CN100516870C - Soft measurement method for SO3 content during phosphoric acid production process by dihydrate wet method - Google Patents
Soft measurement method for SO3 content during phosphoric acid production process by dihydrate wet method Download PDFInfo
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- CN100516870C CN100516870C CNB200610052741XA CN200610052741A CN100516870C CN 100516870 C CN100516870 C CN 100516870C CN B200610052741X A CNB200610052741X A CN B200610052741XA CN 200610052741 A CN200610052741 A CN 200610052741A CN 100516870 C CN100516870 C CN 100516870C
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Abstract
A soft test method uses for measuring SO3 content during the dihydrate wet-process phosphoric acid production process. The content of dissociative vitriol SO3 is the leading variable in phosphoric acid extraction equipment. The assistant variables are pulp flux, vitriol flux, material slurry flux, fluid level, pulp proportion, material slurry proportion, material slurry liquid phase proportion, material slurry liquid solid ratio, phosphorite CaO content, vitriol proportion and vitriol concentration. The dynamic mechanism soft test model of the wet-process phosphoric acid extraction equipment bases on the leading variable and assistant variables and calculate the SO3 content of the phosphoric acid extraction equipment at real time. At natural produce condition, it can exactly forecast the change current to leading variable SO3, and provide great forecast effect at non-normal condition when the key data take place big fluctuate. It has preferable precision with long observation and provides beneficial direction for the production to avoid the fluctuate of the production and establish automatism forecast control.
Description
Technical field
The present invention relates to the chemical process technical field, free sulfuric acid SO in particularly a kind of dihydrate wet phosphoric acid extraction process
3Flexible measurement method.
Background technology
SO in the extraction tank slip
3Content is very important controlling index in the Wet-process Phosphoric Acid Production.By this content of control within the specific limits, make course of reaction obtain suitable phosphogypsum crystal on the one hand in the production, be convenient to follow-up filter operation; Instruct the addition of the raw material concentrated sulphuric acid on the other hand, with the control production cost.In commercial production, produce to instruct by this index of regular chemical examination.Because the routine test frequency is low, is generally chemical examination in, two hour once, thereby can not in time instructs control; In addition, routine sampling is difficult to take into account the difference of CONCENTRATION DISTRIBUTION in the reactor, and the material sample is got by institute might not be representative.When relying on the laboratory analysis in the production run, the normal fluctuation that occurs controlling overshoot and produce controlling index is unfavorable for increasing economic efficiency.Soft-measuring technique is used for estimating the key variables of production run, plays a significant role in growing field.Conventional soft-sensing model is generally static model, is based upon on the stable state hypothesis basis, only considers the single-point corresponding relation between the variable, when bigger fluctuation appears in production, is difficult to obtain correct predicting the outcome even distortion usually.The data point instantaneous value has wild value usually, can not well react the situation of true process.Therefore, need the soft-sensing model or the strategy of dynamic mechanism of a kind of combination and process experience, the relation between the treatment variable preferably predicts the outcome in the hope of correct providing in process of production, revises plan and dispatch command, improves controlling level.
Summary of the invention
The objective of the invention is to regulate untimely problem, production process data is being carried out on the statistical study basis in order to overcome owing to laboratory values lags behind, the operating experience of coupling apparatus operation, the further investigation Principle of Process proposes SO in the dihydrate wet phosphoric acid production run
3The flexible measurement method of content.
SO in the dihydrate wet phosphoric acid production run of the present invention
3The flexible measurement method of content is with free sulfuric acid SO in the phosphoric acid extraction device
3Content is taken variable as the leading factor, with mineral slurry flux, vitriolic acid flux, slip flow, liquid level, ore pulp proportion, slip proportion, slip liquid phase proportion, slip liquid-solid ratio, phosphorus ore CaO content, sulfuric acid proportion and sulfuric acid concentration is auxiliary variable, sets up the dynamic mechanism soft-sensing model of phosphoric acid by wet process extraction equipment:
C
0-C+τ×r-dC/dt＝0
In the formula: C
0Be H
2SO
4Advance reactor concentration; τ is a mean residence time; The H of r for generating
2SO
4Concentration rate is represented during negative value to consume; C is SO in the extraction tank
3Content; Calculate SO in the extraction tank
3During content, with the model prediction result of a last computation period, as introducing soft-sensing model with the multidate information of time correlation.
The invention has the beneficial effects as follows: a kind of phosphoric acid extraction device SO based on dynamic mechanism mathematical model is provided
3The real-time flexible measurement method of content can calculate phosphoric acid extraction device SO in real time
3Content, life period does not lag behind, and in time reflects the situation that the extraction reactor internal-response carries out.Soft-sensing model not only can correctly be estimated leading variable SO under the ordinary production situation
3Variation tendency, open, stop at device, shutdown of short term and owing to also good prediction effect can be arranged when changing the critical data fluctuation of generations such as groove.The long-term observation result has better precision, and anticipation trend can carry out useful guidance to production, the product quality fluctuation of avoiding overshoot to cause.Lay a good foundation for realizing automatic PREDICTIVE CONTROL.
Description of drawings
Fig. 1 is the corresponding simplification device process chart of the present invention that adopts.
Embodiment
The invention will be further described below in conjunction with accompanying drawing.
With reference to phosphoric acid extraction device technique flow process shown in Figure 1, the phosphorus ore slurry is delivered to reactive tank first Room 1 after flowmeter metering and densitometer mensuration; 93～98% the concentrated sulphuric acid is delivered to reactive tank first Room 1 and second Room 2 equally after metering.Phosphorus ore slurry, sulfuric acid and phosphoric acid carry out chemical reaction in reactive tank, generate two (gypsum) crystallization of water thing calcium sulphate and phosphoric acid.Reaction slurry dodges cold ebullator by the low level that is positioned at reactive tank the 3rd Room 3 and circulates, and the cooling slip dodges the fourth ventricle 4 that the cooler power of relying on for support turns back to reactive tank from low level.Dodge the gas of discharging the cooler from low level, the phosphoric acid material pulp of reactive tank fourth ventricle partly overflows to digestive shelf, and to prolong the residence time, slip is sent to filter from digestive shelf through shurry pump.
Dihydrate wet phosphoric acid generates phosphogypsum crystal and relates to consumption H
2SO
4Reactional equation can be expressed as:
(1)CaO+H
2SO
4→CaSO
4+H
2O
(2)MgO+H
2SO
4→MgSO
4+H
2O
(3)CaSO
4+2H
2O→CaSO
4·2H
2O
H
2SO
4Mainly consumed by CaO composition in the rock phosphate in powder, the MgO in the phosphorus ore is to liquid phase SO
3The influence of content shows as: the MgSO that MgO reaction back generates
4To all enter in the phosphoric acid, cause apparent SO in the liquid phase
3Concentration raises, therefore to containing the sulfuric acid that the higher phosphorus ore of MgO just must consider simultaneously that MgO consumes.
SO in the dihydrate wet phosphoric acid production run
3The flexible measurement method of content is at first set up soft measurement mathematical model, and mathematical model is based on following some hypothesis: (1), reactor model is reduced to continuous feed, complete mixing flow (CSTR) reactor of discharging continuously; (2), CaO and H in the extraction tank reactor
2SO
4Reaction, H
2SO
4Be excessive; (3), reaction rate controlled by diffusing step, course of reaction does not have solid film and forms; (4), SO
3Concentration solubleness in slip is high, does not consider that other separate out or lose.With free sulfuric acid SO in the phosphoric acid extraction device
3Content is taken variable as the leading factor, with mineral slurry flux, vitriolic acid flux, slip flow, liquid level, ore pulp proportion, slip proportion, slip liquid phase proportion, slip liquid-solid ratio, phosphorus ore CaO content, sulfuric acid proportion and sulfuric acid concentration is auxiliary variable, and the dynamic mechanism soft-sensing model of setting up the phosphoric acid by wet process extraction equipment is as follows:
C
0-C+τ×r-dC/dt＝0
In the formula: C
0Be H
2SO
4Advance reactor concentration, by reactive tank H
2SO
4Flow and concentration thereof are determined; τ is a mean residence time, is determined by slip volume in the reactive tank and slip flow; The H of r for generating
2SO
4Concentration rate is represented during negative value to consume, and is determined by reactive tank mineral slurry flux and CaO content thereof; C is SO in the extraction tank
3Content is unknown variable.
The instantaneous value of each auxiliary variable or laboratory values read DCS (Distributed Control System (DCS)) item by the host computer at soft measuring system place and obtain.Calculate SO in the extraction tank
3During content, with the model prediction result of a last computation period, as introducing soft-sensing model with the multidate information of time correlation.
Owing to avoided the stable state supposition, and introduced a last execution cycle predicted value relevant with process time and introduced as multidate information, so this model also can have very strong stability and provide correct anticipation trend and result when data fluctuate widely at the scene.
For fear of owing to sampling error or systematic error, obtain reactive tank fourth ventricle SO by timing
3The laboratory assay value, compare with the predicted value in sampling time and judge, proofread and correct according to the correction rule of setting.
The correction rule that the present invention adopts: at first design a soft measuring system evaluation module, make the decision-making whether needs are proofreaied and correct according to the laboratory values of reading in and the deviation of corresponding predicted value by the system evaluation module.Need timing when being judged as,
BIAS＝K×(SO
3_LAB-SO
3_PRED)
BIAS is a correcting action, and K is a correction factor, 0≤K≤1, SO
3_ LAB is sampling time laboratory values, SO
3_ PRED is the sampling time predicted value.BIAS is added the predicted value of current time, and BIAS puts 0 afterwards.
By proofreading and correct, this model can be avoided and may make the problem of model prediction distortion owing to limited several laboratory values of error that exist, and eliminates systematic error.
Claims (3)
1. SO in the dihydrate wet phosphoric acid production run
3The flexible measurement method of content is characterized in that with free sulfuric acid SO in the phosphoric acid extraction device
3Content is taken variable as the leading factor, with mineral slurry flux, vitriolic acid flux, slip flow, liquid level, ore pulp proportion, slip proportion, slip liquid phase proportion, slip liquid-solid ratio, phosphorus ore CaO content, sulfuric acid proportion and sulfuric acid concentration is auxiliary variable, sets up the dynamic mechanism soft-sensing model of phosphoric acid by wet process extraction equipment:
C
0-C+τ×r-dC/dt＝0
In the formula: C
0Be H
2SO
4Advance reactor concentration; τ is a mean residence time; The H of r for generating
2SO
4Concentration rate is represented during negative value to consume; C is SO in the extraction tank
3Content; Calculate SO in the extraction tank
3During content, with the model prediction result of a last computation period, as introducing soft-sensing model with the multidate information of time correlation.
2. SO in the dihydrate wet phosphoric acid production run according to claim 1
3The flexible measurement method of content is characterized in that obtaining SO in the extraction tank by timing sampling
3The laboratory assay value, and compare with the soft measurement predicted value in sampling time and judge, proofread and correct according to the correction rule of setting.
3. SO in the dihydrate wet phosphoric acid production run according to claim 2
3The flexible measurement method of content, it is characterized in that said correction rule is at first to design a soft measuring system evaluation module, make the decision-making whether needs are proofreaied and correct by the system evaluation module according to the laboratory values of reading in and the deviation of corresponding predicted value, need timing when being judged as
BIAS＝K×(SO
3_LAB-SO
3_PRED)
BIAS is a correcting action, and K is a correction factor, 0≤K≤1, SO
3_ LAB is sampling time laboratory values, SO
3_ PRED is the soft measurement predicted value in sampling time, and BIAS is added the predicted value of current time, and BIAS puts 0 afterwards.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103091458B (en) * | 2013-01-09 | 2014-12-10 | 浙江大学 | Soft measurement method for reaction tank slurry phosphoric acid concentration in wet phosphoric acid production process |
| CN105417512B (en) * | 2016-01-25 | 2017-06-16 | 当阳市星光磷化有限公司 | Phosphoric acid by wet process mechanized production system |
| CN106250694B (en) * | 2016-08-01 | 2019-01-29 | 浙江中控软件技术有限公司 | A kind of the quality index flexible measurement method and device of caprolactam product |
| CN108455544A (en) * | 2018-03-30 | 2018-08-28 | 东华工程科技股份有限公司 | A kind of modified dihydrate wet phosphoric acid production system and phosphoric acid preparation method |
| CN112687345B (en) * | 2020-12-28 | 2024-05-14 | 中国科学院过程工程研究所 | Prediction method and prediction device for phosphoric acid extraction process |
| CN113066536A (en) * | 2021-04-19 | 2021-07-02 | 工数科技(广州)有限公司 | Method for optimizing extraction production of phosphoric acid by dihydrate wet method |
| CN115504440B (en) * | 2022-10-29 | 2024-05-14 | 山东联盟磷复肥有限公司 | Double-circulation wet-process phosphoric acid production method |
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