CN1373118A - Intelligent control method for reaction temp in liquid-phase oxidizing reactor of p-xylene - Google Patents
Intelligent control method for reaction temp in liquid-phase oxidizing reactor of p-xylene Download PDFInfo
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Abstract
An intelligent control method for the reaction temp of liquid-phase oxidizing reactor of p-xylene is characterized by that the relative meters are used to measure the variables which can influence the control of reaction temp. such as mixture flow, air flow, reaction pressure, oxygen partial pressure and the flow of pumped-out water, existing distributed control system is also used, and an intelligent system is used to search in intelligent knowledgement library for real-time control.
Description
One, technical field
The invention belongs to the chemical reaction engineering field, relate to p-Xylol (PX, P-xylene) reaction process temperature controlling method in the oxidation reactor in pure terephthalic acid (PTA, the Pure TerephthalicAcid) production.
Two, background technology
In the multiple production technique of crude terephthalic acid (TA, Terephthalic Acid), the PX oxidizing reaction becomes the main flow technology of producing TA gradually with advantages such as its lower acid consumption, material consumptions.Therefore, here in the oxidation reactor intelligence control method of reaction process temperature also be at this production technique.And by distributed control system (DCS, Distributed Control Systems) production process is monitored, all parameters show, monitor, report to the police and control is all carried out in the DCS system.
The PX oxidation reaction process is: raw material (liquid phase P X) is mixed into a kind of acid slurry mutually with certain catalyzer, enters reactor then, generate TA with oxygen reaction under high temperature, high pressure, its main byproduct is 4-CBA.Still unoxidized intermediate product then carries out secondary oxidation in first crystallizer, further reduce the 4-CBA content among the TA.By the crystallization of second and third grade crystallizer, the slurry of generation after filtration, drying obtains TA.
In the PX oxidation reaction process, its quality index be try hard to among the TA (4-CBA, 4-carboxybenzaldehyde) content maintains necessarily in " scope " to carboxyl benzaldehyde.Oxidizing reaction temperature then is the main sign that embodies reaction condition: temperature of reaction is too high, the combustion reactions aggravation, and 4-CBA content reduces, but brings other side reaction simultaneously, causes the increase of other by product; And that reaction temperature is spent is low, does not reach the reaction depth requirement, and 4-CBA content is increased, and increases the weight of the operational load of follow-up secondary oxidation reaction and even refined unit.Therefore we can say that steadily temperature of reaction in the oxidation reactor is the core of smooth running of whole PTA production equipment and production quality control.
Influence the more (see figure 2) of the factor of temperature of reaction in the oxidation reactor, mainly contain: CO in reaction pressure, air input, oxygen partial pressure, the residence time, the reaction end gas in the catalyzer composition in the charging, solvent ratio, reactant concn, the oxidation reactor
2Content, reactor head condenser reflux temperature and quantity of reflux etc.
Because oxidation reactor need be operated under constant voltage, therefore if reactor load is stable, and the parallel feeding concentration proportioning that enters reactor is basicly stable, then the adjustment means of temperature of reaction only have air (oxygen) flow and reactor head condensing reflux flow quantity in the controlled oxidation reactor, and the adjustment of these variablees also can have influence on oxygen level in the tail gas and the water-content in the reactive system etc. simultaneously.As: the reaction end gas oxygen level directly influences production safety, and oxygen level surpasses 10%, and gaseous mixture promptly is in the limits of explosion scope, and oxygen level is low excessively, and then explanation reaction anoxic need be augmented air (oxygen) amount; When water content is higher than 13% (weight) in the reactor, reaction can't be carried out by forward,, can increase the load of solvent dehydration tower again if water content is low excessively.Therefore, temperature of reaction simultaneously, also need be taken into account the variation of tail oxygen concentration, system water content stably in guaranteeing oxidation reactor, suitably determines the amplitude and the frequency of each adjustment variable.
In addition, if under the situation of oxidation reaction process fluctuation of load or under the difference in operation situation of many reactors, also can bring the fluctuation of each component in the whole circulation system (as acid content, water-content and catalyst content etc.), bring bigger difficulty to temperature of reaction control in the reactor.In these cases, only be difficult to reach the steadily requirement of control of temperature with simple single loop control.
It is the gas-liquid-solid phase reaction of middle temperature, middle pressure that the p-Xylol liquid-phase air oxidation is produced terephthalic acid, relate to the chemical engineering problems such as heat transfer, mass transfer, reactive crystallization and solid suspension of gas-liquid phase in the reaction process, and intercouple with multivariable, this brings great difficulty for steady control of reaction process temperature in the reactor.Intelligent control (also be called the expert and control EC, Expert Control) is based on the intelligent control of knowledge, and its major advantage is on the hierarchical structure, have handiness on the control method and in the knowledge representation.Since the notion of intelligent control in 1986 proposes, develop very rapidly, various intelligence control systems have obtained successful Application in being difficult to mathematical model description, multiple coupled and nonlinear Industrial processes.In view of intelligence control system is adapted to occasion highly non-linear or that process prescription is difficult, and in these occasions, traditional controller design method is difficult to prove effective.Therefore, this invention designs a kind of real-time intelligent control method according to the characteristics of oxidation reactor in the PTA production equipment, further improves the quality of PTA product by the temperature of reaction process in the steady controlling reactor.
Three, summary of the invention
(1) goal of the invention
In the PX oxidation reactor, owing to exist intercoupling or disturbing of many process variables, its temperature of reaction control obviously can not be regulated by simple single argument or tandem loop; Therefore, under the situation that the PX oxidation reaction mechanism is not known clearly as yet fully, best control measures be exactly can be comprehensively skilled operator's on-site experience, with its induction-arrangement, form intelligence base, and, form control method with artificial intelligence in conjunction with the DCS resource.In view of this, this goal of the invention is the intelligence control system method that proposes temperature of reaction in a kind of PX oxidation reactor, can guarantee when system water content and tail oxygen level satisfy processing requirement, in real time temperature of reaction in the controlling reactor.
(2) selection of Fa Ming technical scheme 1. intelligence control system reference variables
At the characteristics of PX oxidation reactor, this invention has designed the real-time intelligent Controlling System that has trouble diagnosis; Controlled target is a temperature of reaction in the stopping reaction device, and control measures are for extracting the flow of water out; The Consideration that enters intelligence control system has: the tail oxygen level of extracting discharge and valve position thereof, reactor in the parallel feeding flow of reactor, the air flow quantity of reactor, reactor middle part temperature of reaction, the reactor in reaction pressure, the reactor out.
Here not only adopt the real time data of above-mentioned variable, and used the setting range of mean value, controlled variable and manipulated variable parameter of each variable rolling time section and amplitude limit value thereof etc.2. the method for temperature of reaction intelligence control system in the oxidation reactor
Oxygen level is the main judging criterion of reactor smooth running in temperature of reaction in the reactor (main reference is reactor middle part temperature here) and the tail gas, and they are adjusted indirectly by variablees such as reaction pressures in reactor feed, reactor airload, reactor head lime set backflow extraction water and the reactor usually.
The intelligence control method of temperature of reaction is in the p-Xylol liquid-phase oxidation reactor of the present invention, by measuring the temperature of reaction of oxidation reactor, reaction pressure, the parallel feeding flow, air capacity, reactor head phegma extraction amount, oxygen level in the reaction end gas etc., set up temperature of reaction Controlling System in the oxidation reactor, control enters the stable of material concentration in the compound of oxidation reactor, as catalyst proportion concentration, solvent ratio etc., make it to be complementary, export conditioned reaction pressure respectively when comparing with temperature of reaction and tail oxygen level parameter and standard value with the PX flow, keep extracting out the water yield, the parallel feeding flow, air capacity, reactor head phegma extraction amount.
The controlled variable of temperature of reaction and tail oxygen level, following control embodiment can provide.
The present invention's design philosophy more specifically is:
1) at first guarantees stable (especially catalyzer and promoter concentration is stable) of material proportion in the parallel feeding, to eliminate autoreactor interference in addition;
2) consider that load is to be determined by the explained hereafter condition, so parallel feeding is not as the program calling and controlling means;
3) generally speaking, reaction pressure should be kept relatively stable, that is: corresponding with the reaction depth that requires in the reactor; Therefore, if when temperature of reaction is fixed (remain on a certain value or certain among a small circle in), reaction pressure should guarantee constant voltage operation;
4) air of oxidizing reaction (oxygen) amount should become corresponding relation with parallel feeding, therefore, can set up the suggestion reference flow of air capacity according to the flow situation of different parallel feedings.In addition, because the oxygen level claimed range in the reaction end gas also should make air flow quantity follow the oxygen level variation in the certain limit near reference value and adjust;
5) after above-mentioned 4 conditions are guaranteed, the temperature of reaction adjustment can be extracted how much realizing of the water yield out by adjusting the reactor head backflow in the reactor.For stablizing of water-content in the assurance system, for the separate unit reactor, water yield adjustment will be carried out the scope restriction; For many reactors, water-content can be adjusted respectively according to the adjustable nargin of Current Temperatures.Be the vapour-liquid two-phase owing to reflux in the top, extract the uncertainty of current value out.Therefore can't throw under the situation of " automatically " at the extraction water flow controller, the output of intelligence control system directly can be controlled the valve position of extracting water out;
To sum up, this intelligence system has incorporated the load variations situation, can satisfy the control requirement under work condition state is good, also can satisfy the situation of needs reactor reduction loads such as separate unit filter operation.Like this, guaranteed the operational percentage of intelligence control system on the maximization degree.3. reactor intelligence control system inference mechanism
The intelligence control system here directly provides control signal, influences controlled process.In the case, intelligence control system directly is included in the control loop, and each sampling instant must provide control signal by intelligence control system, and system can move.
It during the native system on-line operation forward reasoning method of taking data to promote, it from raw data to the reasoning of controlled target direction, system is one group of precondition fact providing of Information Monitoring pattern recognition pretreater and knowledge base at first, search in the knowledge base control law that precondition therewith is complementary then, if the match is successful, and be status target, just finish a series of reasoning actions of this rule conclusion; If do not match, then continue the rule that search can be mated, till reaching dbjective state.
In real time the task of search be system under (or a plurality of) objectives guide, the approach that search is set up target, the optimum solution of last problem of comprehensive selection.For the requirement of control in real time, in native system, intelligent knowledge is divided into some stratums of intellectual, different stratums of intellectual is used to find the solution separating of different accuracy, so just can progressively improve separating of problem along with the going deep into of stratum of intellectual." the breadth-first search method " that adopts satisfies the node of goal condition the earliest and enables earlier, and the decision-making that forms in the search " minor matters " is a lot, but not " length ", when this tree of search, the reasoning degree of depth is more shallow like this, and key is rapid " beta pruning ".Adopt this searching algorithm speed fast, not out of control, be fit to real-time reasoning control.
(3) Fa Ming effect
1. the present invention is on the basis that utilizes existing instrument (parallel feeding rate of flow meter, air flowmeter, tail oxygen concentration analyser, extraction discharge/valve position, reactor pressure indicating gauge, thermometer), set up intelligent knowledge base, and can be by real-time reasoning, temperature of reaction in the controlling reactor guarantees that simultaneously oxygen level, water-content are in normal range.
2. control method of the present invention is the basic control law of online modification easily, allows user and system interaction dialogue, the timely dynamic and static information of procurement process, to system carry out in real time, inline diagnosis;
3. this invention can be at separate unit reactor, many reactor multiple situations such as (series and parallels), and the content of invention and method generally are applicable to the control of temperature of reaction in the PX oxidation reactor.
Four, description of drawings
Fig. 1 is an intelligence control system time variable control block diagram of the present invention
Program shown in Fig. 1 and the table 1 is carried out by control device DCS.
Fig. 2 is oxidation reactor structure and parameter control of the present invention and reactant flow synoptic diagram
Five, embodiment:
In the following table, under the reactor load change conditions, intelligence control system itself can be judged according to the heuristic knowledge that is solidificated in the program, if original knowledge experience is changed, then can be undertaken by the people-machine connection interface of intelligence control system talking with program.As: extract the bound of water, the bound of temperature of reaction, the bound of tail oxygen concentration control etc. out, all can in the parameter list of intelligent controller, show.
Table 1 is the execution list (under the constant load situation) of reactor intelligence control system knowledge base
| T mean value (20mins) | Q mean value (20mins) | Intelligence control system output |
| ∈ [T_LO T_HI] normal range | ∈ [Q_LO Q_HI]; Normal range | Reactor is normal; Each variable keeps; |
| ∈ [T_LO T_HI] normal range | ＜Q_LO; Be lower than lower bound | Increase air capacity; Reaction pressure, the extraction water yield keep |
| ∈ [T_LO T_HI] normal range | ＞Q_HI; Be higher than high limit | Reduce air capacity; Reaction pressure, the extraction water yield keep |
| ＞T_HI is higher than high limit | ∈ [Q_LO Q_HI]: normal range | Reduce reaction pressure; Air capacity, the extraction water yield keep |
| ＞T_HI is higher than high limit | ＜Q_HI; Be lower than high limit | The extraction water yield reduces; Reaction pressure, air capacity keep |
| ∈ [T_MID T_HI] normal range, but temperature increase speed＞DelT in certain timed interval simultaneously | ＜Q_HI; Be lower than high limit | Extracting the water valve position out reduces; Reaction pressure, air capacity keep |
| ＞T_HI is higher than high limit | ＞Q_HI; Be higher than high limit | Reactor conditions is unusual; Reaction pressure, air capacity, the extraction water yield keep; Alarm |
| ＜T_LO is lower than lower bound | ∈ [Q_LO Q_HI]; Normal range | Augmenting response pressure; Air capacity, the extraction water yield keep |
| ＜T_LO is lower than lower bound | ＜Q_LO; Be lower than lower bound | Reactor conditions is unusual; Reaction pressure, air capacity, the extraction water yield keep; Alarm |
| ＜T_LO is lower than lower bound | ＞Q_LO; Be higher than lower bound | Extracting the water valve position out increases; Reaction pressure, air capacity keep |
| ∈ [T_LO T_MID] normal range, but temperature reduces speed＞DelT in certain timed interval simultaneously | ＞Q_LO; Be higher than lower bound | Extracting the water valve position out increases; Reaction pressure, air capacity keep |
At first, finish collection by the DCS system to input, output variable information history and real time data; As the data of (as desirable 10 minutes) in current sampling instant one segment limit of related variables such as temperature of reaction distance, the sampling of these data is carried out continuously.
The information that collection comes is sent in the knowledge base and is handled, and the order of processing is carried out according to Fig. 1 and table 1 with the adjustment action; (is well-defined reaction temp, as [180 ℃ 182 ℃] according to knowledge base gained information (being current temperature of reaction, reaction pressure, reactor feed amount and air capacity etc.) with the index of expecting; Normal tail oxygen level is as [2.0 3.0]) compare, it is suitable earlier whether current parallel feeding and air flow quantity to be mated, otherwise air capacity is adjusted (perhaps also can adjust current parallel feeding according to air capacity); Judge one by one according to table 1 then, whether need to adjust the extraction water yield, reaction pressure, air capacity (fine setting), adjust if need, then carry out control output by the program that operates on the DCS, be specially: judge that according to the information of gathering the situation of object is (as the departure degree of current temperature of reaction and normal temps, the variation tendency of (as 10 minutes) in temperature of reaction for some time in the reactor, the departure degree of current tail oxygen concentration and normal tail oxygen concentration, the variation tendency of (as 10 minutes) in tail oxygen concentration for some time, reaction pressure situation judgement etc.), inform that knowledge base enables corresponding adjustment variable, after the adjusting range, drop into control, control performance is approached to the desired destination value.
Here the intelligence control system of Ying Yonging directly acts on controlled member, is included in the control loop, need all will provide control signal in each sampling instant, and system can normally move.In addition, here also add the system monitoring link and carried out real time monitoring, data by intelligence system correlated variables that DCS is gathered are analyzed (as operating restraint detection, rate of change detection, the detection of instrument outlier etc.), unusual circumstance provides alarm, makes the intelligence system controller to the variation of operating mode stronger adaptivity and robustness be arranged.
The condition of above-mentioned requirements all can satisfy, so this invention has universality in most PTA production equipment.
Claims (6)
1, the intelligence control method of temperature of reaction in the p-Xylol liquid-phase oxidation reactor, by measuring the temperature of reaction of oxidation reactor, reaction pressure, the parallel feeding flow, air capacity, reactor head phegma extraction amount, oxygen level in the reaction end gas etc., utilize the intelligence system technology, set up temperature of reaction Controlling System in the oxidation reactor, enter the stable of material concentration in the compound of oxidation reactor in control, comprise catalyst proportion concentration, solvent ratio etc., under the prerequisite that makes it to be complementary, export conditioned reaction pressure respectively when comparing with temperature of reaction and tail oxygen level parameter and standard value with the PX flow, extract the water yield out, the parallel feeding flow, air capacity, reactor head phegma extraction amount.
2, by the intelligence control method of temperature of reaction in the described p-Xylol liquid-phase oxidation reactor of claim 1, it is characterized in that under the constant load situation, is that controlled variable is controlled in the following manner with temperature of reaction and tail oxygen level:
T mean value (20mins) Q mean value (20mins) Intelligence control system output
∈ [T_LO T_HI] normal range ∈ [Q_LO Q_HI]; Normal range Reactor is normal; Each variable keeps;
∈ [TLO T_HI] normal range ＜Q_LO; Be lower than lower bound Increase air capacity; Reaction pressure, the extraction water yield keep
∈ [T_LO T_HI] normal range ＞Q_HI; Be higher than high limit Reduce air capacity; Reaction pressure, the extraction water yield keep
＞T_HI is higher than high limit ∈ [Q_LO Q_HI]; Normal range Reduce reaction pressure; Air capacity, the extraction water yield keep
＞T_HI is higher than high limit ＜Q_HI; Be lower than high limit The extraction water yield reduces; Reaction pressure, air capacity keep
∈ [T_MID T_HI] normal range, but temperature increase speed＞DelT in certain timed interval simultaneously ＜Q_HI; Be lower than high limit Extracting the water valve position out reduces; Reaction pressure, air capacity keep
＞T_HI is higher than high limit ＞Q_HI; Be higher than high limit Reactor conditions is unusual; Reaction pressure, air capacity, the extraction water yield keep; Alarm
＜T_LO is lower than lower bound ∈ [Q_LO Q_HI]; Normal range Augmenting response pressure; Air capacity, the extraction water yield keep
3, by the intelligence control method of temperature of reaction in the described p-Xylol liquid-phase oxidation reactor of claim 1, it is characterized in that having added monitoring link in the intelligence control system, be convenient to realize processing abnormal conditions.
4,, it is characterized in that the knowledge base of this intelligence control system and reasoning link are completely integrated in the DCS system, can guarantee the real-time of controlling by the intelligence control method of temperature of reaction in the described p-Xylol liquid-phase oxidation reactor of claim 1.
5, by the intelligence control method of temperature of reaction in the described p-Xylol liquid-phase oxidation reactor of claim 1, it is characterized in that under the reactor load change conditions, then can be undertaken by the people-machine connection interface of intelligence control system talking with program, promptly extract the bound of water, the bound of temperature of reaction, the bound of tail oxygen concentration control etc. out, all can in the parameter list of intelligent controller, show.
6, by the intelligence control method of temperature of reaction in the described p-Xylol liquid-phase oxidation reactor of claim 1, it is characterized in that the forward reasoning method that the present invention takes data to promote, it from raw data to the reasoning of controlled target direction, system is one group of precondition fact providing of Information Monitoring pattern recognition pretreater and knowledge base at first, search in the knowledge base control law that precondition therewith is complementary then, if the match is successful, and be status target, just finish a series of reasoning actions of this rule conclusion; If do not match, then continue the rule that search can be mated, till reaching dbjective state.
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| CN102375414A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Method for automatically controlling p-xylene adsorption and concentration device |
| CN111574355A (en) * | 2020-03-31 | 2020-08-25 | 南京延长反应技术研究院有限公司 | Intelligent oxidation system and method for preparing terephthalic acid from p-xylene |
| CN111574345A (en) * | 2020-03-31 | 2020-08-25 | 南京延长反应技术研究院有限公司 | Intelligent strengthening reaction system and process for built-in micro-interface unit for producing PTA (purified terephthalic acid) by PX (para-xylene) |
| CN111574341A (en) * | 2020-05-14 | 2020-08-25 | 南京延长反应技术研究院有限公司 | Intelligent reaction system and method for preparing cyclohexanone by selective hydrogenation of benzene |
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- 2002-03-12 CN CNB021127522A patent/CN1166617C/en not_active Expired - Fee Related
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| CN102375414A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Method for automatically controlling p-xylene adsorption and concentration device |
| CN112457155A (en) * | 2019-09-06 | 2021-03-09 | 南京延长反应技术研究院有限公司 | Intelligent enhanced production system and process of 1, 4-butanediol |
| CN112457161A (en) * | 2019-09-06 | 2021-03-09 | 南京延长反应技术研究院有限公司 | Reinforcing system and process for preparing 1, 4-butanediol from acetylene and formaldehyde |
| CN112457162A (en) * | 2019-09-06 | 2021-03-09 | 南京延长反应技术研究院有限公司 | Reinforcing system and process for preparing 1, 4-butanediol by taking n-butane as raw material |
| CN112457156A (en) * | 2019-09-06 | 2021-03-09 | 南京延长反应技术研究院有限公司 | Reinforcing system and process for preparing 1, 4-butanediol from butadiene and acetic acid |
| CN112457165A (en) * | 2019-09-06 | 2021-03-09 | 南京延长反应技术研究院有限公司 | Reinforcing system and process for preparing 1, 4-butanediol by allyl alcohol hydrogenation |
| CN112479840A (en) * | 2019-09-12 | 2021-03-12 | 南京延长反应技术研究院有限公司 | Intelligent control reaction system and process for preparing butanol and octanol through propylene carbonylation |
| CN112479809A (en) * | 2019-09-12 | 2021-03-12 | 南京延长反应技术研究院有限公司 | Intelligent control reaction system and process for preparing ethylene glycol based on ethylene hydration method |
| CN111574355A (en) * | 2020-03-31 | 2020-08-25 | 南京延长反应技术研究院有限公司 | Intelligent oxidation system and method for preparing terephthalic acid from p-xylene |
| CN111574345A (en) * | 2020-03-31 | 2020-08-25 | 南京延长反应技术研究院有限公司 | Intelligent strengthening reaction system and process for built-in micro-interface unit for producing PTA (purified terephthalic acid) by PX (para-xylene) |
| CN111574341A (en) * | 2020-05-14 | 2020-08-25 | 南京延长反应技术研究院有限公司 | Intelligent reaction system and method for preparing cyclohexanone by selective hydrogenation of benzene |
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Owner name: SINOPEC YANGZI PETROCHEMICAL CO.; EAST CHINA UNIV Free format text: FORMER OWNER: YANGZI PETROCHEMICAL CO., LTD.; EAST CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY Effective date: 20080314 |
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Effective date of registration: 20080314 Address after: Nanjing, Jiangsu province Liuhe District Dachang Xinhua Road zip code: 210048 Co-patentee after: East China University of Science and Technology Patentee after: Sinopec Yangzi Petrochemical Co., Ltd. Address before: Dachang District, Jiangsu, Xinhua Road, Nanjing 210048, China Co-patentee before: East China University of Science and Technology Patentee before: Yangzi Petrochemical Limited by Share Ltd |
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Granted publication date: 20040915 Termination date: 20190312 |
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