、优化操作指导的确定等步骤。本发明能大幅度提高浸出率,使生产维持在最佳损伤状态,并能减少原料和能源的消耗,延长设备的运行周期。

Figure 200910010295

The hydrometallurgical extraction process component content prediction and optimization operation method adopts the hydrometallurgical extraction process of the multi-stage extraction tank, and realizes the real-time prediction of the raffinate component content through the mixed modeling of the hydrometallurgical extraction process. And provide online optimization operation guidance for the extraction process. Including data collection, auxiliary variable selection and standardization processing, establishment of mixed model, correction of mixed model, determination of optimization operation guidance and other steps. The invention can greatly increase the leaching rate, maintain the production in the best damaged state, reduce the consumption of raw materials and energy, and prolong the operation period of the equipment.

Figure 200910010295

Description

湿法冶金萃取过程组分含量预测与优化操作方法 Component Content Prediction and Optimal Operation Method in Hydrometallurgical Extraction Process

技术领域technical field

本发明属于湿法冶金领域,特别提供一种基于混合模型的萃取组分含量预测与优化操作方法,即提供一种实时预测萃余液组分浓度并提供优化操作指导的方法。The invention belongs to the field of hydrometallurgy, and in particular provides a method for predicting and optimizing the content of extraction components based on a mixed model, that is, providing a method for predicting the concentration of raffinate components in real time and providing guidance for optimal operations.

背景技术Background technique

湿法冶金工艺是逐渐成熟并且迫切需要工业化的新工艺,与传统的火法冶炼相比,湿法冶金技术具有高效、清洁、适用于低品位复杂金属矿产资源回收等优势。特别是针对我国矿产资源贫矿多,复杂共生,杂质含量高的特点,湿法冶金工艺工业化对于提高矿产资源的综合利用率,降低固体废弃物产量,减少环境污染,都有着重大意义。Hydrometallurgy technology is a new technology that is gradually mature and urgently needs industrialization. Compared with traditional pyrometallurgy, hydrometallurgy technology has the advantages of high efficiency, cleanness, and suitable for recovery of low-grade complex metal mineral resources. Especially in view of the characteristics of my country's mineral resources, which are rich in lean ore, complex symbiosis, and high impurity content, the industrialization of hydrometallurgical processes is of great significance for improving the comprehensive utilization of mineral resources, reducing solid waste production, and reducing environmental pollution.

近几年湿法冶金工艺、设备研究进展迅速。但是湿法冶金工艺流程复杂,设备类型多样,工艺条件恶劣,如高温、高压、强腐蚀等,所以湿法冶金工艺要实现大规模工业化自动控制水平的提高,才能保证生产安全、稳定、连续的运行,才能保证产品质量和产量。In recent years, research on hydrometallurgical technology and equipment has progressed rapidly. However, the hydrometallurgical process is complicated, the equipment types are diverse, and the process conditions are harsh, such as high temperature, high pressure, strong corrosion, etc. Therefore, the hydrometallurgical process must realize the improvement of the automatic control level of large-scale industrialization in order to ensure safe, stable and continuous production. Only by running can the product quality and output be guaranteed.

湿法冶金串级萃取除杂过程工艺流程如图1所示,整条萃取生产线由多级萃取槽串联组成,自左向右依次为由多级萃取槽构成的萃取段、洗涤段、反萃段和反铁段。每级萃取槽由混合室和澄清室组成,在萃取分离过程中,通过对萃取槽体独特的结构设计和萃取过程混合室内搅拌电机的动力作用,使得有机相和水相在混合室、澄清室并流,而整体却产生逆向流动。有机相总是从左向右流动,水相总是从右向左流动。澄清室中的溶液根据有机萃取剂与水互不相溶的原理分为两层:上层为有机相,下层为水相。操作者根据串级萃取原理,按照一定平衡比例关系,控制有机、料液、洗液、反萃液以及反铁液的流量。萃取段的作用是把水相料液中的绝大部分杂质金属和少量有价金属萃入有机相;洗涤段的作用是通过洗液与有机相的接触,把绝大部分有价金属洗回水相;而反萃段与反铁段的作用是使杂质金属重新返回水相,从而有机相得以再生。The process flow of hydrometallurgical cascade extraction and impurity removal process is shown in Figure 1. The entire extraction production line is composed of multi-stage extraction tanks in series. segment and anti-iron segment. Each stage of extraction tank is composed of a mixing chamber and a clarification chamber. During the extraction and separation process, through the unique structural design of the extraction tank and the power of the stirring motor in the mixing chamber during the extraction process, the organic phase and the water phase are separated in the mixing chamber and clarification chamber. parallel flow, but the whole produces reverse flow. The organic phase always flows from left to right and the aqueous phase always flows from right to left. The solution in the clarification chamber is divided into two layers according to the principle that the organic extractant and water are immiscible: the upper layer is the organic phase, and the lower layer is the water phase. According to the cascade extraction principle, the operator controls the flow of organic, feed liquid, washing liquid, stripping liquid and anti-iron liquid according to a certain balance ratio. The function of the extraction section is to extract most of the impurity metals and a small amount of valuable metals in the aqueous phase into the organic phase; the function of the washing section is to wash back most of the valuable metals through the contact between the washing liquid and the organic phase. The water phase; and the role of the stripping section and the anti-iron section is to return the impurity metals to the water phase, so that the organic phase can be regenerated.

为了保证产品的质量,提高金属的收率,降低消耗,充分发挥设备的生产能力,生产过程中需要对萃取生产线水相出口(萃余液)中产品组分浓度进行化验。在实际生产中,组分浓度均无法在线测量,而是采用离线实验室分析获得,但离线分析滞后数小时,且分析采样次数少(1次/天),远远不能满足控制的要求。有两种途径来解决这一问题,其一是采用在线分析仪;其二是通过对过程进行建模,实现组分浓度的预测。由于前者功能还不完善,且投资较大、难以维护,尚不能全面满足湿法冶金萃取分离生产过程的连续在线检测需求;因此最好的解决方案是使用第二种途径,即建立萃取过程组分含量的预测模型,在不增加投资的前提下在线预测各组分的浓度。In order to ensure the quality of the product, increase the yield of metals, reduce consumption, and give full play to the production capacity of the equipment, it is necessary to test the concentration of product components in the aqueous phase outlet (raffinate) of the extraction production line during the production process. In actual production, the concentration of the components cannot be measured online, but obtained by offline laboratory analysis, but the offline analysis lags for several hours, and the analysis sampling frequency is small (1 time/day), which is far from meeting the control requirements. There are two ways to solve this problem, one is to use online analyzer; the other is to realize the prediction of component concentration by modeling the process. Since the function of the former is not perfect, and the investment is large and difficult to maintain, it cannot fully meet the continuous on-line detection requirements of the hydrometallurgical extraction and separation production process; therefore, the best solution is to use the second approach, that is, to establish an extraction process group The prediction model of component content can predict the concentration of each component online without increasing investment.

目前,尚未见有关湿法冶金萃取过程组分含量混合建模方法与优化操作指导的报道。工厂所采用的方法是对这些组分浓度取样进行人工化验,通过离线分析方式获得,操作者根据组分浓度化验值来调整流量设定值,以保证生产目标所规定的产品纯度和料液处理量。这种方法的缺点是,人工化验滞后大,达数小时;另外由于化验成本问题使得采样周期都较长,因此,这些化验值难以直接用于质量控制。操作者主要依靠各自的经验进行调节,从而使产品的一次合格率很难保证,辅料消耗增加,产品成本提高。At present, there is no report on the mixing modeling method and optimization operation guidance of the component content in the hydrometallurgical extraction process. The method adopted by the factory is to manually test the concentration of these components and obtain them through off-line analysis. The operator adjusts the flow rate setting value according to the test value of the component concentration to ensure the product purity and material liquid treatment specified in the production target. quantity. The disadvantage of this method is that the artificial assay has a large lag, which can reach several hours; in addition, due to the cost of the assay, the sampling period is long, so it is difficult for these assay values to be directly used for quality control. Operators mainly rely on their own experience to adjust, so that it is difficult to guarantee the first pass rate of the product, the consumption of auxiliary materials increases, and the cost of the product increases.

发明内容Contents of the invention

本发明提供一种湿法冶金萃取过程组分含量预测与优化操作方法,通过对湿法冶金萃取过程的混合建模,实现萃余液组分含量的实时预测,并对萃取过程提供在线优化操作指导。The invention provides a hydrometallurgical extraction process component content prediction and optimization operation method, through the mixed modeling of the hydrometallurgical extraction process, real-time prediction of raffinate component content is realized, and online optimization operation is provided for the extraction process guide.

本发明的目的是寻求一种供湿法冶金萃取分离生产过程中组分含量预测与优化操作的方法,它用于解决如下问题:The object of the present invention is to seek a kind of method for component content prediction and optimal operation in hydrometallurgical extraction separation production process, and it is used to solve following problem:

(1)为湿法冶金萃取除杂过程实现自动控制提供组分含量监测数据,实现萃取除杂过程的优化操作指导;(1) Provide component content monitoring data for the automatic control of the hydrometallurgical extraction and impurity removal process, and realize the optimal operation guidance for the extraction and impurity removal process;

(2)通过对料液成分、流量等易变因素的实际波动情况进行模拟,掌握不同波动幅度对产品质量的影响,提供适时而合理地优化操作指导,保证产品质量,实现萃取过程的优化控制;(2) By simulating the actual fluctuations of variable factors such as feed liquid composition and flow rate, grasp the impact of different fluctuation ranges on product quality, provide timely and reasonable guidance on optimizing operations, ensure product quality, and realize optimal control of the extraction process ;

(3)本发明的软测量方法既考虑了机理模型的优势,又综合了数据模型的特点,并能够模拟萃取除杂生产过程,掌握生产过程中的辅料消耗,制定合理的生产计划。(3) The soft sensing method of the present invention not only considers the advantages of the mechanism model, but also integrates the characteristics of the data model, and can simulate the production process of extraction and impurity removal, grasp the consumption of auxiliary materials in the production process, and formulate a reasonable production plan.

(4)取代人工化验分析,达到及时准确检测生产状况的目的。(4) Replace manual laboratory analysis to achieve the purpose of timely and accurate detection of production status.

本发明所提供的湿法冶金萃取过程组分含量预测与优化操作方法包括:(1)过程数据采集、(2)辅助变量的选择以及标准化处理、(3)混合模型的建立、(4)混合模型的校正、(5)优化操作指导的确定等步骤。The method for predicting and optimizing the content of components in the hydrometallurgical extraction process provided by the present invention includes: (1) process data collection, (2) selection and standardization of auxiliary variables, (3) establishment of a mixing model, (4) mixing Calibration of the model, (5) Determination of the optimization operation guidance and other steps.

(1)过程数据采集(1) Process data acquisition

本发明装置包括萃取过程组分含量预测与优化操作系统、上位机、PLC、现场传感变送部分,如图2所示。其中现场传感变送部分包括pH值、温度、流量等检测仪表。在萃取过程现场安装检测仪表,检测仪表将采集的信号通过Profibus-DP总线送到PLC,PLC通过以太网定时将采集信号传送到上位机,上位机把接受的数据传到萃取过程组分含量预测与优化操作系统,进行萃余液组分含量的实时预测,并提供在线优化操作指导。The device of the present invention includes an extraction process component content prediction and optimization operating system, a host computer, a PLC, and on-site sensing and transmission parts, as shown in FIG. 2 . Among them, the field sensing and transmission part includes pH value, temperature, flow and other detection instruments. The detection instrument is installed on site during the extraction process, and the detection instrument sends the collected signal to the PLC through the Profibus-DP bus, and the PLC regularly transmits the collected signal to the host computer through Ethernet, and the host computer transmits the received data to the extraction process component content prediction With the optimization of the operating system, real-time prediction of the content of raffinate components is performed, and online optimization operation guidance is provided.

本发明装置的各部分功能:The functions of each part of the device of the present invention:

(A)现场传感变送部分:包括pH值、温度、流量等检测仪表由传感器组成,负责过程数据的采集与传送;(A) On-site sensing and transmission part: including pH value, temperature, flow and other detection instruments are composed of sensors, responsible for the collection and transmission of process data;

(B)PLC:负责把采集的信号A/D转换,并通过以太网把信号传送给上位机;(B) PLC: Responsible for A/D conversion of the collected signal, and transmit the signal to the host computer through Ethernet;

(C)上位机:收集本地PLC数据,传送给萃取过程组分含量预测与优化操作系统,并提供在线优化操作指导。(C) Host computer: collect local PLC data, send it to the extraction process component content prediction and optimization operating system, and provide online optimization operation guidance.

(2)辅助变量的选择以及标准化处理(2) Selection and standardization of auxiliary variables

本发明所选择的辅助变量包括,The auxiliary variables selected by the present invention include,

(A)料液中被萃组分的浓度x1(A) concentration x 1 of the extracted component in the feed liquid;

(B)料液的流量x2(B) The flow rate x 2 of feed liquid;

(C)洗液的流量x3(C) flow rate x 3 of washing liquid;

(D)有机相的流量x4 (D) Flow rate of organic phase x 4

(D)萃余液的pH值x5(D) pH value x 5 of raffinate;

(E)料液的温度x6(E) Temperature x 6 of feed liquid.

为了防止各检测变量由于单位不同而对数据模型产生影响,首先将采集到的传感器测量数据进行标准化处理,In order to prevent the impact of each detection variable on the data model due to different units, the collected sensor measurement data is first standardized.

xx ~~ jj (( ii )) == xx jj (( ii )) -- xx jj (( minmin )) xx jj (( maxmax )) -- xx jj (( minmin )) -- -- -- (( 11 ))

式中

Figure G200910010295XD00032
-第i个数据样本,第j个传感器测量值的标准化值;In the formula
Figure G200910010295XD00032
- the i-th data sample, the normalized value of the j-th sensor measurement;

xj(i)-第i个数据样本,第j个传感器测量值;x j (i) - i-th data sample, j-th sensor measurement;

-第j个传感器测量值的最小值; - the minimum value of the measured value of the jth sensor;

Figure G200910010295XD00034
-第j个传感器测量值的最大值。
Figure G200910010295XD00034
- the maximum value of the jth sensor measurement.

(3)混合模型的建立(3) Establishment of mixed model

I、混合模型的结构I. The structure of the mixed model

混合使用多种建模方法建立对象的数学模型,可以达到各种方法取长补短的效果,目前已成为研究的热点。若系统有先验的物理知识可以利用,则尽量利用,以把黑箱模型转化成灰箱模型,从而把机理方法和数据方法相结合。数据方法可提取机理方法所无法解释的对象内部的复杂信息,而机理模型又可提高统计模型的推广能力。结合方式一般分为并行和串行两种。Mixed use of multiple modeling methods to establish the mathematical model of the object can achieve the effect of various methods complementing each other, and has become a research hotspot at present. If the system has prior physical knowledge that can be used, it should be used as much as possible to transform the black box model into a gray box model, so as to combine the mechanism method with the data method. The data method can extract the complex information inside the object that cannot be explained by the mechanism method, and the mechanism model can improve the generalization ability of the statistical model. Combination methods are generally divided into parallel and serial.

(A)串行结合方式:首先用机理方法得到一个带参数的模型结构,然后用数据方法来确定那些参数;(A) Serial combination method: first use the mechanism method to obtain a model structure with parameters, and then use the data method to determine those parameters;

(B)并行结合方式:采用数据方法确定一个补偿器,对机理模型得到的结果进行补偿。(B) Parallel combination method: use the data method to determine a compensator to compensate the results obtained by the mechanism model.

先验知识的应用,与单纯地根据数据建立的黑箱模型相比,提高了模型的精度,增强了模型的推广能力,而且减少了参数估计所需的数据,减少了计算量。The application of prior knowledge improves the accuracy of the model, enhances the generalization ability of the model, reduces the data required for parameter estimation, and reduces the amount of calculation compared with the black-box model established purely based on data.

在很多情况下,单纯利用机理模型不足以描述过程的所有特性,一些过程中的可测变量由于与主导变量间的关系复杂,难以全部包含在机理模型之中;另外,一些过程中的未知影响因素同样会降低机理模型的预测精度,这时可利用数据模型对机理模型中的未建模动态进行补偿,以提高模型的预测精度。针对萃取过程的特点,本发明采用并行混合模型的结构,如图3所示。本发明采用基于非线性PLS的并行混合模型结构对机理模型中的未建模动态进行补偿。In many cases, simply using the mechanistic model is not enough to describe all the characteristics of the process. Due to the complicated relationship between the measurable variables and the leading variables in some processes, it is difficult to include them all in the mechanistic model; Factors will also reduce the prediction accuracy of the mechanism model. At this time, the data model can be used to compensate the unmodeled dynamics in the mechanism model to improve the prediction accuracy of the model. Aiming at the characteristics of the extraction process, the present invention adopts the structure of the parallel mixing model, as shown in FIG. 3 . The invention adopts the parallel hybrid model structure based on nonlinear PLS to compensate the unmodeled dynamics in the mechanism model.

II、机理模型II. Mechanism model

在全面深刻了解过程的反应机理后,就可以列写有关平衡方程式,确定不可测主导变量和可测二次变量的数学关系,建立估计主导变量的机理模型。机理建模要求对具体对象有深入的了解,全面把握实际过程所牵涉到的基本规律,包括热力学中的状态方程,物理化学中的相平衡、反应动力学、物料平衡、能量平衡,以及高分子化学等诸多方面的知识。机理建模已经在很多方面取得了成功,在机理模型建好后,可以用来模拟实际系统的运行情况,加深对实际过程的理解,提高操作水平;同时通过模型仿真,可以帮助掌握对象的动态特性,为过程优化和控制奠定基础。然而建立一个机理模型通常需要耗费很大的精力,且不适用于机理尚不完全清楚的工业过程,因此本发明通过一定的假设对机理模型进行简化。After a comprehensive understanding of the reaction mechanism of the process, the relevant balance equations can be written, the mathematical relationship between the unmeasurable leading variable and the measurable secondary variable can be determined, and the mechanism model for estimating the leading variable can be established. Mechanism modeling requires an in-depth understanding of specific objects and a comprehensive grasp of the basic laws involved in the actual process, including the equation of state in thermodynamics, phase balance, reaction kinetics, material balance, energy balance in physical chemistry, and polymer Chemistry and many other aspects of knowledge. Mechanism modeling has achieved success in many aspects. After the mechanism model is built, it can be used to simulate the operation of the actual system, deepen the understanding of the actual process, and improve the operation level; at the same time, through model simulation, it can help to grasp the dynamics of the object. characteristics, laying the foundation for process optimization and control. However, establishing a mechanism model usually requires a lot of energy, and is not suitable for industrial processes whose mechanism is not completely clear. Therefore, the present invention simplifies the mechanism model through certain assumptions.

本发明中采用的机理模型由m+n级混合清澄器组成,其中m级用于萃取、n级用于洗涤,其等效结构如图4所示。通常,由于反萃、反铁效率较高,经过反萃段后的新鲜有机相中各金属离子的浓度可视为0。因此为简化机理模型结构,仅考虑对萃取段以及洗涤段进行建模。The mechanism model adopted in the present invention is composed of m+n stage mixing clarifiers, wherein m stage is used for extraction and n stage is used for washing, and its equivalent structure is shown in Fig. 4 . Usually, due to the high efficiency of stripping and anti-iron, the concentration of each metal ion in the fresh organic phase after the stripping section can be regarded as zero. Therefore, in order to simplify the mechanism model structure, only the extraction section and the washing section are considered to be modeled.

依据物料衡算关系,对于萃取段第i级,i=1,2,...m-1,存在如下物料衡算关系:According to the material balance relationship, for the i-th stage of the extraction section, i=1, 2,...m-1, there is the following material balance relationship:

Vyi-1+(L+L′)xi+1=Vyi+(L+L′)xi                                        (2)Vy i-1 +(L+L′)x i+1 =Vy i +(L+L′)x i (2)

而对于萃取段第m级(进料级),即i=m,存在如下物料衡算关系:And for the m grade (feed grade) of extraction section, i.e. i=m, there is following material balance relation:

Vym-1+Lx0+L′xm+1=Vym+(L+L′)xm                     (3)Vy m-1 +Lx 0 +L′x m+1 =Vy m +(L+L′)x m (3)

对于洗涤段第j级,j=m+1,...,n-1,存在如下物料衡算关系:For the jth stage of the washing section, j=m+1,...,n-1, there is the following material balance relationship:

Vyj-1+L′xj+1=Vyj+L′xj                             (4)Vy j-1 +L′x j+1 =Vy j +L′x j (4)

而对于洗涤段第n级,即j=n,存在如下物料衡算关系:And for the nth stage of the washing section, i.e. j=n, there is the following material balance relationship:

Vyn-1+L′x′0=Vyn+L′xn                             (5)Vy n-1 +L'x' 0 =Vy n +L'x n (5)

式中V-有机相流量;In the formula, V-organic phase flow rate;

L-料液流量;L-material liquid flow rate;

L′-洗液流量;L'- washing liquid flow rate;

yi-从第i级混合澄清器流出有机相中被萃组分的浓度;y i - the concentration of the extracted component in the organic phase effluent from the i-stage mixing-settler;

xi-从第i级混合澄清器流出有机相中被萃组分的浓度;x i - the concentration of the extracted component in the organic phase effluent from the i-stage mixing and clarifying device;

yj-从第j级混合澄清器流出有机相中被萃组分的浓度;y j - the concentration of the extracted component in the organic phase effluent from the j-stage mixing-settler;

xj-从第j级混合澄清器流出有机相中被萃组分的浓度;x j - the concentration of the extracted component in the organic phase effluent from the j-stage mixing-settler;

y0-新鲜有机相中被萃组分的浓度; y0 - the concentration of the extracted component in the fresh organic phase;

x0-料液中被萃组分的浓度;x 0 - the concentration of the extracted component in the feed liquid;

x′0-洗液中被萃组分的浓度。x' 0 - the concentration of the extracted component in the washing solution.

上述m+n个物料衡算关系组成了一个具有2(m+n)个未知数的方程组,为了求解上述方程组,还需要引入萃取平衡关系方程The above m+n material balance relations form a system of equations with 2(m+n) unknowns. In order to solve the above system of equations, it is also necessary to introduce the extraction balance relation equation

yi=f(xi)                                             (6)y i =f(x i ) (6)

为了建立理想情况下平衡时有机相中金属离子的浓度与水相金属离子浓度之间的未知函数关系f(·),需要进行离线萃取平衡实验以获取用于辨识的样本数据。首先取出少量新鲜的有机相用于萃取平衡实验,分别配制具有不同金属离子浓度的水相,用分液漏斗进行萃取平衡实验,有机相和水相按一定的相比加入分液漏斗,振荡混合一定时间静置分层,调节平衡后的水相pH值,分析水相金属离子浓度,记录用于辨识的实验数据。通过分析,可以将模型具体化为半经验模型In order to establish the unknown functional relationship f(·) between the concentration of metal ions in the organic phase and the concentration of metal ions in the aqueous phase in an ideal equilibrium, an offline extraction equilibrium experiment is required to obtain sample data for identification. First, take out a small amount of fresh organic phase for the extraction equilibrium experiment, prepare the aqueous phases with different metal ion concentrations respectively, and use the separatory funnel for the extraction equilibrium experiment, add the organic phase and the aqueous phase to the separatory funnel according to a certain ratio, and oscillate to mix Stand and stratify for a certain period of time, adjust the pH value of the balanced water phase, analyze the concentration of metal ions in the water phase, and record the experimental data for identification. Through analysis, the model can be embodied as a semi-empirical model

ythe y ‾‾ ii == ff (( xx ‾‾ ii )) == aa 11 ·&Center Dot; xx ‾‾ ii aa 22 ++ xx ‾‾ ii -- -- -- (( 77 ))

式中a1,a2-待辨识参数。In the formula, a 1 , a 2 - parameters to be identified.

由(7)式的物理意义,可以判断出a1,a2的值应大于0。因为优化计算的结果往往不是惟一的,为了尽可能使计算结果符合实际情况,下面采用带约束的非线性优化算法,可根据经验将a1,a2的值限制在一定的范围之内,对式(7)进行反向优化计算。具体步骤是:From the physical meaning of formula (7), it can be judged that the values of a 1 and a 2 should be greater than 0. Because the results of optimization calculations are often not unique, in order to make the calculation results conform to the actual situation as much as possible, the nonlinear optimization algorithm with constraints is used below, and the values of a 1 and a 2 can be limited within a certain range based on experience. Equation (7) for reverse optimization calculation. The specific steps are:

(A)随机产生一组大于0,小于a1,a2规定范围的初始值;(A) Randomly generate a group of initial values greater than 0 and less than the specified range of a 1 and a 2 ;

(B)将a1,a2代入式(6),计算yi的估计值

Figure G200910010295XD00061
(B) Substitute a 1 and a 2 into formula (6) to calculate the estimated value of y i
Figure G200910010295XD00061

(C)将样本值与估计误差平方和(C) Sum of the sample value and the estimated error square

EMSEMS == ΣΣ ii == 11 nno (( ythe y ‾‾ ii -- ythe y ‾‾ ^^ ii )) 22 -- -- -- (( 88 ))

作为优化计算的目标函数,判断目标函数是否符合要求,如满足要求,则停止计算,否则进入下一步;As the objective function of the optimization calculation, judge whether the objective function meets the requirements, if the requirements are met, stop the calculation, otherwise enter the next step;

式中yi-为第i个样本的观测值;In the formula, y i - is the observed value of the i-th sample;

Figure G200910010295XD00063
-为第i个样本的估计值;
Figure G200910010295XD00063
- is the estimated value of the i-th sample;

n-为样本的个数。n- is the number of samples.

(D)用BFGS方法进行带约束条件的迭代计算,得到新的a1,a2(D) Use the BFGS method to perform iterative calculation with constraints to obtain new a 1 and a 2 ;

(E)重复(B)~(D)步,直到目标函数满足要求。(E) Repeat steps (B) to (D) until the objective function meets the requirements.

III、数据模型III. Data Model

根据系统的输入输出数据,建立与系统外特性等价的数学模型的方法,称为数据建模。数据建模将系统看作黑箱,在不了解系统内部结构和机理的情况下,选取一组与主导变量有密切联系且容易测量的二次变量,根据某种最优准则,利用统计方法构造二次变量与主导变量间的数学模型。According to the input and output data of the system, the method of establishing a mathematical model equivalent to the external characteristics of the system is called data modeling. Data modeling regards the system as a black box. Without knowing the internal structure and mechanism of the system, a group of secondary variables that are closely related to the leading variable and easy to measure are selected. According to an optimal criterion, the secondary variable is constructed using statistical methods. The mathematical model between the secondary variable and the leading variable.

本发明中采用非线性PLS(RBF-PLS)作为数据建模方法补偿机理模型中的未建模动态,RBF-PLS方法由RBF网络与PLS算法结合而成,其模型结构如图5所示。RBF-PLS方法通常选用高斯径向基函数,将自变量数据矩阵X转化为激活矩阵A。A的元素可以利用下式进行定义:In the present invention, non-linear PLS (RBF-PLS) is used as the data modeling method to compensate the unmodeled dynamics in the mechanism model. The RBF-PLS method is formed by combining the RBF network and the PLS algorithm, and its model structure is shown in FIG. 5 . The RBF-PLS method usually uses the Gaussian radial basis function to transform the independent variable data matrix X into the activation matrix A. The elements of A can be defined using the following formula:

aa ijij == expexp (( -- || || xx ii -- cc jj || || 22 σσ jj 22 )) ii ,, jj == 1,21,2 ,, .. .. .. kk -- -- -- (( 99 ))

式中k-数据样本的个数;In the formula, k-the number of data samples;

xi-第i个数据样本的输入向量;x i - the input vector for the ith data sample;

aij-A第i行,第j列的元素;a ij - the element in row i, column j of A;

cj-高斯函数的中心参数;c j - the central parameter of the Gaussian function;

σj-高斯函数的宽度参数。σ j - the width parameter of the Gaussian function.

在RBF-PLS方法中,中心参数cj选为每个数据样本的输入向量,即In the RBF-PLS method, the center parameter c j is selected as the input vector for each data sample, namely

cj=xj                             (10)c j =x j (10)

而宽度参数σj可由下式进行计算:The width parameter σ j can be calculated by the following formula:

σσ jj == ee kk ΣΣ ii == 11 kk || || xx ii -- xx jj || || -- -- -- (( 1111 ))

式中e-大于0的常数,本发明中取1,In the formula, e- is greater than the constant of 0, gets 1 among the present invention,

因此矩阵A是一个对角元为1的k×k维方阵。Therefore, matrix A is a k×k-dimensional square matrix with diagonal elements of 1.

在进行上述变换之后,利用PLS算法建立矩阵A与输出数据向量y之间的线性回归模型,若T是由前h个得分向量组成的k×h维矩阵,则模型可以利用下式进行描述:After the above transformation, use the PLS algorithm to establish a linear regression model between the matrix A and the output data vector y. If T is a k×h dimensional matrix composed of the first h score vectors, the model can be described by the following formula:

A=TPT+E                            (12)A=TP T +E (12)

y=Tq+r=Ab+r                       (13)y=Tq+r=Ab+r (13)

式中A-激活矩阵;where A-activation matrix;

T-得分矩阵;T-score matrix;

P-载荷矩阵;P-loading matrix;

E-残差矩阵;E-residual matrix;

y-输出数据向量;y - output data vector;

q-载荷向量;q - loading vector;

r-残差向量;r - residual vector;

b-PLS的回归系数向量。Vector of regression coefficients for b-PLS.

利用上述算法的建模步骤如下:The modeling steps using the above algorithm are as follows:

(A)将训练样本进行标准化处理;(A) standardize the training samples;

(B)计算各训练样本与中心的欧氏距离,并利用(11)式计算宽度参数σj(B) Calculate the Euclidean distance between each training sample and the center, and use (11) formula to calculate the width parameter σ j ;

(C)利用(9)式计算得到激活矩阵A;(C) Utilize formula (9) to calculate and obtain activation matrix A;

(D)建立激活矩阵A与输出数据向量y之间的线性回归模型,并利用PLS算法求得回归系数b。(D) Establish a linear regression model between the activation matrix A and the output data vector y, and use the PLS algorithm to obtain the regression coefficient b.

(4)混合模型的校正(4) Correction of the mixed model

由于某些过程数据不够可靠,因此仅仅利用上述方法建立的模型还不足以提供可靠的预测精度,因此在上述模型的基础上,我们还利用预测误差来进一步校正混合模型,该递推算法中的校正量d(t)可由下式进行确定Because some process data are not reliable enough, the model established by the above method alone is not enough to provide reliable prediction accuracy. Therefore, on the basis of the above model, we also use the prediction error to further correct the mixed model. The recursive algorithm in The correction amount d(t) can be determined by the following formula

d(t)=wd0(t)+(1-w)d(t-1)                               (14)d(t)=wd 0 (t)+(1-w)d(t-1) (14)

式中d(t)-上一次预测误差与历史误差的加权和;In the formula, d(t)-the weighted sum of the previous forecast error and historical error;

d0(t)-当前预测误差;d 0 (t) - current forecast error;

w-加权系数,本发明专利中取0.5;w-weighting coefficient, 0.5 is taken in the patent of the present invention;

且有d(0)=0,d0(t)可由下式进行计算And d(0)=0, d 0 (t) can be calculated by the following formula

d0(t)=ylab(t-1)-ymod(t-1)                             (15)d 0 (t)=y lab (t-1)-y mod (t-1) (15)

式中ylab-离线化验值;In the formula, y lab -offline assay value;

ymod-模型预测值;y mod - model predicted value;

最终的模型校正输出可以利用下式进行计算The final model-corrected output can be calculated using the following formula

ycor(t)=ymod(t)+d(t)                              (16)y cor (t) = y mod (t) + d (t) (16)

式中ycor-校正后的模型预测值。where ycor - corrected model prediction.

(5)优化操作指导的确定(5) Determination of optimal operation guidance

本发明采用基于混合模型的专家系统为萃取过程提供在线优化操作指导,通过现场与操作者的交流,得到一系列操作经验,并结合混合模型,通过迭代运算给出各操作变量的指导,其具体算法步骤如下:The present invention adopts an expert system based on a mixed model to provide online optimization operation guidance for the extraction process, obtains a series of operating experience through on-site communication with the operator, and combines the mixed model to provide guidance for each operating variable through iterative calculations. The algorithm steps are as follows:

(A)设定萃余液中各被萃组分的浓度要求;(A) setting the concentration requirements of each extracted component in the raffinate;

(B)读取料液中各被萃组分的浓度以及料液的流量;(B) read the concentration of each extracted component in the feed liquid and the flow rate of the feed liquid;

(C)根据操作者的经验,选择一个合适的有机相流量,以及与之相应的洗液流量作为初始值;(C) According to the experience of the operator, select an appropriate organic phase flow rate and the corresponding washing liquid flow rate as the initial value;

(D)在上述操作条件下,利用混合模型预测萃余液中各被萃组分的浓度,判断是否达标;若有一不达标,返回(C)步重新选择一个初始化有机相流量;若均达标进入(E)步;(D) Under the above operating conditions, use the mixed model to predict the concentration of each extracted component in the raffinate, and judge whether it meets the standard; if one fails to meet the standard, return to step (C) to re-select an initial organic phase flow rate; if all reach the standard Go to step (E);

(E)将有机相流量在上述初始值的条件下减小ΔV,洗液流量同时进行相应调整,重新调用混合模型,对萃余液中各被萃组分的浓度进行预测,判断是否达标;若有一不达标,则停止计算,前次求得的有机相流量与洗液流量为当前时刻的优化操作指导;若均达标,则(E)步重复。(E) Reduce the flow rate of the organic phase by ΔV under the condition of the above initial value, adjust the flow rate of the washing solution accordingly, call the mixing model again, predict the concentration of each extracted component in the raffinate, and judge whether it meets the standard; If one fails to meet the standard, then stop the calculation, and the organic phase flow rate and washing liquid flow rate obtained last time are the optimal operation guidance at the current moment; if both reach the standard, repeat step (E).

本发明能大幅度提高萃取效率,使生产维持在最佳操作状态,并能有效减小辅料和能源的消耗,延长设备的运行周期。The invention can greatly improve the extraction efficiency, maintain the production in the best operating state, effectively reduce the consumption of auxiliary materials and energy, and prolong the operation period of the equipment.

附图说明Description of drawings

图1为湿法冶金萃取过程工艺流程图,其中,PHT1-萃余液pH值传感器,PH2-洗涤余液pH值传感器,PH3-反萃余液pH值传感器,FT1-料液流量传感器,FT2-洗液流量传感器,FT3-反萃液流量传感器,FT4-反铁液流量传感器,FT5-有机相流量传感器,TT1-料液温度传感器;Fig. 1 is a process flow diagram of hydrometallurgical extraction process, wherein, PHT1-raffinate pH value sensor, PH2-washing raffinate pH value sensor, PH3-reverse raffinate pH value sensor, FT1-feed liquid flow sensor, FT2 - washing liquid flow sensor, FT3- stripping liquid flow sensor, FT4- anti-iron liquid flow sensor, FT5- organic phase flow sensor, TT1- feed liquid temperature sensor;

图2为本发明装置的硬件结构示意图,Fig. 2 is a schematic diagram of the hardware structure of the device of the present invention,

图3为混合模型结构图;Fig. 3 is a hybrid model structure diagram;

图4为机理模型等效结构图;Fig. 4 is the equivalent structure diagram of mechanism model;

图5为非线性PLS模型结构图;Fig. 5 is a structural diagram of the nonlinear PLS model;

图6为铜萃取萃余液Cu离子浓度化验值与预测值曲线趋势图;Fig. 6 is the curve trend chart of copper extraction raffinate Cu ion concentration test value and predicted value;

图7为铜萃取组分浓度预测与优化操作指导界面图;Fig. 7 is the interface diagram of copper extraction component concentration prediction and optimization operation guidance;

图8为P204预萃取萃余液Cu离子浓度化验值与预测值曲线趋势图;Fig. 8 is P204 pre-extraction raffinate Cu ion concentration test value and predicted value curve trend figure;

图9为P204预萃取萃余液Mn离子浓度化验值与预测值曲线趋势图;Fig. 9 is P204 pre-extraction raffinate Mn ion concentration test value and predicted value curve trend figure;

图10为P204预萃检测界面图;Figure 10 is a P204 pre-extraction detection interface diagram;

图11为钴湿法冶金萃取车间组分含量预测界面图;Figure 11 is the interface diagram of component content prediction in the cobalt hydrometallurgical extraction workshop;

图12为钴湿法冶金萃取车间优化操作指导界面图。Fig. 12 is an interface diagram of the optimization operation guidance interface of the cobalt hydrometallurgical extraction workshop.

具体实施方式Detailed ways

下面的具体实施例在钴湿法冶金生产厂的萃取车间里得到了实际应用,并取得了显著的效果。The following specific examples have been practically applied in the extraction workshop of a cobalt hydrometallurgical production plant, and have achieved remarkable results.

实施例1Example 1

在铜萃除杂生产线上的实施。Implementation on the copper extraction and impurity removal production line.

该生产线上铜萃取共有5级串级萃取槽,2级用于萃取,1级用于洗涤,2级用于反萃,共5台搅拌电机,4个流量计,4台泵,4台变频器,1个pH计,1个温度计组成。萃取过程检测系统主要由流量检测、pH值检测、温度检测构成。There are 5 stages of cascaded extraction tanks for copper extraction on this production line, 2 stages for extraction, 1 stage for washing, 2 stages for stripping, a total of 5 stirring motors, 4 flow meters, 4 pumps, and 4 frequency conversion device, a pH meter, and a thermometer. The extraction process detection system is mainly composed of flow detection, pH value detection and temperature detection.

PLC控制器采用Simens 300系列的CPU 315-2DP,具有Profibus-DP口连接分布式IO。为PLC配备以太网通讯模块,用于上位机访问PLC数据。PLC控制器和以太网通讯模块放置在中央控制室中的PLC柜中。PLC controller adopts CPU 315-2DP of Siemens 300 series, with Profibus-DP port to connect distributed IO. Equip the PLC with an Ethernet communication module for the host computer to access PLC data. The PLC controller and Ethernet communication module are placed in the PLC cabinet in the central control room.

萃取过程的pH值是通过Cole-parmer公司生产的玻璃电极进行pH值在线检测,将溶液pH值的变化转化为mV信号的变化。玻璃电极pH测量系统将一支对于pH敏感的玻璃膜的玻璃管端部吹成泡状,管内充填有含饱和AgCl的3mol/l KCL缓冲溶液,pH值为7。存在于玻璃膜二面的反映pH值的电位差用Ag/AgCl传导系统,导出电位差,然后用mA采集仪器将mA数换算成pH值显示出来。The pH value of the extraction process is detected online through the glass electrode produced by Cole-parmer Company, and the change of the pH value of the solution is converted into the change of the mV signal. The glass electrode pH measurement system blows the end of a glass tube with a pH-sensitive glass membrane into a bubble shape, and the tube is filled with a 3mol/l KCL buffer solution containing saturated AgCl, with a pH value of 7. The potential difference reflecting the pH value existing on the two sides of the glass film uses the Ag/AgCl conduction system to derive the potential difference, and then uses the mA acquisition instrument to convert the mA value into a pH value and display it.

本发明采用Cole-parmer公司生产的pH200型酸度控制器进行pH值的就地显示以及检测信号的变送。pH200型酸度控制器利用pH电极对被测溶液中氢离子浓度产生不同的直流电位,通过前置放大器输入到A/D转换器,以达到pH测量的目的,然后由数字显示pH值,同时把pH值转换成电流信号输出。The invention adopts the pH200 acidity controller produced by Cole-parmer Company to display the pH value on the spot and transmit the detection signal. The pH200 acidity controller uses the pH electrode to generate different DC potentials for the concentration of hydrogen ions in the measured solution, which are input to the A/D converter through the preamplifier to achieve the purpose of pH measurement, and then the pH value is displayed digitally, and the The pH value is converted into a current signal output.

萃取过程料液的温度是通过SOLUTION公司生产的铂电阻温度计来进行检测的,铂电阻温度计是利用电气参数随温度变化的特性来检测温度的。The temperature of the feed liquid in the extraction process is detected by the platinum resistance thermometer produced by SOLUTION. The platinum resistance thermometer uses the characteristics of electrical parameters changing with temperature to detect the temperature.

由于有机相不导电,因此对于流量检测采用不同的流量传感器:Since the organic phase is not conductive, different flow sensors are used for flow detection:

(A)水相流量检测:料液、酸液、碱液都导电且具有腐蚀性,选用KROHNE公司生产的具有聚四氟乙烯内衬的电磁流量计进行检测。电磁流量计为无阻力件检测具有精度高、使用寿命长、保养方便等优点。电磁流量计配备的就地显示仪表可以实现流量计就地显示、流量信号变送和流量累计等功能。电磁流量计输出的信号为标准的电流信号。(A) Water phase flow detection: material liquid, acid liquid, and alkali liquid are all conductive and corrosive, and the electromagnetic flowmeter with polytetrafluoroethylene lining produced by KROHNE company is selected for detection. The electromagnetic flowmeter has the advantages of high precision, long service life and convenient maintenance for the detection of non-resistance parts. The local display instrument equipped with the electromagnetic flowmeter can realize the functions of flowmeter local display, flow signal transmission and flow accumulation. The signal output by the electromagnetic flowmeter is a standard current signal.

(B)有机相流量检测:萃取段有机相不导电不能采用电磁流量计,流量的检测选用ELETTA公司生产的差压流量计。其原理是管道中的差压作用在橡胶隔膜上,产生隔膜杆的机械运动,该运动作用在监控器电路板上安装的线性电位器上,由于监控器具有差压和流量之间的线性转换功能,因此电路板就可以提供线性流量输出信号。差压流量计的输出的信号为标准的电流信号。(B) Organic phase flow detection: The organic phase in the extraction section is non-conductive and cannot use an electromagnetic flowmeter. The flow detection uses a differential pressure flowmeter produced by ELETTA. The principle is that the differential pressure in the pipeline acts on the rubber diaphragm to generate mechanical movement of the diaphragm rod, which acts on the linear potentiometer installed on the circuit board of the monitor, because the monitor has a linear conversion between differential pressure and flow function, so the board can provide a linear flow output signal. The output signal of the differential pressure flowmeter is a standard current signal.

上位机选用Core 2 DELL计算机,采用WINDOW XP操作系统。The host computer is a Core 2 DELL computer with WINDOW XP operating system.

组分含量预测与优化操作系统运行在Core 2 DELL计算机上,采用C#2005编程软件,混合模型算法采用Matlab 2007a编程软件。The component content prediction and optimization operating system runs on a Core 2 DELL computer, using C#2005 programming software, and the mixed model algorithm uses Matlab 2007a programming software.

PLC与组分含量预测与优化操作系统的信号传送软件是采用C#2005编程软件。The signal transmission software of PLC and component content prediction and optimization operating system adopts C#2005 programming software.

在萃取过程现场安装检测仪表,检测仪表将采集的信号通过Profibus-DP传送到PLC中,PLC定时将采集信号通过以太网传送给上位机,上位机把接受的数据传给组分含量预测与优化操作系统进行组分浓度在线实时预测,并提供在线的优化操作指导。The detection instrument is installed on site during the extraction process, and the detection instrument transmits the collected signal to the PLC through Profibus-DP, and the PLC regularly transmits the collected signal to the host computer through Ethernet, and the host computer transmits the received data to the component content prediction and optimization The operating system performs online real-time prediction of component concentration and provides online optimization operation guidance.

第一步、机理模型参数辨识:依据萃取平衡实验确定机理模中的萃取平衡关系;The first step, parameter identification of the mechanism model: determine the extraction balance relationship in the mechanism model according to the extraction balance experiment;

(A)配置具有不同浓度被萃组分的水相,并记录水相的体积;(A) Configure the water phase with different concentrations of the extracted components, and record the volume of the water phase;

(B)取一定体积的新鲜有机相,将水相与有机相按一定的相比在分液漏斗内混合,搅拌均匀,静置分层;(B) Get a certain volume of fresh organic phase, mix the water phase and the organic phase in a separatory funnel according to a certain ratio, stir evenly, and let stand to separate layers;

(C)取出水相,化验水相中被萃组分的浓度;(C) take out the water phase, and test the concentration of the extracted component in the water phase;

(D)用差减法计算有机相中被萃组分的浓度,重复上述步骤,并记录实验数据;(D) Calculate the concentration of the extracted component in the organic phase by subtraction, repeat the above steps, and record the experimental data;

(E)利用BFGS算法辨识萃取平衡关系中的未知参数。(E) BFGS algorithm is used to identify unknown parameters in the extraction balance relationship.

第二步、收集数据:收集与离线化验数据对应的传感器测量数据,并记录离线化验数据值ylab(1),...,ylab(n);The second step, collecting data: collecting the sensor measurement data corresponding to the offline test data, and recording the offline test data values y lab (1), ..., y lab (n);

第三步、机理模型预测:利用机理模型对萃余液的被萃组分含量进行预测,并记录与离线化验数据对应的预测结果ymod(1),...,ymod(n);The third step, mechanism model prediction: use the mechanism model to predict the content of the extracted components of the raffinate, and record the prediction results y mod (1), ..., y mod (n) corresponding to the offline test data;

第四步、将预测结果与离线化验值进行比较,并计算预测值与真实值之间的误差值d(1),...,d(n),其中The fourth step, compare the predicted result with the offline test value, and calculate the error value d(1),...,d(n) between the predicted value and the real value, where

d(i)=ylab(i)-ymod(i),i=1,...,n                      (17)d(i) = y lab (i) - y mod (i), i = 1, ..., n (17)

第五步、数据模型建立:将上述误差值与其对应的标准化后的检测值,组成输入输出数据对,利用RBF-PLS方法进行训练,得到数据模型中的参数;The fifth step, data model establishment: the above-mentioned error value and its corresponding standardized detection value are combined to form an input-output data pair, and the RBF-PLS method is used for training to obtain the parameters in the data model;

第六步、混合模型的预测:将所建立机理模型与数据模型的结构组成并行混合模型,利用混合模型对萃余液组分含量进行实时预测;The sixth step is the prediction of the mixed model: the structure of the established mechanism model and the data model are combined into a parallel mixed model, and the mixed model is used to predict the content of the raffinate components in real time;

第七步、混合模型的校正:利用校正算法对混合模型的预测值根据每天的离线化验值进行校在线校正,并输出校正后的预测值;The seventh step, the correction of the mixed model: use the correction algorithm to correct the predicted value of the mixed model according to the daily offline test value, and output the corrected predicted value;

第八步、优化操作指导:利用优化算法,根据操作变量值,提供在线的优化操作指导。The eighth step, optimization operation guidance: use the optimization algorithm to provide online optimization operation guidance according to the value of the operation variable.

表1和图6分别给出了萃余液中Cu的浓度的离线化验值与模型预测值的曲线趋势。Table 1 and Figure 6 respectively show the curve trend of the off-line assay value and model prediction value of Cu concentration in the raffinate.

分析测量数据和混合模型预测值得到预测均方根误差为0.0694,均在本发明所预测值的范围之内,完全满足生产实际的需要。Analyzing the measured data and the predicted value of the mixed model gives a predicted root mean square error of 0.0694, which is within the range of the predicted value of the present invention and fully meets the needs of actual production.

编号serial number   料液浓度Feed liquid concentration   料液流量Feed liquid flow   洗液流量lotion flow   有机相流量Organic phase flow   萃余液pH值Raffinate pH value 温度temperature   萃余液浓度Raffinate concentration   模型预测浓度Model predicted concentration   1 1   14.8914.89   1.251.25   0.200.20   3.003.00   0.510.51   29.229.2   0.380.38   0.360.36   2 2   11.3111.31   1.401.40   0.200.20   2.902.90   0.490.49   28.628.6   0.500.50   0.490.49   33   13.1613.16   1.201.20   0.180.18   4.004.00   0.500.50   9.29.2   0.150.15   0.170.17   ......   ......   2828   17.3717.37   1.201.20   0.200.20   2.002.00   0.540.54   29.529.5   1.741.74   1.821.82   2929   18.1318.13   1.201.20   0.190.19   3.903.90   0.530.53   29.329.3   2.252.25   2.182.18   3030   16.7916.79   1.801.80   0.200.20   4.004.00   0.550.55   27.527.5   1.791.79   1.621.62

表1铜萃取萃余液Cu离子浓度化验值与预测值对比Table 1 Comparison of test value and predicted value of Cu ion concentration in copper extraction raffinate

另外基于前面建立的混合模型,并采用我们设计的优化算法,对该萃取过程进行在线优化指导,依据优化操作条件与现场操作进行对比,累计一个月数据对照结果如表3所示:In addition, based on the previously established mixing model, and using the optimization algorithm designed by us, the extraction process was optimized online and compared with the on-site operation according to the optimized operating conditions. The cumulative data comparison results for one month are shown in Table 3:

  有机相流量(累计)Organic phase flow rate (cumulative)   洗涤液流量(累计)Washing liquid flow (cumulative)   反萃液流量(累计)Stripping liquid flow (cumulative)   历史值historical value   2592.042592.04   116.64116.64   1296.271296.27

  有机相流量(累计)Organic phase flow rate (cumulative)   洗涤液流量(累计)Washing liquid flow (cumulative)   反萃液流量(累计)Stripping liquid flow (cumulative)   优化后值Optimized value   2462.402462.40   103.68103.68   1166.371166.37   节省量Savings   129.64129.64   12.9612.96   129.90129.90   百分比percentage   5.00%5.00%   11.11%11.11%   10.02%10.02%

表2优化结果对照表Table 2 Comparison table of optimization results

本发明将铜萃取组分含量预测界面与优化操作指导界面相结合,协调一致,如图7所示为萃取过程组分含量预测和专家系统优化操作指导统一界面。The present invention combines the copper extraction component content prediction interface with the optimization operation guidance interface, which is coordinated, as shown in Figure 7, which is a unified interface for the extraction process component content prediction and expert system optimization operation guidance.

实施例2Example 2

在P204预萃除杂生产线上的实施。Implementation on the P204 pre-extraction and impurity removal production line.

该生产线上P204预萃取共有20级串级萃取槽,10级用于萃取,3级用于洗涤,3级用于反萃,3级用于反铁,共20台搅拌电机,5个流量计,5台泵,5台变频器,3个pH计,1个温度计组成。萃取过程检测系统主要由流量检测、pH值检测、温度检测构成。There are 20 cascaded extraction tanks for P204 pre-extraction on this production line, 10 for extraction, 3 for washing, 3 for stripping, 3 for anti-iron, a total of 20 stirring motors, 5 flow meters , 5 pumps, 5 inverters, 3 pH meters, and 1 thermometer. The extraction process detection system is mainly composed of flow detection, pH value detection and temperature detection.

编号serial number   料液浓度Feed liquid concentration   料液流量Feed liquid flow   洗液流量lotion flow   有机相流量Organic phase flow   萃余液pH值Raffinate pH value 温度temperature   萃余液浓度Raffinate concentration   模型预测浓度Model predicted concentration   1 1   4.604.60   3.03.0   0.220.22   2.42.4   4.644.64   15.115.1   0.200.20   0.210.21   2 2   6.356.35   2.02.0   0.250.25   3.03.0   4.454.45   12.412.4   0.220.22   0.210.21   33   4.944.94   2.02.0   0.240.24   2.62.6   4.504.50   9.29.2   0.210.21   0.200.20   ......   ......   2828   5.715.71   2.52.5   0.200.20   2.82.8   4.374.37   9.59.5   0.220.22   0.230.23   2929   2.922.92   4.04.0   0.150.15   1.61.6   4.514.51   10.110.1   0.220.22   0.190.19   3030   3.173.17   3.53.5   0.260.26   33   4.604.60   9.69.6   0.150.15   0.160.16

表3萃余液Cu离子浓度化验值与预测值对比Table 3 Raffinate Cu ion concentration test value and predicted value comparison

表3、4和图8、9分别给出了萃余液中Cu、Mn的浓度的离线化验值与模型预测值的曲线趋势。Tables 3 and 4 and Figures 8 and 9 respectively show the curve trends of the off-line assay values and model prediction values of the concentrations of Cu and Mn in the raffinate.

分析测量数据和混合模型预测值的到预测均方根误差分别为0.0231和0.0059,均在本发明所预测值的范围之内,完全满足生产实际的需要。The root mean square errors of the analysis measurement data and the prediction value of the mixed model are respectively 0.0231 and 0.0059, both of which are within the range of the prediction value of the present invention, fully meeting the actual production needs.

编号serial number   料液浓度Feed liquid concentration   料液流量Feed liquid flow   洗液流量lotion flow   有机相流量Organic phase flow   萃余液pH值Raffinate pH value 温度temperature   萃余液浓度Raffinate concentration   模型预测浓度Model predicted concentration   1 1   0.390.39   3.03.0   0.220.22   2.42.4   4.644.64   15.115.1   0.0010.001   0.0030.003   2 2   0.700.70   2.02.0   0.250.25   3.03.0   4.454.45   12.412.4   0.0200.020   0.0210.021   33   0.510.51   2.02.0   0.240.24   2.62.6   4.504.50   9.29.2   0.0210.021   0.0230.023   ......   ......   2828   1.271.27   2.52.5   0.200.20   2.82.8   4.374.37   9.59.5   0.020.02   0.0180.018   2929   0.730.73   4.04.0   0.150.15   1.61.6   4.514.51   10.110.1   0.0220.022   0.0190.019   3030   1.831.83   3.53.5   0.260.26   33   4.604.60   9.69.6   0.0460.046   0.0410.041

表4萃余液Mn离子浓度化验值与预测值对比Table 4 Raffinate Mn ion concentration test value and predicted value comparison

另外基于前面建立的混合模型,并采用我们设计的优化算法,对该萃取过程进行在线优化指导,依据优化操作条件与现场操作进行对比,累计一个月数据对照结果如表3所示:In addition, based on the previously established mixing model and the optimization algorithm designed by us, the extraction process was optimized online and compared with the on-site operation according to the optimized operating conditions. The results of the accumulated one-month data comparison are shown in Table 3:

  有机相流量(累计)Organic phase flow rate (cumulative)   洗涤液流量(累计)Washing liquid flow (cumulative)   反萃液流量(累计)Strip flow (cumulative)   反铁液流量(累计)Anti-ferrous liquid flow (cumulative)   历史值historical value   1259.641259.64   64.8264.82   1310.401310.40   1346.581346.58   优化后值Optimized value   1135.371135.37   57.6057.60   1195.361195.36   1188.491188.49   节省量Savings   124.27124.27   7.227.22   115.04115.04   158.09158.09   百分比percentage   9.87%9.87%   11.13%11.13%   8.78%8.78%   11.74%11.74%

表5优化结果对照表Table 5 Comparison table of optimization results

本发明将P204预萃取组分含量预测界面与优化操作指导界面相结合,协调一致,如图10所示为萃取过程组分含量预测和专家系统优化操作指导统一界面。The present invention combines the P204 pre-extraction component content prediction interface with the optimization operation guidance interface, which is coordinated, as shown in Figure 10, which is a unified interface for the extraction process component content prediction and expert system optimization operation guidance.

本发明在对某湿法冶金萃取车间组分含量进行预测并提供优化操作指导时,友好的人机交互界面也是必不可少的。本发明也充分考虑到这一要求,将总的预测结果与优化操作指导同时列出,如图11、12所示,更便于操作者进行整个萃取工段的监控。When the present invention predicts the component content of a certain hydrometallurgical extraction workshop and provides optimized operation guidance, a friendly human-computer interaction interface is also essential. The present invention also fully takes this requirement into consideration, and lists the overall prediction results and the optimization operation guidance at the same time, as shown in Figures 11 and 12, which is more convenient for the operator to monitor the entire extraction section.

Claims (2)

1. wet-process metallurgic extraction process component content prediction and Optimizing operation method, be the hydrometallurgical extraction technology that adopts known employing multitple extraction groove, it is characterized in that: by hybrid modeling wet-process metallurgic extraction process, realize the real-time estimate of raffinate component concentration, and provide online Optimizing operation to instruct to extraction process, what comprise that the correction of foundation, mixture model of the selection of data acquisition, auxiliary variable and standardization, mixture model and Optimizing operation instruct step such as determines;
1) process data collection
The hardware unit that the present invention uses comprises extraction process component content prediction and Optimizing operation system, host computer, PLC, on-the-spot sensing becomes send part, wherein on-the-spot sensing becomes send part to comprise the pH value, measuring instrument such as temperature and flow, in the on-the-spot installation and measuring instrument of extraction process, measuring instrument is delivered to PLC with the signal of gathering by the Profibus-DP bus, PLC realizes the A/D conversion with the signal of gathering, and regularly acquired signal is sent to host computer by Ethernet, host computer passes to extraction process component content prediction and Optimizing operation system to the local plc data of accepting, carry out the real-time estimate of raffinate component concentration, and provide online Optimizing operation to instruct;
2) selection of auxiliary variable and standardization
The selected auxiliary variable of the present invention comprises:
1. in the feed liquid by collection component concentrations x 1
2. the flow X of feed liquid 2
3. the flow X of washing lotion 3
4. the flow X of organic phase 4
5. the pH value X of raffinate 5
6. the temperature X of feed liquid 6
At first the sensor measurement data that collect are carried out standardization:
x ~ j ( i ) = x j ( i ) - x j ( min ) x j ( max ) - x j ( min )
In the formula -Di i data sample, the standardized value of j measurement value sensor;
x j(i)-and an i data sample, j measurement value sensor;
Figure F200910010295XC00013
The minimum value an of-Di j measurement value sensor;
Figure F200910010295XC00021
The maximal value an of-Di j measurement value sensor;
3) set up mixture model
The present invention adopts the structure of parallel mixture model, adopts the parallel mixture model structure based on non-linear PLS that the not modeling in the mechanism model is dynamically compensated;
The mechanism model that adopts among the present invention mixes limpid device by the m+n level and forms, and wherein the m level is used for extraction, the n level is used for washing; Usually,, can be considered 0, therefore, only consider extraction section and washing section are carried out modeling for simplifying the mechanism model structure through the concentration of each metallic ion in the fresh organic phase behind the stripping section because back extraction, anti-iron efficient are higher,
According to the mass balance relation, for extraction section i level, i=1,2 ... there is following mass balance relation in m-1:
Vy i-1+(L+L′)x i+1=Vy i+(L+L′)x i
And be charging level i=m for extraction section m level, there is following mass balance relation:
Vy m-1+Lx 0+L′x m+1=Vy m+(L+L′)x m
For washing section j level, j=m+1 ..., there is following mass balance relation in n-1:
Vy j-1+L′x j+1=Vy j+L′x j
And for washing section n level, i.e. there is following mass balance relation in j=n:
Vy n-1+L′x′ 0=Vy n+L′x n
V-organic phase flow in the formula;
L-feed liquid flow;
L '-eluent flow;
y i-flow out the organic phase by the collection component concentrations from i level mixer-settler extractor;
x i-flow out the organic phase by the collection component concentrations from i level mixer-settler extractor;
y j-flow out the organic phase by the collection component concentrations from j level mixer-settler extractor;
x j-flow out the organic phase by the collection component concentrations from j level mixer-settler extractor;
y 0Quilt collection component concentrations in the-fresh organic phase;
x 0Quilt collection component concentrations in the-feed liquid;
X ' 0Quilt collection component concentrations in the-washing lotion;
Above-mentioned m+n mass balance relation formed a system of equations with the individual unknown number of 2 (m+n), in order to find the solution above-mentioned system of equations, also needs to introduce the extraction equilibrium relation equation:
y i=f(x i)
The concentration of metallic ion and the unknown function between the aqueous metal ion concentration concern f () in the organic phase when setting up balance ideally, need carry out the experiment of off-line extraction equilibrium to obtain the sample data that is used for identification; At first take out a small amount of fresh organic phase and be used for the extraction equilibrium experiment, prepare water respectively with different metal ion concentration, carry out the extraction equilibrium experiment with separating funnel, organic phase and water are by certain adding separating funnel of comparing, vibration mixes, standing demix, aqueous pH values behind the adjustment is analyzed the aqueous metal ion concentration, and record is used for the experimental data of identification; By analyzing, model can be embodied as semiempirical model:
y ‾ i = f ( x ‾ i ) = a 1 · x ‾ i a 2 + x ‾ i
A in the formula 1, a 2-parameter to be identified;
From the physical significance of above-mentioned radius empirical model, can judge a 1, a 2Value should be greater than 0; Because the result of computation optimization often is not only, tally with the actual situation in order to make result of calculation as far as possible, adopt the nonlinear optimization algorithm of belt restraining below, can be rule of thumb with a 1, a 2Value be limited within certain scope, to above-mentioned radius empirical model y ‾ i = f ( x ‾ i ) = a 1 · x ‾ i a 2 + x ‾ i Carry out reverse computation optimization; Concrete steps are:
1. produce one group at random greater than 0, less than a 1, a 2The initial value of specialized range;
2. with a 1, a 2The substitution following formula calculates y iEstimated value
Figure F200910010295XC00033
3. with sample value and estimated error sum of squares
EMS = Σ i = 1 n ( y ‾ i - y ‾ ^ i ) 2
As the objective function of computation optimization, judge whether objective function meets the requirements, as meet the demands, then stop to calculate, otherwise enter next step;
Y in the formula i-be the observed reading of i sample;
Figure F200910010295XC00035
-be the estimated value of i sample;
N-is the number of sample;
4. carry out the iterative computation of belt restraining condition with the BFGS method, obtain new a 1, a 2
5. repeat 2.~4. step, meet the demands up to objective function;
Adopt non-linear PLS (RBF-PLS) dynamic as the not modeling in the data modeling method compensatory michanism model among the present invention, the RBF-PLS method is by RBF network and PLS algorithm be combined into,
What Optimizing operation instructed determines
The present invention adopts the system based on mixture model to instruct for extraction process provides online Optimizing operation, by exchanging of on-the-spot and operator, obtain the sequence of operations experience, and in conjunction with mixture model, provide the guidance of each performance variable by interative computation, its specific algorithm step is as follows:
1. set each quilt collection component concentrations requirement in the raffinate;
2. read the flow of each come together component concentrations and feed liquid in the feed liquid;
3. according to operator's experience, select a suitable organic phase flow, and eluent flow correspondingly is as initial value;
4. under the aforesaid operations condition, utilize each quilt collection component concentrations in the mixture model prediction raffinate, judge whether up to standard; If do not have one up to standardly, return that 3. the step is reselected an initialization organic phase flow; If all up to standard entering 5. goes on foot;
5. the organic phase flow is reduced Δ V under the condition of above-mentioned initial value, eluent flow adjusts accordingly simultaneously, calls mixture model again, to each is predicted by the collection component concentrations in the raffinate, judges whether up to standard; If do not have one up to standardly, then stop to calculate, have valency phase flow rate and the eluent flow of last time trying to achieve are the Optimizing operation guidance of current time; If all up to standard, then 5. the step repeats.
2. wet-process metallurgic extraction process component content prediction and Optimizing operation method based on mixture model according to claim 1 are to implement on copper collection removal of impurities production line, it is characterized in that:
Copper extraction has 5 grades of cascade extraction grooves on the production line, and 2 grades are used for extraction, and 1 grade is used for washing, and 2 grades are used for back extraction, totally 5 stirring motors, and 4 flowmeters, 4 pumps, 4 frequency converters, 1 pH meter, 1 thermometer is formed; The extraction process detection system mainly is made of flow detector, pH value detector, temperature monitor;
The PLC controller adopts the CPU 315-2DP of Simens 300 series, has the Profibus-DP mouth and connects distributed I/O; For PLC is equipped with the ethernet communication module, be used for host computer visit plc data; PLC controller and ethernet communication module are placed in the PLC cabinet in the central control room;
The pH value of extraction process is to carry out the online detection of pH value by the glass electrode that Cole-parmer company produces, and the variation of pH value of solution value is converted into the variation of mV signal; Glass electrode PH measuring system is blown out blister with a glass tube end for the glass-film of pH sensitivity, and casing pack has the 3mol/l KCL buffer solution that contains saturated AgCl, and the pH value is 7; The potential difference (PD) Ag/AgCl conducting system that is present in the reflection pH value of two of glass-films is derived potential difference (PD), with the mA acquisition instrument mA number is converted into the pH value then and shows;
The pH200 type acidity controller that the present invention adopts Cole-parmer company to produce carries out the change of showing on the spot of pH value and detection signal and send pH200 type acidity controller to utilize the different DC potential of pH generation in the pH electrode pair detected solution, be input to A/D converter by prime amplifier, to reach the purpose that pH measures, show the pH value by numeral then, simultaneously the pH value is converted to current signal output;
The temperature of extraction process feed liquid is to detect by the platinum-resistance thermometer that SOLUTION company produces, and platinum-resistance thermometer utilizes the temperature variant characteristic of electric parameter to come detected temperatures;
Because organic phase is non-conductive, therefore adopt different flow sensors for flow detection:
1. water flow detection: feed liquid, acid solution, alkali lye all conduct electricity and have corrosivity, and the teflon-lined electromagnetic flowmeter that has of selecting for use KROHNE company to produce detects; Electromagnetic Flow is counted non-resistance spare and is detected; The Displaying Meter on the spot that electromagnetic flowmeter is equipped with can realize that flowmeter shows on the spot, the flow signal change is sent and the flux cumulating function; The signal of electromagnetic flowmeter output is the current signal of standard;
2. the organic phase flow detects: the extraction section organic phase is non-conductive can not to adopt electromagnetic flowmeter, the differential pressure flowmeter that the detection of flow selects for use ELETTA company to produce, and the signal of the output of differential pressure flowmeter is the current signal of standard;
Host computer is selected Core 2 DELL computing machines for use, adopts WINDOW XP operating system;
Component content prediction and Optimizing operation system operate on the Core 2 DELL computing machines, adopt the C#2005 programming software, and the mixture model algorithm adopts Matlab 2007a programming software;
It is to adopt the C#2005 programming software that the signal of PLC and component content prediction and Optimizing operation system transmits software;
In the on-the-spot installation and measuring instrument of extraction process, measuring instrument is sent to the signal of gathering among the PLC by Profibus-DP, PLC regularly sends acquired signal to host computer by Ethernet, the data of accepting are passed to component content prediction to host computer and the Optimizing operation system carries out the prediction of concentration of component online in real time, and provide online Optimizing operation to instruct;
The first step, mechanism model parameter identification: determine that according to the extraction equilibrium experiment extraction equilibrium in the mechanism mould concerns:
1. configuration has variable concentrations the come together water of component and the volume of record water;
2. get the fresh organic phase of certain volume, water is mixed by certain comparing in separating funnel with organic phase, stir standing demix;
3. take out water, the chemical examination aqueous phase is by the component concentrations of coming together;
4. calculate quilt collection component concentrations in the organic phase with minusing, repeat above-mentioned steps, and the record experimental data;
5. utilize the unknown parameter in the BFGS algorithm identification extraction equilibrium relation;
Second step, collection data: collect and off-line analysis data corresponding sensor measurement data, and record off-line analysis data value y 1ab(1) ..., y 1ab(n);
The 3rd step, mechanism model prediction: utilize mechanism model that the component concentration that come together of raffinate is predicted, and record the predict the outcome y corresponding with the off-line analysis data Mod(1) ..., y Mod(n);
The 4th step, will predict the outcome and the off-line laboratory values compares, and calculate error amount d (1) between predicted value and the actual value ..., d (n), wherein
d(i)=y 1ab(i)-y mod(i),i=1,...,n
The 5th step, data model are set up: the detected value after the standardization that above-mentioned error amount is corresponding with it, and it is right to form inputoutput data, utilizes the RBF-PLS method to train, and obtains the parameter in the data model;
The prediction of the 6th step, mixture model: the structure of foundation mechanism model and data model is formed parallel mixture model, utilize mixture model that the raffinate component concentration is carried out real-time estimate;
The correction of the 7th step, mixture model: utilize correcting algorithm that the predicted value of mixture model is carried out on-line correction according to the off-line laboratory values of every day, and the predicted value behind the output calibration;
The 8th step, Optimizing operation instruct: utilize optimized Algorithm, according to the performance variable value, provide online Optimizing operation to instruct;
System interface comprises: A reads the main interface that respectively extracts workshop section's off-line analysis data and show predicted data in real time; B provides online Optimizing operation to instruct the interface; C reads the interface of important parameter in the model; The technological process interface that D shows predicted data in real time and provides online Optimizing operation to instruct.
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