CN115055134A - Rubber polymerization kettle temperature control system and control method thereof - Google Patents
Rubber polymerization kettle temperature control system and control method thereof Download PDFInfo
- Publication number
- CN115055134A CN115055134A CN202210757450.XA CN202210757450A CN115055134A CN 115055134 A CN115055134 A CN 115055134A CN 202210757450 A CN202210757450 A CN 202210757450A CN 115055134 A CN115055134 A CN 115055134A
- Authority
- CN
- China
- Prior art keywords
- temperature
- heat exchange
- exchange medium
- less
- stirring
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 54
- 229920001971 elastomer Polymers 0.000 title claims abstract description 34
- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 102
- 239000000463 material Substances 0.000 claims abstract description 92
- 238000001816 cooling Methods 0.000 claims abstract description 67
- 238000006243 chemical reaction Methods 0.000 claims abstract description 64
- 230000004913 activation Effects 0.000 claims abstract description 26
- 239000000178 monomer Substances 0.000 claims abstract description 13
- 239000003999 initiator Substances 0.000 claims abstract description 9
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 8
- 230000035484 reaction time Effects 0.000 claims abstract description 7
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 5
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 5
- 230000008859 change Effects 0.000 claims description 82
- 230000001133 acceleration Effects 0.000 claims description 51
- 238000001994 activation Methods 0.000 claims description 38
- 230000001105 regulatory effect Effects 0.000 claims description 31
- 239000007788 liquid Substances 0.000 claims description 18
- 230000001276 controlling effect Effects 0.000 claims description 17
- 230000009471 action Effects 0.000 claims description 2
- 230000007246 mechanism Effects 0.000 abstract description 9
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000003213 activating effect Effects 0.000 abstract 1
- 230000008569 process Effects 0.000 description 12
- 239000012267 brine Substances 0.000 description 4
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 4
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical group COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000013019 agitation Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000010485 coping Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920001084 poly(chloroprene) Polymers 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D23/00—Control of temperature
- G05D23/19—Control of temperature characterised by the use of electric means
- G05D23/30—Automatic controllers with an auxiliary heating device affecting the sensing element, e.g. for anticipating change of temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00054—Controlling or regulating the heat exchange system
- B01J2219/00072—Mathematical modelling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
- B01J2219/00081—Tubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
- B01J2219/00085—Plates; Jackets; Cylinders
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00189—Controlling or regulating processes controlling the stirring velocity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Automation & Control Theory (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a temperature control system of a rubber polymerization kettle and a control method thereof, wherein the temperature control method of the rubber polymerization kettle is used for the temperature control system of the rubber polymerization kettle and comprises the following steps: s1, adding monomers and pre-cooling; s2, adding an initiator and an auxiliary agent; s3, waiting for material activation; s4, activating materials; s5, reacting materials; s6, adding a terminator; s7, adding an antioxidant. In the invention, the stirring frequency conversion of the rubber polymerization kettle is used for accurately controlling the temperature, which is more accurate than the conventional temperature control mode; the invention provides a method for automatically judging whether a material is really activated through a program, which greatly improves the accuracy compared with the conventional judging method; the invention provides a cooperative control method of a plurality of actuating mechanisms, which maximizes the heat release rate of material reaction through cooperative control of the actuating mechanisms, is beneficial to polymerization of material monomers, shortens the reaction time and improves the yield in unit time.
Description
Technical Field
The invention relates to the technical field of temperature control, in particular to a temperature control system of a rubber polymerization kettle and a control method thereof.
Background
The existing method for controlling the temperature of a polymerization kettle basically adjusts the flow of circulating water, frozen brine, heat conduction oil or other heat exchange media to control the temperature. The flow of the heat exchange medium is controlled accurately, and the frequency of the stirring motor is generally kept unchanged or changed in a stepped manner.
The existing temperature control schemes aiming at the reaction kettle in the fine chemical industry can realize the control targets of rapid heating, constant-speed heating, constant temperature and cooling. The control algorithm is variable PID control, cascade control or split control, and the actuating mechanism is generally a valve for regulating the flow of the heat exchange medium.
The prior art has the following disadvantages:
(1) the effect of the frequency of the agitator motor is not taken into account.
(2) There is no method for determining whether the material is activated.
(3) The prior art aims to control the temperature of the feed by controlling the removal of the exothermic heat of polymerization, without involving control of the rate of exothermic polymerization.
Disclosure of Invention
The invention provides a rubber polymerization kettle temperature control system and a control method thereof in order to overcome the defects of the above technology.
The invention aims at certain rubber products, the flow of a heat exchange medium is not the only main influence factor for the temperature of a kettle in the polymerization process of the products, the frequency of a stirring motor is also an important influence factor, namely, the final accurate temperature control mode is realized by adjusting the frequency of the stirring motor.
Interpretation of terms:
1. PID: proportional, integral and differential control is the most common closed-loop control algorithm in automatic control.
2. And (3) cascade control: two PID controllers work in series, with the output of one controller acting as the setpoint for the other.
3. DCS: the Distributed Control System is an English abbreviation of a Distributed Control System.
Summary of the invention:
the monomers are put into a polymerization kettle, then a certain amount of initiator and auxiliary agent are added, and a heat exchange medium is introduced to reduce the temperature of the kettle to be close to the reaction temperature for waiting for the activation of the materials. After the materials are activated, a plurality of actuating mechanisms are controlled to control the temperature, and meanwhile, the reaction heat release rate is guaranteed to be maximized. In the middle and later stages of the reaction, if the reaction rate is reduced or the temperature is too low, the initiator needs to be supplemented. Sampling the density of the tested material after the reaction time is reached, and adding a terminator to end the reaction after the density reaches the standard.
The technical scheme adopted by the invention for overcoming the technical problems is as follows:
the invention discloses a temperature control system of a rubber polymerization kettle, which at least comprises a kettle body, a stirring device, an inner cooling coil, a heat exchange medium pressure pump and a DCS control system, wherein a jacket is wrapped on the outer wall of the kettle body, the inner cooling coil is arranged in the kettle body, a heat exchange medium switch valve is arranged on a liquid inlet end of the heat exchange medium pressure pump, the heat exchange medium pressure pump comprises two liquid outlet ends, one liquid outlet end is connected into the jacket, the other liquid outlet end is connected to the inner cooling coil, an inner cooling coil inlet adjusting valve is arranged at the liquid inlet end of the inner cooling coil, a jacket outlet adjusting valve is arranged at the liquid outlet end of the jacket, and control circuits of the stirring device, the heat exchange medium pressure pump, the heat exchange medium switch valve, the inner cooling coil inlet adjusting valve and the jacket outlet adjusting valve are connected to the DCS control system.
Further, agitating unit includes agitator motor and agitator at least, and the agitator sets up in the cauldron internal and is connected with agitator motor's output.
The invention also discloses a temperature control method of the rubber polymerization kettle, which is used for the temperature control system of the rubber polymerization kettle and comprises the following steps:
s1, adding monomers and pre-cooling: adding a monomer into the kettle body, setting the stirring frequency to be F1, wherein F1 is more than 0Hz, judging whether the initial temperature in the kettle body exceeds a preset T1, if so, pre-cooling, otherwise, directly entering the next step; at this stage, the jacket outlet regulating valve is in a state of being opened all the time;
s2, adding an initiator and an auxiliary agent: adding an initiator and an auxiliary agent into the kettle body, and then executing the next step, wherein the stirring frequency is continuously set to be F1;
s3, waiting for material activation: setting the stirring frequency to be 0Hz, judging whether the material starts to be activated or not, if so, executing the next step, otherwise, continuing to wait until the material starts to be activated, and then entering the next step;
s4, material activation: in the material activation process, the stirring frequency, the on-off or on-off of the heat exchange medium pressure pump, the heat exchange medium switch valve and the inner cooling coil inlet adjusting valve are controlled by a cooperative control method, so that the material is fully activated, the temperature of the activated material can continuously drop under the action of the stirring and heat exchange medium, and when the temperature is lower than a preset T2, the next step is carried out, wherein T2 is less than T1;
s5, material reaction: in the material reaction process, the stirring frequency, the on-off or start-stop of the heat exchange medium pressure pump, the heat exchange medium switch valve and the inner cooling coil inlet adjusting valve are controlled by a cooperative control method to maximize the heat release rate of the material, the material is sampled and tested after the set reaction time is reached, the reaction is ended if the material density reaches the standard, otherwise, the reaction is continued until the material density reaches the standard, and the reaction is ended.
Further, in step S3, determining whether the material is activated specifically includes:
when the temperature change rate exceeds the preset B1, the stirring frequency is increased to F1, and the change condition of the temperature change rate is observed:
if the temperature change rate drops immediately after exceeding B1, the activation is judged to be false activation;
if the time during which the rate of temperature change exceeds B1 and the rate of temperature change exceeds B1 lasts at least 30 seconds, it is determined to be true activation.
Further, after the material is really activated and the temperature change rate is larger than the preset B2, controlling the heat exchange medium switch valve to open, and if the temperature is not reduced after the heat exchange medium switch valve is opened for at least 30 seconds, entering the next step, wherein both B2 and B1 are positive values, and B2 is more than B1.
Further, in step S4, the cooperative control method for the material activation process specifically includes:
if the temperature change rate is less than B3, the temperature acceleration is more than 0.0 and a heat exchange medium pressure pump is not started, setting the stirring frequency to be 0 Hz;
if the temperature change rate is more than B3 and less than B4 and the temperature acceleration is more than 0.0, setting the stirring frequency as F1;
if the temperature change rate is more than B4 and less than B5 and the temperature acceleration is more than 0.0, setting the stirring PID loop to be automatic and starting a heat exchange medium switch valve;
if the temperature change rate is more than 0.0 and less than B5 and the temperature acceleration is more than 0.0, the stirring PID loop is set to be automatic, and the inlet regulating valve of the internal cooling coil is opened;
if the temperature change rate is greater than B5, the temperature acceleration is greater than 0.0, and the temperature is greater than T3, or the temperature is greater than the temperature of the last time of opening the heat exchange medium switch valve +0.6 ℃ and the temperature is greater than T3, setting the stirring PID loop to be automatic, and opening the heat exchange medium pressure pump;
if the temperature change rate is more than B7 and less than B6 and the temperature acceleration is less than 0.0, the stirring PID loop is set to be automatic, and the heat exchange medium pressure pump is closed;
if the temperature change rate is more than B8 and less than B7 and the temperature acceleration is less than 0.0, setting the stirring PID loop to be automatic and closing the heat exchange medium switch valve;
if the temperature change rate is less than B8 and the temperature acceleration is less than 0.0, setting the stirring frequency to be 0 Hz;
if the temperature is lower than the jump temperature +0.8 ℃ in the activation process and the temperature acceleration is lower than J1, closing the heat exchange medium switch valve and the heat exchange medium pressure pump;
when the temperature is lower than the preset T2, the T2 is less than T1, and the next step is carried out;
wherein T3 is less than T2; b3, B4 and B5 are positive numbers, and B3 is more than B4 and more than B5; b6, B7 and B8 are all negative numbers, and B6 is more than B7 is more than B8; j1 is negative.
Further, in step S5, the cooperative control method in the material reaction process specifically includes:
if the temperature change rate is less than B9, the temperature acceleration is more than 0.0, and the heat exchange medium pressure pump is in a closed state, setting the stirring frequency to be 0 Hz;
if the temperature change rate of B9 is less than B10, the temperature acceleration is more than 0.0, and the heat exchange medium pressurizing pump is in a closed state, setting the stirring frequency to be F1;
in 60 minutes, if the temperature change rate is more than B10 and less than B11, the temperature acceleration is more than 0.0, the temperature deviation is more than P1 and less than P2, and the temperature deviation is a numerical value obtained by subtracting a temperature set value from the actual temperature in the kettle body, setting the stirring PID loop to be automatic, and starting a heat exchange medium switch valve;
if the temperature change rate is more than B11 and less than B12, the temperature acceleration is more than 0.0, and the temperature deviation is more than P1 and less than P2, the stirring PID loop is set to be automatic, and the inlet regulating valve of the internal cooling coil is opened;
if the temperature change rate is less than B12, the temperature acceleration is more than 0.0, the temperature is more than T3, or the temperature is more than or equal to the temperature of the last time of opening a heat exchange medium switch valve plus 0.6 ℃, setting the stirring PID loop to be automatic, and opening an inlet regulating valve of the inner cooling coil;
if the temperature change rate is more than B13 and less than B14, the temperature acceleration is less than 0.0, the temperature deviation is more than P1 and less than P2, or the temperature deviation is less than P3, the heat exchange medium pressure pump is closed;
if the temperature change rate is less than B14 and the temperature acceleration is less than 0.0, setting the stirring frequency to be F2, and closing the heat exchange medium switch valve;
when the timing of the material reaction process is more than 30 minutes, if the heat exchange medium switch valve and the inlet regulating valve of the inner cooling coil are in an open state, the temperature deviation is more than P4, and the stirring frequency is more than F3, the heat exchange medium pressure pump is started, and the stirring frequency is reduced to F2;
wherein, B9, B10, B11 and B12 are positive numbers, and B9 is more than B10 and more than B11 and more than B12; b13 and B14 are both negative numbers, and B13 < B14; f2 < F1 < F3; p1, P2, P3 and P4 are all negative numbers, and P2 is more than P1 is more than P4 is more than P3.
Further, after the material activation process of step S4 and the material reaction process of step S5 are timed to sum up to > 240 minutes, in the period:
if the temperature deviation is more than P1, opening the heat exchange medium switch valve and the inner cooling coil inlet regulating valve, otherwise, closing the heat exchange medium switch valve and the inner cooling coil inlet regulating valve;
and if the temperature deviation is P5 < P1, wherein P2 > P1 > P5 > P4 > P3, the heat exchange medium pressurizing pump is started, and otherwise, the heat exchange medium pressurizing pump is closed.
Further, step S6 is further included after step S5, and step S6 specifically includes:
after the reaction is completed, a terminator is added to terminate the reaction.
Further, step S7 is further included after step S6, and step S7 specifically includes:
after the reaction is terminated, an antioxidant is added to complete the reaction.
The invention has the beneficial effects that:
the invention improves the temperature control scheme of the existing polymerization kettle, provides a judgment method for judging the activation point of the material, and provides a method for maximizing the reaction heat release rate.
(1) In the invention, the stirring frequency conversion of the rubber polymerization kettle is used for accurately controlling the temperature, which is more accurate than the conventional temperature control mode, and the accuracy can reach a set value +/-1 ℃.
(2) At present, whether the material is activated or not is judged manually, the accuracy rate is low, and more operation experience of technicians is relied on. Even if the judgment is wrong, a corresponding coping strategy is available.
(3) The invention provides a cooperative control method of a plurality of actuating mechanisms, which maximizes the heat release rate of material reaction through cooperative control of the actuating mechanisms, is beneficial to polymerization of material monomers, shortens the reaction time, shortens 20-30 minutes per production batch on average, and improves the yield per unit time.
Drawings
FIG. 1 is a schematic diagram of a rubber polymerizer temperature control system according to an embodiment of the invention. In figure 1, a kettle body, 2, a stirring device, 3, an inner cooling coil, 4, a heat exchange medium pressure pump, 5, a jacket, 6, a heat exchange medium switch valve, 7, an inner cooling coil inlet regulating valve, 8 and a jacket outlet regulating valve.
FIG. 2 is a temperature profile of a rubber polymerizer temperature control method according to an embodiment of the invention.
FIG. 3 is a flowchart of a method for controlling the temperature of a rubber polymerizer, according to an embodiment of the invention.
FIG. 4 is a graph showing the temperature change rate of activated material with time according to the embodiment of the present invention.
Fig. 5 is a schematic diagram of a cooperative control method of an actuator according to an embodiment of the present invention.
FIG. 6 is a graph showing a comparison of the trend of the temperature of a polymerization vessel in accordance with the present invention, which is controlled by automatic temperature control and manual temperature control.
Detailed Description
In order to facilitate a better understanding of the invention for those skilled in the art, the invention will be described in further detail with reference to the accompanying drawings and specific examples, which are given by way of illustration only and do not limit the scope of the invention.
The system for controlling the temperature of a rubber polymerizer according to the present invention will be specifically described by taking a system for synthesizing rubber shown in fig. 1 as an example.
The rubber polymerization kettle temperature control system at least comprises a kettle body 1, a stirring device 2, an inner cooling coil 3, a heat exchange medium pressure pump 4 and a DCS control system. Agitating unit 2 includes agitator motor and agitator at least, and the agitator sets up in the cauldron body 1 and is connected with agitator motor's output, drives the agitator through agitator motor and rotates the internal material of stirred tank. The outer wall of the kettle body 1 is wrapped with a jacket 5, the inner cooling coil 3 is arranged in the kettle body 1 and spirally arranged to ensure good cooling effect, a liquid inlet end of a heat exchange medium pressure pump 4 is provided with a heat exchange medium switch valve 6, the heat exchange medium pressure pump 4 comprises two liquid outlet ends, one liquid outlet end is connected into the jacket 5, and the other liquid outlet end is connected to the inner cooling coil 3, namely, the heat exchange medium can be introduced into the jacket 5 and also into the inner cooling coil 3 through the heat exchange medium pressure pump 4; the heat exchange medium is introduced into the jacket from the lower part of the jacket 5 and discharged from the upper part of the jacket, and the heat exchange medium is introduced from the lower part of the inner cooling coil 3 and discharged from the upper part of the inner cooling coil. The heat exchange medium is preferably frozen brine at-15 ℃, although other heat exchange media can be used, and the use of frozen brine is not a limitation of the present invention. The liquid inlet end of the inner cooling coil 3 is provided with an inner cooling coil inlet adjusting valve 7, and the liquid outlet end of the jacket 5 is provided with a jacket outlet adjusting valve 8. The stirring device 2, the heat exchange medium pressure pump 4, the heat exchange medium switch valve 6, the inner cooling coil inlet adjusting valve 7 and the jacket outlet adjusting valve 8 are all electrically connected to a DCS control system, wherein the DCS control system can adopt any control system capable of controlling starting and stopping of each actuating mechanism (namely, the stirring device 2, the heat exchange medium pressure pump 4, the heat exchange medium switch valve 6, the inner cooling coil inlet adjusting valve 7 and the jacket outlet adjusting valve 8).
The method for controlling the temperature of the rubber polymerizer described in this embodiment is implemented by a DCS system, and specifically includes the following steps, as shown in fig. 3, the whole temperature control process is divided into 7 stages, that is, the following 7 steps:
step S1 (stage 1), adding monomer and pre-cooling
Adding a monomer into the kettle body 1, wherein the monomer is a material for synthesizing rubber, the rubber is chloroprene rubber, the stirring frequency of a stirring motor is set to be F1, preferably, F1 is 5Hz in the embodiment, judging whether the initial temperature in the kettle body exceeds preset T1, and if the initial temperature exceeds T1, pre-cooling is carried out, otherwise, the next step is directly carried out. In the embodiment, T1 is preferably 16 ℃, namely, if the temperature exceeds 16 ℃, the temperature is reduced; the initial temperature is generally 20-22 ℃, so the temperature is basically reduced through a pre-cooling stage. During the whole temperature control process, the jacket outlet regulating valve 8 is always in an open state.
Step S2 (stage 2), addition of initiator and auxiliary
Adding a certain amount of initiator and auxiliary agent into the kettle body 1, wherein the auxiliary agent is preferably dimethyl ether; the next step is then carried out during which the stirring frequency is continued to be F1, i.e. 5 Hz.
Step S3 (stage 3), waiting for material activation
The stirring frequency is set to be 0Hz, the temperature of the materials is slowly reduced before the materials are activated, and the temperature change rate is a negative value. And judging whether the material starts to be activated or not in real time, if so, executing the next step, otherwise, continuously waiting until the material starts to be activated, and then entering the next step.
The material has two conditions of true activation and false activation, and the technical key point of the invention is to judge whether the material is true activation. Before the material is activated, the stirring frequency is lowest, the material temperature is slowly reduced, and the kettle temperature change rate is a negative value. When the material is activated, the temperature in the kettle starts to continuously rise, and the method for judging whether the material is activated is as follows:
when the temperature change rate exceeds the preset B1, the stirring frequency is increased to F1, and the change condition of the temperature change rate is observed:
if the temperature change rate exceeds B1 and the stirring frequency drops immediately after increasing to F1, the activation is judged to be false activation;
if the time during which the temperature change rate exceeds B1 and the stirring frequency is increased to F1, the kettle temperature continues to rise and the temperature change rate exceeds B1 continues for at least 30 seconds, it is determined as true activation.
In this embodiment, B1 is preferably 0.07 ℃/s, and as shown in fig. 4, the vertical axis in the figure represents the rate of change and the horizontal axis represents time. The dotted line is the value 0 of the rate of change, the rate of change above the dotted line is positive, the rate of change below the dotted line is negative, and the curve is the actual rate of change in temperature. In fig. 4, after the temperature change rate reaches 0.07 ℃/s for the first time, the stirring frequency is set to 5Hz, and the temperature change rate is immediately reduced, which indicates that the reaction exotherm is small, and is pseudo-activation; and after the temperature change rate exceeds 0.07 ℃/s for the second time and the stirring frequency is 5Hz, the temperature change rate continues to rise, and if the time of more than 0.07 ℃/s lasts for more than 30 seconds, the activation is considered to be true.
After the material is activated and the temperature change rate is greater than a preset value B2, wherein both B2 and B1 are positive values and B2 is greater than B1, in this embodiment, preferably, B2 is 0.25 ℃/s, the heat exchange medium switch valve 6 is controlled to be opened, and if the temperature of the heat exchange medium switch valve 6 is not reduced after being opened for at least 30 seconds, the next step is performed.
Step S4 (stage 4), Material activation
In the material activation process, the temperature may be pressed down again, the temperature fluctuates for a plurality of times, the stirring frequency, the opening and closing or starting and stopping of the heat exchange medium pressurizing pump 4, the heat exchange medium switch valve 6 and the inner cooling coil inlet adjusting valve 7 are controlled by a cooperative control method, so that the material is fully activated, and when the temperature is lower than the preset T2, wherein T2 is less than T1, the next step is carried out.
The cooperative control method for the material activation process specifically comprises the following steps:
the temperatures, temperature rates and temperature accelerations involved in this phase are set and assigned values before a specific material activation coordinated control process is introduced. T3 < T2; b3, B4 and B5 are positive numbers, and B3 is more than B4 and more than B5; b6, B7 and B8 are all negative numbers, and B6 is more than B7 is more than B8; j1 is negative. The assigned values are not intended to limit the present invention, but are merely preferred values of the present embodiment, and specific assigned values of the present embodiment are placed in parentheses after the temperature, the temperature change rate, and the temperature acceleration. The temperature control process of the stage 4 is sequentially executed according to the following sequence:
if the temperature change rate is less than B3(0.05 ℃/s), the temperature acceleration is more than 0.0, and the heat exchange medium pressure pump 4 is not started, setting the stirring frequency to be 0 Hz;
if the temperature change rate is more than B3(0.05 ℃/s) and less than B4(0.15 ℃/s) and the temperature acceleration is more than 0.0, setting the stirring frequency to be F1(5 Hz);
if the temperature change rate is more than B4(0.15 ℃/s) and less than B5(0.32 ℃/s) and the temperature acceleration is more than 0.0, setting the stirring PID loop to be automatic, and starting the heat exchange medium switch valve 6; in the embodiment, when the stirring PID loop is set to be automatic, the manual stirring program does not work any more, and only when the automatic condition of the stirring PID loop is switched, the manual stirring program works;
if the temperature change rate is more than 0.0 and less than B5(0.32 ℃/s) and the temperature acceleration is more than 0.0, setting the stirring PID loop to be automatic, and opening the inlet regulating valve 7 of the inner cooling coil;
if the temperature change rate is more than B5(0.32 ℃/s), the temperature acceleration is more than 0.0, and the temperature is more than T3(8.5 ℃), or the temperature is more than the temperature of starting the heat exchange medium switch valve 6 last time plus 0.6 ℃ and the temperature is more than T3(8.5 ℃), setting the stirring PID loop to be automatic, and starting the heat exchange medium pressure pump 4;
if the temperature change rate is more than B7(-0.45 ℃/s) and less than B6(-0.35 ℃/s) and the temperature acceleration is less than 0.0, setting the stirring PID loop to be automatic, and closing the heat exchange medium pressure pump 4;
if the temperature change rate is more than B8(-0.60 ℃/s) and less than B7(-0.45 ℃/s) and the temperature acceleration is less than 0.0, setting the stirring PID loop to be automatic, and closing the heat exchange medium switch valve 6;
if the temperature change rate is less than B8(-0.60 ℃/s) and the temperature acceleration is less than 0.0, setting the stirring frequency to be 0 Hz;
if the temperature is less than the jump temperature of the activation process plus 0.8 ℃ and the temperature acceleration is less than J1(-0.2 ℃/s) 2 ) If so, closing the heat exchange medium switch valve 6 and the heat exchange medium pressure pump 4;
when the temperature is lower than the preset T2(12 ℃), the next step is carried out.
The values of the temperature, the temperature change rate, and the temperature acceleration are all the optimal preferred values of the present embodiment, but are not limited to these specific values, and the temperature control process of the stage 4 can also be implemented when values near these values are taken.
Step S5 (stage 5), material reaction: in the reaction process of the materials, the stirring frequency, the opening and closing or starting and stopping of the heat exchange medium pressurizing pump 4, the heat exchange medium switch valve 6 and the inner-cooling coil inlet adjusting valve 7 are controlled by a cooperative control method to maximize the heat release rate of the materials, the materials are sampled and tested after the reaction time is reached, if the density reaches the standard, the reaction is ended, otherwise, the reaction is continued until the density of the materials reaches the standard, and the reaction is ended.
The second technical key point of the invention is a method for controlling the exothermic rate of the material reaction. The control target of the material reaction is not only accurate temperature control, but also the reaction heat release rate is controlled, so that the reaction is carried out under the condition of full heat release, the polymerization of material monomers is facilitated, the reaction time can be shortened, and the yield per unit time is improved. However, because the reaction heat release rate cannot be measured, the heat release rate of the material reaction is reflected by the starting and stopping conditions of actuating mechanisms (comprising the stirring device 2, the heat exchange medium pressurizing pump 4, the heat exchange medium switch valve 6, the inner cooling coil inlet adjusting valve 7 and the jacket outlet adjusting valve 8), and the actuating mechanisms have different degrees of influence on the kettle temperature and different control accuracies. In the process of the reaction from weak to strong, a heat exchange medium switch valve 6, a heat exchange medium pressure pump 4, a jacket outlet regulating valve 8 and an inner cooling coil inlet regulating valve 7 are opened in sequence, and finally the stirring frequency is used for accurately controlling the temperature. For example: when the heat exchange medium pressure pump 4, the heat exchange medium switch valve 6, the inner cooling coil inlet regulating valve 7 and the jacket outlet regulating valve 8 are fully opened, the flow of the heat exchange medium (namely, the frozen brine) is maximized, and the stirring frequency is relatively high, the heat exchange quantity is maximized, the heat release rate is maximized, and the temperature control under the working condition is optimal.
The cooperative control method in the material reaction process specifically comprises the following steps:
before describing a specific material reaction cooperative control process, the temperature change rate, the stirring frequency and the temperature deviation involved in the stage are set and assigned. B9, B10, B11 and B12 are positive numbers, and B9 is more than B10 and more than B11 and more than B12; b13 and B14 are both negative numbers, and B13 < B14; f2 < F1 < F3; p1, P2, P3 and P4 are all negative numbers, and P2 is more than P1 is more than P4 is more than P3. The values given are not intended to limit the invention, but are preferred values in this example, with specific values placed in parentheses after the rate of change of temperature, the frequency of agitation, and the temperature deviation. The temperature control process of the stage 5 is not necessarily performed in the following order, but may be performed as long as these control conditions are satisfied:
if the temperature change rate is less than B9(0.01 ℃/s), the temperature acceleration is more than 0.0, and the heat exchange medium pressure pump 4 is in a closed state, setting the stirring frequency to be 0 Hz;
if the temperature change rate of B9(0.01 ℃/s) is less than B10(0.03 ℃/s), the temperature acceleration is more than 0.0, and the heat exchange medium pressure pump 4 is in a closed state, setting the stirring frequency to be F1(5 Hz);
in 60 minutes, if the temperature change rate is more than B10(0.03 ℃/s) and less than B11(0.08 ℃/s), the temperature acceleration is more than 0.0, the temperature deviation is more than P1(-0.31 ℃) (less than P2(-0.2 ℃), and the temperature deviation is a numerical value obtained by subtracting a temperature set value from the actual temperature in the kettle body, setting the stirring PID loop to be automatic, starting the heat exchange medium switch valve 6, and setting the stirring frequency to be F1(5 Hz);
if B11(0.08 ℃/s) < temperature change rate < B12(0.35 ℃/s), temperature acceleration > 0.0, P1(-0.31 ℃) < temperature deviation < P2(-0.2 ℃), setting the stirring PID loop to be automatic, and opening the inlet regulating valve 7 of the inner cooling coil;
if the temperature change rate is less than B12(0.35 ℃/s), the temperature acceleration is more than 0.0, and the temperature is more than T3(8.5 ℃), or the temperature is more than or equal to the temperature of the last time of opening the heat exchange medium switch valve 6 plus 0.6 ℃, the stirring PID loop is set to be automatic, and the inlet regulating valve 7 of the inner cooling coil is opened;
if B13(-0.5 ℃/s) < the temperature change rate < B14(-0.3 ℃/s), the temperature acceleration < 0.0, and P1(-0.31 ℃) < the temperature deviation < P2(-0.2 ℃), or the temperature deviation < P3(-1.5 ℃), closing the heat exchange medium pressure pump 4;
if the temperature change rate is less than B14(-0.3 ℃/s) and the temperature acceleration is less than 0.0, setting the stirring frequency to be F2(2Hz), and closing the heat exchange medium switch valve 6;
when the timing of the material reaction process is more than 30 minutes, if the temperature deviation is more than P4(-1.0 ℃) and the stirring frequency is more than F3(10Hz) when the heat exchange medium switch valve 6 and the inner cooling coil inlet adjusting valve 7 are in the open state, the heat exchange medium pressure pump 4 is started, and meanwhile, the stirring frequency is reduced to F2(2 Hz). At the moment, the heat exchange medium switch valve 6, the inner cooling coil inlet regulating valve 7 and the heat exchange medium pressurizing pump 4 are all opened, and the stirring frequency is adjusted to control the temperature, so that the optimal reaction working condition is realized, and the reaction heat release rate is maximized.
Further, after the total of the timing of the material activation process of step S4 and the material reaction process of step S5 was > 240 minutes, during this period:
if the temperature deviation is more than P1(-0.31 ℃), opening the heat exchange medium switch valve 6 and the inner cooling coil inlet regulating valve 7, otherwise, closing the heat exchange medium switch valve 6 and the inner cooling coil inlet regulating valve 7;
if the temperature deviation is more than P5(-0.5 ℃) < P1(-0.31 ℃), the heat exchange medium pressure pump 4 is started, otherwise, the heat exchange medium pressure pump 4 is closed.
In steps S4 and S5, the heat exchange medium switch valve 6, the internal cooling coil inlet regulating valve 7, the heat exchange medium pressure pump 4, and the start and stop of the stirring are in a fixed sequence, as shown in fig. 5, the next operation can be performed when the start condition is met, and the operation is backed up when the stop condition is met, the four actuators (the stirring device 2, the heat exchange medium switch valve 6, the internal cooling coil inlet regulating valve 7, and the heat exchange medium pressure pump 4) form a closed loop, the left row represents that the heat exchange medium switch valve 6, the internal cooling coil inlet regulating valve 7, and the heat exchange medium pressure pump 4 are opened or the stirring device 2 is turned on automatically, and the right row represents that the heat exchange medium switch valve 6, the internal cooling coil inlet regulating valve 7, and the heat exchange medium pressure pump 4 are closed or the stirring device 2 is turned manually. This is also the third technical key point of the present invention.
Step S6 (stage 6), adding terminator
After the reaction is finished, a certain amount of terminator is added to terminate the reaction, and then the next step is carried out.
Step S7 (stage 7), adding antioxidant
After the reaction is terminated, a certain amount of antioxidant is added, so that the oxidation reaction of the materials can be avoided when the materials contact air, the characteristics of the materials are kept stable, and then the whole temperature control process is finished.
According to the above 7 steps (7 stages) division, the temperature curve is drawn as shown in fig. 2, and it can be known from fig. 2 that the temperature trend is slowly decreased from stage 1 to stage 4, but it is not required to be controlled on a certain temperature curve, wherein, in fig. 2, the temperature of the whole stage 3 is decreased, because the temperature is only temporarily increased during activation, once the activation is judged, the temperature is pressed, the process time is short, so when the horizontal axis coordinate time span is large, that is, the temporary temperature increase during the activation of stage 3 is not visible in the curve given in fig. 2. Starting from the stage 5, the materials are activated, and the temperature is controlled to be a little lower in the early stage of the reaction (about the first 1 hour of the stage 5), so that the condition that the reaction is too fast and the control cannot be realized in the later stage is prevented; the temperature is properly increased a little in the middle stage of the reaction (about 2 to 4 hours in stage 5); in the later stage of the reaction (after stage 5 until the end of the reaction) the monomer is consumed and the reaction temperature is raised a little more to ensure the reaction continues.
Next, we will look at the automatic temperature control process and the manual temperature control process through a set of comparative graphs, as shown in fig. 6, showing the kettle temperature trends of three batches of a certain polymerization kettle, in which curve a is the actual kettle temperature and curve C is the temperature set value. The first batch on the left side is an automatic temperature control curve, and the two batches on the right side are manual temperature control curves. The comparison shows that the fluctuation range of the temperature of the automatic temperature control is much smaller than that of the manual temperature control, and is about more than 50 percent, which shows that the temperature control precision of the rubber polymerization kettle temperature control method can reach a set value of +/-1 ℃, the kettle temperature control is accurate and stable, and the quality and the stability of a polymerization product can be improved.
The foregoing merely illustrates the principles and preferred embodiments of the invention and many variations and modifications may be made by those skilled in the art in light of the foregoing description, which are within the scope of the invention.
Claims (10)
1. The temperature control system of the rubber polymerization kettle is characterized by at least comprising a kettle body (1), a stirring device (2), an inner cooling coil (3), a heat exchange medium pressure pump (4) and a DCS control system, wherein the outer wall of the kettle body (1) is wrapped by a jacket (5), the inner cooling coil (3) is arranged in the kettle body (1), a heat exchange medium switch valve (6) is arranged at a liquid inlet end of the heat exchange medium pressure pump (4), the heat exchange medium pressure pump (4) comprises two liquid outlet ends, one liquid outlet end is connected into the jacket (5), the other liquid outlet end is connected into the inner cooling coil (3), an inner cooling coil inlet adjusting valve (7) is arranged at a liquid inlet end of the inner cooling coil (3), a jacket outlet adjusting valve (8) is arranged at a liquid outlet end of the jacket (5), the stirring device (2), the heat exchange medium pressure pump (4), the heat exchange medium switch valve (6) and the inner cooling coil (3), Control circuits of an inlet adjusting valve (7) and a jacket outlet adjusting valve (8) of the inner cooling coil are connected to the DCS control system.
2. The temperature control system of the rubber polymerization kettle according to claim 1, wherein the stirring device (2) at least comprises a stirring motor and a stirrer, and the stirrer is arranged in the kettle body (1) and is connected with the output end of the stirring motor.
3. A rubber polymerizer temperature control method, which is used for the rubber polymerizer temperature control system of claim 1 or 2, comprising the steps of:
s1, adding monomers and pre-cooling: adding a monomer into the kettle body (1), setting the stirring frequency to be F1, wherein F1 is more than 0Hz, judging whether the initial temperature in the kettle body exceeds a preset T1, if so, pre-cooling, otherwise, directly entering the next step; at this stage, the jacket outlet regulating valve (8) is in a state of being opened all the time;
s2, adding an initiator and an auxiliary agent: adding an initiator and an auxiliary agent into the kettle body (1), and then executing the next step, wherein the stirring frequency is continuously set to be F1;
s3, waiting for material activation: setting the stirring frequency to be 0Hz, judging whether the material starts to be activated or not, if so, executing the next step, otherwise, continuing to wait until the material starts to be activated, and then entering the next step;
s4, material activation: in the material activation process, the stirring frequency, the heat exchange medium pressure pump (4), the heat exchange medium switch valve (6) and the inner cooling coil inlet adjusting valve (7) are controlled to be switched on or switched off by a cooperative control method, so that the material is fully activated, the temperature of the activated material can be continuously reduced under the action of stirring and a heat exchange medium, and when the temperature is lower than the preset T2, the next step is carried out, wherein T2 is less than T1;
s5, material reaction: in the material reaction process, the stirring frequency, the opening and closing or starting and stopping of the heat exchange medium pressurizing pump (4), the heat exchange medium switch valve (6) and the inner cooling coil inlet adjusting valve (7) are controlled by a cooperative control method to maximize the heat release rate of the material, the material is sampled and tested after the set reaction time is reached, if the material density reaches the standard, the reaction is ended, otherwise, the reaction is continued until the material density reaches the standard, and the reaction is ended.
4. The method for controlling the temperature of a rubber polymerizer of claim 3, wherein, in step S3, the step of determining whether or not the material is activated specifically comprises:
when the temperature change rate exceeds the preset B1, the stirring frequency is increased to F1, and the change condition of the temperature change rate is observed:
if the temperature change rate drops immediately after exceeding B1, the activation is judged to be false activation;
if the time during which the rate of temperature change exceeds B1 and the rate of temperature change exceeds B1 lasts at least 30 seconds, it is determined to be true activation.
5. The method for controlling the temperature of a rubber polymerizer vessel, according to claim 4, wherein after the material is activated and the temperature change rate is higher than the predetermined value B2, the heat transfer medium switching valve (6) is controlled to open, and if the temperature of the heat transfer medium switching valve (6) is not lowered after opening for at least 30 seconds, the next step is performed, wherein both of B2 and B1 are positive values and B2 > B1.
6. The method for controlling the temperature of a rubber polymerizer according to claim 3, wherein in step S4, the method for cooperative control of the material activation process specifically comprises:
if the temperature change rate is less than B3, the temperature acceleration is more than 0.0 and the heat exchange medium pressure pump (4) is not started, setting the stirring frequency to be 0 Hz;
if the temperature change rate is more than B3 and less than B4 and the temperature acceleration is more than 0.0, setting the stirring frequency as F1;
if the temperature change rate is more than B4 and less than B5 and the temperature acceleration is more than 0.0, the stirring PID loop is set to be automatic, and the heat exchange medium switch valve (6) is opened;
if the temperature change rate is more than 0.0 and less than B5 and the temperature acceleration is more than 0.0, the stirring PID loop is set to be automatic, and the inlet regulating valve (7) of the internal cooling coil is opened;
if the temperature change rate is greater than B5, the temperature acceleration is greater than 0.0, and the temperature is greater than T3, or the temperature is greater than the temperature of the last time of opening the heat exchange medium switch valve (6) +0.6 ℃ and the temperature is greater than T3, the stirring PID loop is set to be automatic, and the heat exchange medium booster pump (4) is started;
if the temperature change rate is more than B7 and less than B6 and the temperature acceleration is less than 0.0, the stirring PID loop is set to be automatic, and the heat exchange medium pressure pump (4) is closed;
if the temperature change rate is more than B8 and less than B7 and the temperature acceleration is less than 0.0, the stirring PID loop is set to be automatic, and the heat exchange medium switch valve (6) is closed;
if the temperature change rate is less than B8 and the temperature acceleration is less than 0.0, setting the stirring frequency to be 0 Hz;
if the temperature is less than the jump temperature of the activation process plus 0.8 ℃ and the temperature acceleration is less than J1, closing the heat exchange medium switch valve (6) and the heat exchange medium pressure pump (4);
when the temperature is lower than the preset T2, the T2 is less than T1, and the next step is carried out;
wherein T3 is less than T2; b3, B4 and B5 are positive numbers, and B3 is more than B4 and more than B5; b6, B7 and B8 are all negative numbers, and B6 is more than B7 is more than B8; j1 is negative.
7. The method for controlling the temperature of a rubber polymerizer as claimed in claim 6, wherein in step S5, the method for cooperative control in the reaction of the materials specifically comprises:
if the temperature change rate is less than B9, the temperature acceleration is more than 0.0, and the heat exchange medium pressurizing pump (4) is in a closed state, setting the stirring frequency to be 0 Hz;
if the temperature change rate of B9 is less than B10, the temperature acceleration is more than 0.0, and the heat exchange medium pressurizing pump (4) is in a closed state, setting the stirring frequency to be F1;
in 60 minutes, if the temperature change rate is more than B10 and less than B11, the temperature acceleration is more than 0.0, the temperature deviation is more than P1 and less than P2, and the temperature deviation is a numerical value obtained by subtracting a temperature set value from the actual temperature in the kettle body, the stirring PID loop is set to be automatic, and a heat exchange medium switch valve (6) is opened;
if the temperature change rate is more than B11 and less than B12, the temperature acceleration is more than 0.0, and the temperature deviation is more than P1 and less than P2, the stirring PID loop is set to be automatic, and an inlet regulating valve (7) of the internal cooling coil is opened;
if the temperature change rate is less than B12, the temperature acceleration is more than 0.0, and the temperature is more than T3, or the temperature is more than or equal to the temperature of the heat exchange medium switch valve (6) which is opened last time plus 0.6 ℃, the stirring PID loop is set to be automatic, and the inner cooling coil inlet adjusting valve (7) is opened;
if the temperature change rate is more than B13 and less than B14, the temperature acceleration is less than 0.0, the temperature deviation is more than P1 and less than P2, or the temperature deviation is less than P3, the heat exchange medium pressure pump (4) is closed;
if the temperature change rate is less than B14 and the temperature acceleration is less than 0.0, setting the stirring frequency to be F2, and closing the heat exchange medium switch valve (6);
when the timing of the material reaction process is more than 30 minutes, if the heat exchange medium switch valve (6) and the inner cooling coil inlet regulating valve (7) are in an open state, the temperature deviation is more than P4, and the stirring frequency is more than F3, the heat exchange medium pressure pump (4) is started, and the stirring frequency is reduced to F2;
wherein, B9, B10, B11 and B12 are positive numbers, and B9 is more than B10 and more than B11 and more than B12; b13 and B14 are both negative numbers, and B13 < B14; f2 < F1 < F3; p1, P2, P3 and P4 are all negative numbers, and P2 is more than P1 is more than P4 is more than P3.
8. The method for controlling temperature of a rubber polymerizer vessel of claim 7, wherein, after the sum of the timings of the material activation process of step S4 and the material reaction process of step S5 is > 240 minutes, during the period:
if the temperature deviation is larger than P1, opening the heat exchange medium switch valve (6) and the inner cooling coil inlet regulating valve (7), otherwise, closing the heat exchange medium switch valve (6) and the inner cooling coil inlet regulating valve (7);
and if the temperature deviation is P5 < P1, wherein P2 > P1 > P5 > P4 > P3, the heat exchange medium pressurizing pump (4) is started, and otherwise, the heat exchange medium pressurizing pump (4) is closed.
9. The method for controlling the temperature of a rubber polymerizer of claim 3 or 8, wherein step S6 is further included after step S5, and step S6 specifically includes:
after the reaction is completed, a terminator is added to terminate the reaction.
10. The method for controlling temperature of a rubber polymerizer, according to claim 9, further comprising step S7 after step S6, wherein step S7 specifically comprises:
after the reaction is terminated, an antioxidant is added to complete the reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210757450.XA CN115055134A (en) | 2022-06-29 | 2022-06-29 | Rubber polymerization kettle temperature control system and control method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210757450.XA CN115055134A (en) | 2022-06-29 | 2022-06-29 | Rubber polymerization kettle temperature control system and control method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115055134A true CN115055134A (en) | 2022-09-16 |
Family
ID=83204367
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210757450.XA Pending CN115055134A (en) | 2022-06-29 | 2022-06-29 | Rubber polymerization kettle temperature control system and control method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115055134A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117130406A (en) * | 2023-09-20 | 2023-11-28 | 青岛伊科思技术工程有限公司 | Method for controlling preset temperature of reactor of cracking carbon five fraction device |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4742472A (en) * | 1984-05-24 | 1988-05-03 | Mitsubishi Rayon Co., Ltd. | Method and apparatus for controlling polymerization reaction |
| CN101109966A (en) * | 2007-08-28 | 2008-01-23 | 中昊晨光化工研究院 | Polymer polymerization reaction temperature control method and device thereof |
| CN103030720A (en) * | 2011-09-30 | 2013-04-10 | 中国石油化工股份有限公司 | Apparatus and method for production of polypropylene by batch liquid-phase bulk technique |
| CN103130927A (en) * | 2011-11-29 | 2013-06-05 | 中国石油化工股份有限公司 | Method and system for olefin polymerization temperature control |
| CN107344981A (en) * | 2016-05-04 | 2017-11-14 | 中国石油化工股份有限公司 | A kind of method for producing butyl rubber |
| CN107930563A (en) * | 2017-12-25 | 2018-04-20 | 杭州普适自动化工程有限公司 | A kind of temperature of reaction kettle control system and method |
| CN109694422A (en) * | 2018-12-25 | 2019-04-30 | 重庆化医长寿化工集团有限公司 | Neoprene polymerize autocontrol method |
| CN111690085A (en) * | 2019-03-13 | 2020-09-22 | 山纳合成橡胶有限责任公司 | Automatic control method for chloroprene latex polymerization process |
| CN113934244A (en) * | 2021-09-27 | 2022-01-14 | 浙江大华技术股份有限公司 | Temperature control system and temperature control method |
| CN114570322A (en) * | 2022-02-17 | 2022-06-03 | 郭廷辉 | Polypropylene production system |
-
2022
- 2022-06-29 CN CN202210757450.XA patent/CN115055134A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4742472A (en) * | 1984-05-24 | 1988-05-03 | Mitsubishi Rayon Co., Ltd. | Method and apparatus for controlling polymerization reaction |
| CN101109966A (en) * | 2007-08-28 | 2008-01-23 | 中昊晨光化工研究院 | Polymer polymerization reaction temperature control method and device thereof |
| CN103030720A (en) * | 2011-09-30 | 2013-04-10 | 中国石油化工股份有限公司 | Apparatus and method for production of polypropylene by batch liquid-phase bulk technique |
| CN103130927A (en) * | 2011-11-29 | 2013-06-05 | 中国石油化工股份有限公司 | Method and system for olefin polymerization temperature control |
| CN107344981A (en) * | 2016-05-04 | 2017-11-14 | 中国石油化工股份有限公司 | A kind of method for producing butyl rubber |
| CN107930563A (en) * | 2017-12-25 | 2018-04-20 | 杭州普适自动化工程有限公司 | A kind of temperature of reaction kettle control system and method |
| CN109694422A (en) * | 2018-12-25 | 2019-04-30 | 重庆化医长寿化工集团有限公司 | Neoprene polymerize autocontrol method |
| CN111690085A (en) * | 2019-03-13 | 2020-09-22 | 山纳合成橡胶有限责任公司 | Automatic control method for chloroprene latex polymerization process |
| CN113934244A (en) * | 2021-09-27 | 2022-01-14 | 浙江大华技术股份有限公司 | Temperature control system and temperature control method |
| CN114570322A (en) * | 2022-02-17 | 2022-06-03 | 郭廷辉 | Polypropylene production system |
Non-Patent Citations (3)
| Title |
|---|
| 吴剑波;何水桥;: "氟橡胶聚合的数学模型控制", 自动化与仪器仪表, no. 01, 25 January 2013 (2013-01-25), pages 165 - 167 * |
| 杨广鑫: ""氯丁橡胶乳液聚合的优化控制"", 《中国氯碱》, no. 4, 30 April 2018 (2018-04-30), pages 16 - 19 * |
| 王立伟;: "135m~3聚合釜PVC生产的温度控制方案", 科技资讯, no. 28, 3 October 2008 (2008-10-03), pages 66 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117130406A (en) * | 2023-09-20 | 2023-11-28 | 青岛伊科思技术工程有限公司 | Method for controlling preset temperature of reactor of cracking carbon five fraction device |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN115055134A (en) | Rubber polymerization kettle temperature control system and control method thereof | |
| US4558108A (en) | Aqueous suspension polymerization process | |
| CN100524140C (en) | Polymer polymerization reaction temperature control method and device thereof | |
| CN112830995B (en) | Control method for polymerization reaction in carbon fiber production | |
| JPH0491071A (en) | Method and device for producing solution of nonferrous metal sulfonate | |
| CN111690085B (en) | Automatic control method for chloroprene latex polymerization process | |
| CN114632614B (en) | Automatic control system and method for warm grinding of coal mill | |
| CN101864017A (en) | Automatic control method of butadiene polymerization | |
| EP0115704B1 (en) | Aqueous suspension polymerization process | |
| KR102504881B1 (en) | Reactor temperature control method | |
| CN114534651B (en) | Reactor temperature control method | |
| JP3818375B2 (en) | Polymerization temperature control method | |
| JP2006002032A (en) | Polymer producing method and apparatus therefor | |
| CN104742265A (en) | Degassing temperature and stirring speed control system for epoxy resin secondary mixed material | |
| CN203830013U (en) | Automatic stirring autoclave allowing foaming reduction | |
| CN112817349A (en) | Black body temperature control method | |
| CN112979433A (en) | Control method in triethyl orthoformate synthesis process | |
| RU2084459C1 (en) | Method of controlling thermoelastic plastics polymerization batch process | |
| RU2763336C1 (en) | Method for automatic regulation of the polycondensation process in production of alkyd resins | |
| RU2188210C1 (en) | Method of operation of periodic process of polymerization of butadiene-styrene thermoelastplastics | |
| SU1101293A1 (en) | Method of controlling process of synthesis of boroesters in semicontinuous action reactor | |
| CN217189556U (en) | Polyvinyl chloride resin heat stability refining production process device | |
| CN116116336A (en) | Chemical process control method for synthesis reaction | |
| JP2009270018A (en) | Method for producing polymer particle and polymerization apparatus therefor | |
| CN217248926U (en) | Self-temperature-control reaction kettle for 4-BMA production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |