The process control method copolymerization of acrylyl "b"

 

(57) Abstract:

Use: control of chemical engineering processes, in particular, in the control method of batch polymerization. The inventive method comprises the sequential addition of monomers and solvent. After entering the first dose of initiator in a mixture with solvents to carry out the mixing and heating the reaction mixture at a constant speed to intensive growth temperature vapor. Then regulate the supply of refrigerant in the reverse condenser temperature phlegmy. After stabilization of the temperature in the reactor serves the second dose of initiator in the mixture with the solvent and continue the process of stabilization to break the chain copolymerization, determined to stop the change in the viscosity of the reaction mixture. 1 Il.

The invention relates to the control of chemical engineering processes, in particular to methods for control of batch polymerization.

A known method of controlling the polymerization process by regulating the heat of reaction, which is to regulate the temperature of the refrigerant in the reverse capacitor by changing the flow rate in ocesa polymerization by regulating the heat of polymerization reaction in solution or dispersion, carried out in a reactor equipped with a reflux condenser, which consists in regulating the temperature of the refrigerant in the reverse capacitor by changing the refrigerant flow in the opposite capacitor depending on the temperature of the reaction mass in the reactor, when the temperature in one or more adjacent points in the direction of refrigerant flow in the opposite capacitor [2]

The closest analogue is the way to control the copolymerization process of the production of acrylyl "B", and a linear copolymer of butyl acrylate and amylacetate environment ethyl acetate, comprising the sequential dispensing in a predetermined ratio of monomers and solvent, enter the first dose of initiator, stirring and heating the reaction mixture until intensive growth temperature vapor, after which block the flow of vapor in the heater and open the refrigerant flow in the reverse condenser and jacket, stabilize the temperature in the reactor by varying the pressure of the steam entering the heater temperatures cycle depending on the temperature of hot water flowing into the jacket to heat the reactor, adjustable temperature control in the reactor, then fill in and give a large scatter qualitative indicators of polymerization and significant energy consumption, as well as the duration of the process.

The objective of the proposed invention is to increase the stability of quality indicators while reducing process time and reducing energy consumption.

The technical result is achieved by the fact that in the process control method copolymerization of acrylyl "B" input of the first dose of initiator is carried out in a mixture in a solvent, heating the reaction mixture is conducted at a constant speed in accordance with a predetermined temperature program, when the temperature of solvent vapours (35about(C) stabilization of the temperature in the reactor is carried out in dependence on the temperature of phlegmy output from reverse condensator, affecting the position of the valve of the refrigerant in the feedback capacitor, and when the opening is more than 30% cover steam in heater temperatures cycle, when opening more than 65% proportionally open the supply valve of the refrigerant in TERMOIL, and as ceilings up to 35% dose second dose of initiator, and then return to the previous mode stabilization until breakage of the chain copolymerization, determined to stop the change in the viscosity of reactio krilla "B".

Technological scheme includes a reactor 1, a return condenser 2, a heater 3 temperatures cycle, the pumps 4 and 5, the viscometer 6, capacity 7 to install the viscometer, the selectors 8, 9, 10, 11, 12, 13, 14, regulating valve 15, 16, 17, the temperature sensor 18 (T1) temperature control in the reactor, the temperature sensor 19 (T2) control the water temperature sensor 20 (T3) temperature control phlegmy, electro-pneumatic relays 21 and 22 and the microprocessor 23.

The chart shows the mechanisms and sensors connected respectively with the control channels and data reception microprocessor-based controller.

The schema contains the contours of the temperature control water temperature phlegmy and water circulation.

The contour of temperature control in the reactor 1 is a scheme of interrelated regulation, including the temperature sensor 18 (T1) that is installed in the reactor, and the temperature sensor 19 (T2) installed in the place of merging streams of hot pre-heated in the heat exchanger 3 and chilled coming from the factory network water. At the same time as regulating devices are used, respectively, of the valve 16 and 17 of the steam in the heat exchanger 3 and the cooling water supplied to the mixing with water temperatures cycle in the jacket of the reactor 1. For the tours in the reactor 1 and the set temperature.

The loop temperature control phlegmy at the output of the feedback capacitor 2 refers to the sensor 22 (T3) at the output of phlegmy and control valve 15 to supply cooling water in the condenser 2. Implementation of algorithms for continuous and logical control of the feed of the reactants in the reactor provides in accordance with a given program the microcontroller.

On the command "start" is provided by the installation of the actuators off valves 11, 12, 13, 14 in the initial state and generates requests to load reagents. After the download begins ethyl acetate and butyl acrylate command is sent to heating of the components in the reactor 1. Temperature rise in the reactor 1 should be provided at a given speed, which software is set by the controller. In turn this circuit in accordance with the control algorithm generates the job control loop water temperature entering the jacket of the reactor 1, acting on the valve steam supply to the heater 3 temperatures cycle.

With the increase in temperature in the reactor 1 starts an exothermic reaction of copolymerization, in which there is intense evaporation of ethyl acetate.

When you raise those who odace cooling water in the reactor by feeding commands to the electro-pneumatic actuating valve 17 and change the channel correction setting circuit temperature control hot water loop temperature control phlegmy measured by the sensor 20 (T3by supplying cooling water through the valve 15 in the opposite capacitor 2. The value of the "job" is determined automatically depending on the output signal of the temperature in the reactor.

When you open the valve on the cooling water return condenser 2 by more than 30%, it is necessary to close the control valve 16 and the reliability of the cutter 22 to the steam supply to the heater 3 temperatures cycle, and in further opening in the range of 65-85% proportionally to open the supply valve for the cooling water and thermocycle.

Further the temperature in the reactor 1 T1 support by changing jobs contour sensor 20 (T3) temperature control phlegmy, managing the supply of cold water into the condenser 2. As the exhaustion of the radical groups of the initiator, the reaction of copolymerization starts to fade, which reduces the amount of heat released in the process and to maintain the desired temperature in the reactor 1, the controller 20 (T3) temperature phlegmy begins to cover the valve 15 to supply cooling water return condenser 2. It is obvious that the position of this valve can be used as indirect completeness of the process of sortie initiator, after which at some time again intensifies the reaction of copolymerization. Later in the regulatory process temperature phlegmy valve on the cooling water return condenser is covered up to 75% indicating the need for additional heat in the reactor 1 to compensate for heat loss and stabilization properties of the copolymer. To do this, ensure that the switch channel correction jobs generated by the control loop temperature T1 in the reactor, the control loop temperature T2 of the water in the circulation circuit temperatures cycle, set the path set depending on the output signal of the temperature in the reactor 1. At the same time it is necessary to close the valve on the cooling water in the condenser 2 and to adjust the water temperature in thermocycle by changing the steam supply to the heater 5 temperatures cycle, in the range of 60-80%, it is necessary to proportionally open the valve on the cooling water in the jacket. To improve the dynamic characteristics of control systems it is necessary to provide changes in the tuning parameters of the temperature of hot water in phlegmy. The stabilization of the readings of the viscometer 6 for the circulation konturdurher and delivery of the finished product into the receiving tank.

The use of the proposed method of process control copolymerization of acrylyl "B" allows comparison with the existing reduce by 30% the length of the process, reduce by 15% the energy consumption while improving the stability of indicators of the quality of a copolymer (viscosity at 10%) compared to the prototype.

The PROCESS CONTROL METHOD COPOLYMERIZATION of ACRYLYL "B" linear copolymer of butyl acrylate and vinyl acetate in the environment ethyl acetate, comprising the sequential dispensing in a predetermined ratio of monomers and solvent, enter the first dose of initiator, stirring and heating the reaction mixture to intensive growth temperature vapor, after which block the flow of vapor in the heater and open the refrigerant flow in the reverse condenser and jacket, stabilize the temperature in the reactor by varying the pressure of the steam entering the heater temperatures cycle depending on the temperature of hot water flowing into the jacket to heat the reactor, adjustable temperature control in the reactor, then additionally serves in a mixture with the solvent of the second dose of initiator, characterized in that the input of the first dose of initiator is carried out in a mixture with rastvorimoi, when the temperature of solvent vapours 35oWith the stabilization of the temperature in the reactor is carried out in dependence on the temperature of phlegmy at the output of the feedback capacitor, affecting the position of the valve of the refrigerant in the feedback capacitor, and when the opening is more than 30% cover steam in heater temperatures cycle, when opening more than 65% proportionally open the supply valve of the refrigerant in TERMOIL, and as a cover up to 35% dose second dose of initiator, and then return to the previous mode stabilization until breakage of the chain copolymerization, determined to stop the change in the viscosity of the reaction mixture.

 

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FIELD: organic chemistry, polymers.

SUBSTANCE: invention relates to a method for preparing polyolefins eliciting improved rheological and compatibility properties, and to olefins synthesized by indicated method and their applying also. Method for preparing polyolefins involves: a) grafting stage of acid groups to polyolefins using a grafting monomer comprising at least one functional group taken among carbonyl and acid anhydride residue and if necessary in the presence of another grafting monomer comprising vinyl-unsaturated bond and, possibly, one or some aromatic rings; b) purification stage involving removal of at least part of grafting monomer unreacted with polyolefins and comprising at least one functional group taken among carbonyl and acid anhydride residue; c) stage for neutralization of acid groups using at least one neutralizing agent. Neutralization is carried out with zinc acetate to obtain polyolefins characterizing by the presence of ionic clusters containing ions Zn2+. Also, invention relates to polyolefins obtained by indicated method, to their applying and to a method for extrusion of polyolefins by foaming. Method provides preparing polyolefins eliciting the enhanced stability in melted state and characterizing exponential elevating viscosity value at elongation depending on time and elevating dynamic viscosity at low shift frequencies.

EFFECT: improved preparing method.

22 cl, 3 dwg, 1 ex

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