CN115101139A - Synthesis process of hydroxy pinacolone retinoic acid ester - Google Patents
Synthesis process of hydroxy pinacolone retinoic acid ester Download PDFInfo
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- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 23
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 17
- 229930002330 retinoic acid Natural products 0.000 title abstract description 11
- 229960001727 tretinoin Drugs 0.000 title abstract description 11
- -1 hydroxy pinacolone retinoic acid ester Chemical class 0.000 title abstract description 8
- 230000008569 process Effects 0.000 title abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 111
- 239000000446 fuel Substances 0.000 claims abstract description 107
- 239000002994 raw material Substances 0.000 claims abstract description 45
- 230000008859 change Effects 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims description 50
- 238000012937 correction Methods 0.000 claims description 40
- 238000012544 monitoring process Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000003245 working effect Effects 0.000 claims description 5
- 238000002485 combustion reaction Methods 0.000 claims description 4
- 238000004088 simulation Methods 0.000 claims description 4
- 239000000779 smoke Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 239000003517 fume Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 230000001276 controlling effect Effects 0.000 description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- SHGAZHPCJJPHSC-YCNIQYBTSA-N all-trans-retinoic acid Chemical compound OC(=O)\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C SHGAZHPCJJPHSC-YCNIQYBTSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 208000002874 Acne Vulgaris Diseases 0.000 description 2
- 206010000496 acne Diseases 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000003345 natural gas Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
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- 210000002615 epidermis Anatomy 0.000 description 1
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- 239000000049 pigment Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 102000003702 retinoic acid receptors Human genes 0.000 description 1
- 108090000064 retinoic acid receptors Proteins 0.000 description 1
- 150000004492 retinoid derivatives Chemical class 0.000 description 1
- 210000002374 sebum Anatomy 0.000 description 1
- 210000003491 skin Anatomy 0.000 description 1
- 230000009759 skin aging Effects 0.000 description 1
- 210000000434 stratum corneum Anatomy 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
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- C07C403/20—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by carboxyl groups or halides, anhydrides, or (thio)esters thereof
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Abstract
The invention relates to the technical field of organic synthesis, in particular to a synthesis process of hydroxy pinacolone retinoic acid ester. Through reasonable control by temperature change mode among the reaction vessel in this application, the data of temperature data and fuel among the reconnaissance reaction vessel to can effectually prevent among the reaction vessel influence of other factors to lead to the reaction vessel temperature to take place the sudden change and bring the raw materials reaction unusual among the reaction vessel, and resources are saved that can be certain.
Description
Technical Field
The invention relates to the technical field of organic synthesis, in particular to a synthesis process of hydroxy pinacolone retinoic acid ester.
Background
Hydroxy pinacolone retinoic acid ester, CAS number 893412-73-2, HPR for short, belongs to retinoid (Retinoids) family, can be directly combined with cell retinoic acid receptor, has the functions of regulating metabolism of epidermis and stratum corneum, can resist aging, can reduce sebum overflow, lighten epidermal pigment, and has the effects of preventing skin aging, treating acne, whitening skin and lightening spots and the like. The strong efficacy of retinoic acid is ensured, the irritation of retinoic acid is greatly reduced, and the retinoic acid is mainly used for resisting aging, removing wrinkles and preventing acne recurrence.
With the development of the field of cosmetics, the usage amount of the hydroxy pinacolone retinoic acid ester is continuously increased, but the source of the material is mainly imported abroad, the domestic yield is extremely low, the market demand is difficult to meet, for the synthesis of HPR, no effective and easily-industrialized operation method exists in the currently-published literature, in the prior art, under a proper temperature, the hydroxy pinacolone retinoic acid ester is synthesized by catalytic reaction of biological enzyme in a reaction container, the conversion rate is high, the inevitable relation is formed between the conversion rate and the temperature control in the reaction container, different amounts of raw materials need to be added into the reaction container, and therefore, the temperature control data and the addition amount data need to be coupled, so that the reaction container can accurately dominate the raw materials with different addition amounts, and the conversion rate of synthesis is improved. The control of heat in the reaction vessel is only to simply deduce the temperature of the vessel from the temperature of the raw materials in the vessel, and is not based on the data of burning the raw materials, which can affect the control of temperature in the reaction vessel, the conversion rate of product synthesis and the fuel saving problem.
Disclosure of Invention
In view of the above disadvantages, the present invention provides a process for synthesizing hydroxy pinacolone retinoic acid ester.
The invention provides the following technical scheme:
a method for controlling heat of a reaction vessel comprises the following steps:
setting overall planning data of fuels required by different contents of raw material synthesis reaction in a reaction container by taking data in the synthesis preparation process as a reference, and matching the raw material category and the overall planning data of the fuels with the optimal working effect of the reaction container in the synthesis preparation process;
secondly, setting up container temperature change data in the length direction of the reaction container based on the actual temperature in the monitoring container in each control section in the reaction container; in a field for preparing a product, solving a heat conduction simulation equation by using a finite element difference method according to the volume of a solution in a container;
thirdly, associating temperature monitoring data in the container, and solving a fuel flow standard value and a fuel flow solving value in each control interval in the reaction container under the current state;
comparing the standard value of the fuel flow and the solved value of the fuel flow with the flow monitoring value of the fuel in the control interval, judging the situation at the moment, and obtaining the temperature correction coefficient of the control interval through the comparison of the data of the situation, so that the difference correction of the fuel flow to the temperature of the reaction container under different situations can be realized;
and fifthly, substituting the temperature correction coefficient and other influence coefficients in the container into a solution equation to obtain a temperature correction value of the container in the control interval, and then bringing the temperature correction value back to the initial determination value of the container temperature.
The optimal technical scheme is that data in the synthesis preparation process are taken as a reference, overall data of fuels required by the raw material synthesis reaction with different contents in the reaction vessel are set, and the raw material category and the overall data of the fuels are matched with the optimal working effect of the reaction vessel in the synthesis preparation process; the specific conditions include the category a of the solution in the container, the control interval b of the reaction container, the amount of the synthesized product O (a), the index temperature T (a, b) at the tail section of the control interval, and the flow rate Q of the fuel required by the control interval 1 (a, b) control of the actual flow rate Q of the fuel in the interval 2 (a, b), and controlling the utilization rate u (a, b) of the interval fuel; the raw materials in the reaction container have the same formula and content, the categories of the solution in the container are a, and the formula and the content of the raw materials are matched with the corresponding category a of the raw materials when the reaction rate in the reaction container is stable;
under the condition of stable reaction rate, the index temperature of the liquid raw material in the container at the end of the section of the b-th control interval is obtained by detecting the solution in the container by using a sensor in the reaction container;
Q 1 (a, b) the flow rate of fuel required in the b' th control interval, i.e. the amount of fuel required for the temperature increase of the ingested heat, under conditions of stable reaction rate of the feedstock of category a;
wherein ,
b, under the condition of stable reaction rate, controlling the average specific heat between the temperature of a feeding nozzle and the index temperature of a discharging nozzle in an interval;
ΔT a,b under the condition of stable reaction rate, the temperature difference between the non-index temperature of the b th control section and the temperature of the feeding nozzle of the control section is controlled;
q is the heating value of the fuel.
3. The method of claim 2, wherein O (a) is a raw material of the category a, the amount produced in 60 minutes in each control interval is equal to the amount produced in 60 minutes in each control interval in the condition of a stable reaction rate,
wherein m (b) is the quality of the synthesized product in the b th control section, h (b) is the size of the b th control section, and s is the flow rate of the product;
u (a, b) is the usage of fuel in the b-th control interval under the condition of stable reaction rate of the raw material with the category a; u (a, b) ═ Q 1 (a,b)/Q 2 (a,b)，
in the formula ,Q2 (a, b) is the actual flow rate of the feed of category a in the b-th control interval under conditions of stable reaction rate.
As a preferred technical scheme of the heat control mode of the reaction vessel, the mass O (a, b) of the solution in the vessel in the period of 60 minutes of the solution category a in the b control interval,
wherein m (a, b) is the mass of the synthesized product of the solution with the category a in the b-th control interval in the state prepared at the moment; then, solving is carried out, and the flow of the fuel required by the b th control interval in the preparation state is at the momentNormalized value Q 3 (b)＝∑Q 3 (a, b) solving value of fuel flow rate required by the b th control interval under the situation prepared at the moment
wherein ,Q3 (a, b) in the case of the preparation at this time, a fuel flow specification value is required for the preparation of a solution of the order a in the b-th control interval for 60 minutes;
Q 2 (a, b) actual monitored fuel flow rate of solutions with the same content and the same category as the raw material formula of a in the b-th control interval at a stable reaction rate;
wherein: o (a, b) yield of the synthesized product of category a of the raw material solution at 60 minutes in the b-th control interval in the case where O (a, b) is prepared at this time;
ΔT’ a,b under the condition of preparation, the difference value between the index temperature of the solution in the container with the category a at the tail section of the b-th control interval and the temperature of the input nozzle of the control interval;
q is the heating value of the fuel.
As a preferred technical scheme of a control mode of the heat of the reaction vessel, the method realizes the specific steps of correcting the difference of the flow rate of the fuel to the temperature of the reaction vessel under different conditions: 1. establishing intervals of a flow correction coefficient alpha (b) and a flow change trend correction coefficient beta (b) in the b-th control interval, wherein alpha (b) is between 0.1 and 0.7, and beta (b) is between 0.2 and 0.5; predetermined fuel flow deviation value Δ Q (b) ═ Q 5 (b)-Q 3 (b) Solving for combustionDeviation value delta Q of material flow 1 (b)＝Q 5 (b)-Q 4 (b)，ΔQ 2 (b)＝Q 5 (b)-Q 5 Old age (b)，Q 5 (b) Under the condition of preparation, actually monitoring the fuel flow value in the b th control interval; q 5 Old age (b) In the preparation situation, the fuel flow value monitored last time in the b th control interval; 2. by Δ Q (b), Δ Q 1 (b) And Δ Q 2 (b) Selecting a proper flow correction coefficient alpha (b) and a flow change trend correction coefficient beta (b) according to experience; 3. the temperature correction coefficient Φ (b) in the b-th control interval in the preparation at this time was obtained as α (b) × β (b).
As a preferred technical scheme of a control mode of the heat of the reaction vessel, the final determined value T "(b) of the vessel temperature in the b th control interval is as follows:
T”(b)＝T(b)-ΔT”(b)
wherein, Delta T "(b) is the corrected value of the container temperature in the b-th control interval;
t (b) is the initial determined value of the container temperature in the b-th control interval;
theta is an air-fuel ratio;
gamma is the ratio of oil fume generated by fuel combustion;
C’ o under the preparation condition, a monitoring part in the b-th control interval monitors the specific heat of the oil smoke matched with the temperature;
q is the fuel calorific value.
The invention has the beneficial effects that: according to the method and the device, the temperature data in the reaction container and the data of the fuel are linked through a reasonable temperature control mode in the reaction container, so that the phenomenon that the raw material reaction in the reaction container is abnormal due to the fact that the temperature of the reaction container is suddenly changed due to the influence of other factors in the reaction container can be effectively prevented, and resources can be saved to a certain extent; the control mode of the application is particularly suitable for reaction vessels with high reaction speed and different raw materials.
Detailed Description
The conception, the specific structure and the technical effects of the present invention will be clearly and completely described in the following with reference to the embodiments, so that the objects, the schemes and the effects of the present invention can be fully understood.
A method for controlling heat of a reaction vessel comprises the following steps:
the method comprises the following steps of firstly, setting overall data of fuels required by different contents of raw material synthesis reaction in a reaction container by taking data in the synthesis preparation process as a reference, and matching raw material categories and the overall data of the fuels to the optimal working effect of the reaction container in the synthesis preparation process; the specific situation is as follows:
the raw materials in the reaction container have the same formula and content, the categories of the solution in the container are a, and the formula and the content of the raw materials are matched with the corresponding category a of the raw materials when the reaction rate in the reaction container is stable;
under the condition of stable reaction rate, the index temperature of the liquid raw material in the container at the end of the section of the b-th control interval is obtained by detecting the solution in the container by using a sensor in the reaction container;
Q 1 (a, b) the flow rate of fuel required in the b' th control interval, i.e. the amount of fuel required for the temperature increase of the ingested heat, under conditions of stable reaction rate of the feedstock of category a;
wherein ,
b, under the condition of stable reaction rate, controlling the average specific heat between the temperature of a feeding nozzle and the index temperature of a discharging nozzle in an interval;
ΔT a,b under the condition of stable reaction rate, the temperature difference between the non-index temperature of the b th control section and the temperature of the feeding nozzle of the control section is controlled; q is the calorific value of the fuel;
o (a) the production of starting materials of the class a in each control interval for 60 minutes at a steady reaction rate is equal in each control interval for 60 minutes at a steady reaction rate,
wherein m (b) is the quality of the synthesized product in the b-th control section, h (b) is the size of the b-th control section, and s is the flow rate of the product;
u (a, b) is the usage of fuel in the b-th control interval under the condition of stable reaction rate of the raw material with the category a;
u(a,b)＝Q 1 (a,b)/Q 2 (a, b) wherein Q 2 (a, b) actual flow rates of starting materials of class a in the b-th control interval under conditions of stable reaction rates.
Secondly, setting up container temperature change data in the length direction of the reaction container based on the actual temperature in the monitoring container in each control section in the reaction container; in the field of product preparation, a finite element difference method is utilized to solve a heat conduction simulation equation according to the volume of the solution in the container. Linking the distribution condition of each part in the reaction vessel, and establishing vessel temperature change data in the length direction of the reaction vessel by taking the real vessel temperature of each control interval in the reaction vessel as the root; according to the theory of a heat conduction simulation equation, a finite element difference method is used for solving, so that the temperature in the container is monitored in real time, and a starting determination value T (b) of the container temperature in a b-th control interval is obtained by solving the necessary temperature of the solution in the control interval through a terminal of large analytical force.
Thirdly, associating the temperature monitoring data in the container, and solving a fuel flow standard value and a fuel flow solving value in the current state in each control interval in the reaction container; solving the mass O (a, b) of the solution in the container in the b-th control interval in the 60-minute solution of the solution category a under the condition,
wherein m (a, b) is the mass of the synthesized product of the solution with the category a in the b-th control interval in the state prepared at the moment; then solving is carried out, and in the preparation state, the flow standard value Q of the fuel needed in the b th control interval 3 (b)＝∑Q 3 (a, b) solving value Q of fuel flow rate required in the b th control interval under the situation prepared at the moment 4 (b)＝∑ 4 Q (a, b); at the end, the utilization rate u (b) of the b-th control interval under the preparation situation at the moment is solved,
wherein ,Q3 (a, b) in the case of the preparation at this time, a fuel flow specification value is required for the preparation of a solution of the order a in the b-th control interval for 60 minutes;
Q 2 (a, b) the actually monitored fuel flow rate of the solution with the same content in the same raw material formula with the category a in the b control interval at the stable reaction rate;
wherein: o (a, b) yield of the synthesized product of the category a of the raw material solution at 60 minutes in the b-th control interval in the case where O (a, b) is prepared at this time;
ΔT’ a,b under the condition of preparation, the difference value between the index temperature of the solution in the container with the category a at the tail section of the b-th control interval and the temperature of the input nozzle of the control interval;
q is the calorific value of the fuel;
comparing the standard value of the fuel flow and the solved value of the fuel flow with the flow monitoring value of the fuel in the control interval, judging the situation at the moment, and obtaining the temperature correction coefficient of the control interval through the comparison of the data of the situation, so that the difference correction of the fuel flow to the temperature of the reaction container under different situations can be realized; 1. establishing intervals of a flow correction coefficient alpha (b) and a flow change trend correction coefficient beta (b) in the b-th control interval, wherein alpha (b) is between 0.1 and 0.7, and beta (b) is between 0.2 and 0.5; predetermined fuel flow deviation value Δ Q (b) ═ Q 5 (b)-Q 3 (b) Solving the fuel flow deviation value delta Q 1 (b)＝Q 5 (b)-Q 4 (b)，ΔQ 2 (b)＝Q 5 (b)-Q 5 Old age (b)，Q 5 (b) Under the condition of preparation, actually monitoring the fuel flow value in the b th control interval; q 5 Old age (b) Under the condition of preparation, the fuel flow value monitored last time in the b th control interval; 2. by Δ Q (b), Δ Q 1 (b) And Δ Q 2 (b) Selecting a proper flow correction coefficient alpha (b) and a flow change trend correction coefficient beta (b) according to experience; the temperature correction coefficient Φ (b) in the b-th control interval in the preparation case at this time was obtained as α (b) × β (b).
If Δ Q (b) and Δ Q 1 (b) When the temperature monitoring data and the fuel flow rate data are positive or negative, the actual conditions of the container reflected by the prepared solution product temperature monitoring data and the fuel flow rate data can be verified to be similar, and meanwhile, the flow correction coefficient alpha (b) can select the maximum terminal value in the range; conversely, the terminal minimum may be chosen.
Determine Δ Q (b) and Δ Q 2 (b) The relation between the flow change and the correction coefficient is selected in the established interval;
| Δ Q (b) is 0 or more | Δ Q (b) less than 0 | |
| ΔQ 2 (b) Is greater than or equal to 0 | E | F |
| ΔQ 2 (b) Less than 0 | G | H |
E, the value of the monitored fuel flow is higher, the monitored fuel flow changes in an increasing manner, and the value of the flow change trend correction coefficient is the rightmost value in the range;
f: at the moment, the value of the monitored fuel flow is small, the monitored fuel flow changes in an increasing manner, and the value of the flow change trend correction coefficient is the leftmost value in the range;
g: at the moment, the value of the monitored fuel flow is higher, the monitored fuel flow is in reduced change, and the value of the flow change trend correction coefficient is the leftmost value in the range;
h: at the moment, the value of the monitored fuel flow is small, the monitored fuel flow changes in a decreasing mode, and the value of the flow change trend correction coefficient is the rightmost value in the range;
and fifthly, substituting the temperature correction coefficient and other influence coefficients in the container into a solution equation to obtain a temperature correction value of the container in a control interval, and then bringing the temperature correction value back to a starting determined value T (b) of the container temperature, wherein the final determined value T "(b) of the container temperature in the b-th control interval comprises the following specific solution process:
T”(b)＝T(b)-ΔT”(b)
wherein, the delta T' (b) is a corrected value of the container temperature in the b-th control interval;
t (b) is the initial determined value of the container temperature in the b-th control interval;
theta is an air-fuel ratio;
gamma is the ratio of oil fume generated by fuel combustion;
C’ o under the preparation condition, the monitoring part in the b-th control interval monitors the specific heat of the oil smoke matched with the temperature;
q is the fuel calorific value;
taking a reaction vessel of the company to prepare a synthetic product as a specific example, the reaction vessel is formed in a cuboid shape, has a total length of about 4.6 meters, and can be divided into an ending zone, a preheating zone, a zone 1, a zone 2 and a soaking zone, wherein the preheating zone, the zone 1, the zone 2 and the soaking zone respectively correspond to the b, and the value of the b is 1/2/3/4; the fuel is natural gas with a heating value of 5646kcal/m 3 An air-fuel ratio of 10; the ratio of oil smoke generated by fuel combustion is 0.856; the feed categories fed to the reaction vessel were 1 and 2, and the product flow rate s was 16 m/h.
In the preparation situation, the flow rate of the fuel is monitored in each control interval as shown in table 1:
TABLE 1
| Control interval | 1 | 2 | 3 | 4 |
| Q 5 (m 3 /h) | 17 | 18 | 15.88 | 14.88 |
| Q Old age 5 (m 3 /h) | 14.26 | 13.50 | 14.20 | 17.80 |
In the case of the preparation, the temperatures of the inlet nozzles of the products of different categories in the respective control zones are obtained by monitoring the temperature of the solution in the reaction vessel as shown in table 2:
TABLE 2
The starting temperature determination value t (b) in the container in each control section is set as shown in table 3 below:
TABLE 3
| Each control section b | 1 | 2 | 3 | 4 |
| Determined vessel temperature T (b) | 50℃ | 55℃ | 62℃ | 65℃ |
Under the stable reaction speed in the container, the hour preparation yield corresponding to the raw material solution with the categories of 1 and 2 is 20Kg and 25Kg, the flow rate of the matched product is 15m/h and 18m/h, the temperature of the raw material solution entering the 1 st control interval is 35 ℃, and the established natural gas information data is shown in table 4;
TABLE 4
Where the solution of the feedstock of category a is at a steady reaction rate, the flow rate of the fuel required in the control interval b:
Q 1 (1,1)＝20×(50-35)×805/5646×4.18＝10.23
Q 1 (1,2)＝20×(55-50)×771/5646×4.18＝3.26
Q 1 (1,3)＝20×(60-55)×670/5646×4.18＝2.83
Q 1 (1,4)＝20×(65-60)×670/5646×4.18＝2.83
Q 1 (2,1)＝25×(50-35)×821/5646×4.18＝13.04
Q 1 (2,2)＝25×(55-50)×729/5646×4.18＝3.86
Q 1 (2,3)＝25×(60-55)×645/5646×4.18＝3.86
Q 1 (2,14)＝25×(65-60)×660/5646×4.18＝3.49
in the preparation state of the reaction vessel at the moment, solving the flow specification value Q of the fuel flow required by each control interval 3 (b) And the solved value Q of the fuel flow required by each control interval 4 (b)。
The preparation yield of each control interval in 1 hour is equal and is 20 Kg;
TABLE 5
In the preparation state of the reaction vessel at this time, the specification value of the fuel flow required by the hourly preparation amount matched in the b-th control interval for the raw material with the category a is solved as follows:
Q 3 (1,1)＝0/(20×15.25)＝0
Q 3 (1,2)＝10/(20×20.23)＝10.15
Q 3 (1,3)＝20/(20×14.89)＝14.89
Q 3 (1,4)＝20/(20×10.25)＝10.25
Q 3 (2,1)＝20/(25×15)＝12.00
Q 3 (2,2)＝14/(25×19.56)＝10.95
Q 3 (2,3)＝0/(25×11.25)＝0
Q 3 (2,4)＝0/(25×10)＝0
in the preparation case, the solution of the fuel utilization rate in the b-th control interval is as follows:
u(1)＝(0.6524×0+0.6945×12)/12＝0.6945
u(2)＝(0.6423×10.15+0.6420×10.95)/21.1＝0.6421
u(3)＝(0.6023×14.89+0.6123×0)/14.89＝0.6023
u(4)＝(0.4561×10.25+0.4523×0)/10.25＝0.4561
| each control interval b | u(b) |
| 1 | 0.6945 |
| 2 | 0.6421 |
| 3 | 0.6023 |
| 4 | 0.4561 |
The temperature difference delta T 'of the solution in the container a in the b-th control section can be obtained by using the difference between the temperature of the tail section of each control section and the temperature of the input nozzle of each control section' a,b ；
In the case of preparation, the solution raw material in the container of the category a is in the b-th control interval, and the fuel flow required for preparing the synthetic quantity in 60 minutes is matched to solve:
Q 4 (1,1)＝(805×0×12/(0.6524×5646×4.18)＝0
Q 4 (1,2)＝(771×10×15)/(0.6423×5646×4.18)＝7.629
Q 4 (1,3)＝(670×20×15)/(0.6023×5646×4.18)＝14.14
Q 4 (1,4)＝(670×10×12)/(0.4561×5646×4.18)＝7.46
Q 4 (2,1)＝(821×20×9)/(0.6945×5646×4.18)＝9.02
Q 4 (2,2)＝(729×10×15)/(0.6420×5646×4.18)＝7.21
Q 4 (2,3)＝(645×0×19)/(0.6123×5646×4.18)＝0
Q 4 (2,4)＝(660×0×15)/(0.4523×5646×4.18)＝0
under the preparation condition, the b th control interval needs the fuel flow to solve a numerical value;
and (4) determining the temperature correction coefficient phi (b) of the b-th control interval by combining the above principle through calculation given below.
ΔQ(1)＝Q 5 (1)-Q 3 (1)＝17-12＝5
ΔQ(2)＝Q 2 (2)-Q 3 (2)＝18-21.1＝-3.1
ΔQ(3)＝Q 5 (3)-Q 3 (3)＝15.88-14.89＝1
ΔQ(4)＝Q 5 (4)-Q 3 (4)＝14.88-10.25＝4.63
ΔQ 1 (1)＝Q 5 (1)-Q 4 (1)＝17-9.02＝7.88
ΔQ 1 (2)＝Q 5 (2)-Q 4 (2)＝18-14.84＝3.16
ΔQ 1 (3)＝Q 5 (3)-Q 4 (3)＝15.88-14.14＝1.74
ΔQ 1 (4)＝Q 5 (4)-Q 4 (4)＝14.88-7.46＝7.42
| b | 1 | 2 | 3 | 4 |
| ΔQ(b) | 5 | -3.1 | 1 | 4.63 |
| ΔQ1(b) | 7.88 | 3.16 | 1.74 | 7.42 |
| α(b) | 0.7 | 0.1 | 0.7 | 0.7 |
| b | 1 | 2 | 3 | 4 |
| ΔQ(b) | 5 | -3.1 | 1 | 4.63 |
| ΔQ2(b) | 2.74 | 4.50 | 1.68 | 3.08 |
| β(b) | 0.5 | 0.2 | 0.5 | 0.5 |
| b | 1 | 2 | 3 | 4 |
| Φ(b) | 0.35 | 0.02 | 0.35 | 0.35 |
The temperature correction value of the reaction vessel in the control interval is obtained by solving the temperature correction coefficient and other parameters in the reaction vessel
After solving for Δ T ″ (b) of the reaction vessel, solving for T ″ (b) ═ T — (b) - Δ T ″ (b) of the control interval to obtain a corrected determination temperature;
| control interval b | 1 | 2 | 3 | 4 |
| Start to determine the temperature | 50℃ | 55℃ | 62℃ | 65℃ |
| Final determination of temperature | 48℃ | 55℃ | 62℃ | 62℃ |
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method for controlling the heat of a reaction vessel is characterized by comprising the following steps:
setting overall planning data of fuels required by different contents of raw material synthesis reaction in a reaction container by taking data in the synthesis preparation process as a reference, and matching the raw material category and the overall planning data of the fuels with the optimal working effect of the reaction container in the synthesis preparation process;
secondly, setting up container temperature change data in the length direction of the reaction container based on the actual temperature in the monitoring container in each control section in the reaction container; in a field for preparing a product, solving a heat conduction simulation equation by using a finite element difference method according to the volume of a solution in a container;
thirdly, associating the temperature monitoring data in the container, and solving a fuel flow standard value and a fuel flow solving value in the current state in each control interval in the reaction container;
comparing the standard value of the fuel flow and the solved value of the fuel flow with the flow monitoring value of the fuel in the control interval, judging the situation at the moment, and obtaining the temperature correction coefficient of the control interval through the comparison of the data of the situation, so that the difference correction of the fuel flow to the temperature of the reaction container under different situations can be realized;
and fifthly, substituting the temperature correction coefficient and other influence coefficients in the container into a solution equation to obtain a temperature correction value of the container in the control interval, and then bringing the temperature correction value back to the initial determination value of the container temperature.
2. The method of claim 1, wherein the overall data of fuels required by the synthesis reaction of the raw materials with different contents in the reaction vessel is established based on the data in the synthesis preparation process, and the raw material category and the overall data of the fuels are matched with the optimal working effect of the reaction vessel in the synthesis preparation process; the specific conditions are that the category of solution in the container is a, the control zone of the reaction container is b, the amount of the synthetic product is O (a), the index temperature of the tail section of the control zone is T (a, b), and the flow rate of fuel required by the control zone is Q 1 (a, b) actual flow rate Q of fuel in control section 2 (a, b) controlling the utilization rate u (a, b) of interval fuel; the raw materials in the reaction container have the same formula and content, the categories of the solution in the container are a, and the formula and the content of the raw materials are matched with the corresponding category a of the raw materials when the reaction rate in the reaction container is stable;
the target temperature of the liquid raw material in the container at the end of the b-th control interval section under the condition of stable reaction rate of the raw material with the category of T (a, b) a is obtained by detecting the solution in the container by using a sensor in the reaction container;
Q 1 (a, b) the flow rate of fuel required in the b' th control interval, i.e. the amount of fuel required for the temperature increase of the ingested heat, under conditions of stable reaction rate of the feedstock of category a;
wherein ,
b, under the condition of stable reaction rate, controlling the average specific heat between the temperature of a feeding nozzle and the index temperature of a discharging nozzle in an interval;
ΔT a,b under the condition of stable reaction rate, the temperature difference between the non-index temperature of the b th control section and the temperature of the feeding nozzle of the control section is controlled;
q is the heating value of the fuel.
3. The method of claim 2, wherein O (a) is a raw material of the category a, the amount produced in 60 minutes in each control interval is equal to the amount produced in 60 minutes in each control interval in the condition of a stable reaction rate,
wherein m (b) is the quality of the synthesized product in the b th control section, h (b) is the size of the b th control section, and s is the flow rate of the product;
u (a, b) is the usage of fuel in the b-th control interval under the condition of stable reaction rate of the raw material with the category a; u (a, b) ═ Q 1 (a,b)/Q 2 (a,b)，
in the formula ,Q2 (a, b) is the actual flow rate of the feed of category a in the b-th control interval under conditions of stable reaction rate.
4. According to the claimThe method for controlling the heat of a reaction vessel according to claim 1, wherein the mass O (a, b) of the solution in the vessel in the period of 60 minutes in the b-th control interval of the solution category a,
wherein m (a, b) is the mass of the synthesized product of the solution with the category a in the b-th control interval in the state prepared at the moment; then, solving is carried out, and in the preparation state, the flow specification value Q of the fuel needed in the b-th control interval 3 (b)＝∑Q 3 (a, b) solving value Q of fuel flow rate required in the b th control interval under the situation prepared at the moment 4 (b)＝∑ 4 Q (a, b); and finally, solving the utilization rate of the b-th control interval in the preparation situation at the moment
wherein ,Q3 (a, b) in the case of the preparation at this time, the preparation of a solution of the order a in the b-th control interval for 60 minutes requires a fuel flow specification value;
Q 2 (a, b) the actually monitored fuel flow rate of the solution with the same content in the same raw material formula with the category a in the b control interval at the stable reaction rate;
wherein: o (a, b) yield of the synthesized product of the category a of the raw material solution at 60 minutes in the b-th control interval in the case where O (a, b) is prepared at this time;
ΔT’ a,b in the case of preparation, the difference between the index temperature of the solution in the container with the category a at the tail section of the b-th control interval and the temperature of the input nozzle in the control interval;
q is the heating value of the fuel.
5. A method for controlling the heat of a reaction vessel according to claim 1, characterized by the specific steps of carrying out the correction of the difference in the flow rate of the fuel versus the temperature of the reaction vessel for different situations: 1. establishing intervals of a flow correction coefficient alpha (b) and a flow change trend correction coefficient beta (b) in the b-th control interval, wherein alpha (b) is between 0.1 and 0.7, and beta (b) is between 0.2 and 0.5; predetermined fuel flow deviation value Δ Q (b) ═ Q 5 (b)-Q 3 (b) Solving the fuel flow deviation value delta Q 1 (b)＝Q 5 (b)-Q 4 (b)，ΔQ 2 (b)＝Q 5 (b)-Q 5 Old age (b)，Q 5 (b) Under the condition of preparation, actually monitoring the fuel flow value in the b th control interval; q 5 Old age (b) In the preparation situation, the fuel flow value monitored last time in the b th control interval; 2. by Δ Q (b), Δ Q 1 (b) And Δ Q 2 (b) Selecting a proper flow correction coefficient alpha (b) and a flow change trend correction coefficient beta (b) according to experience; 3. the temperature correction coefficient Φ (b) in the b-th control interval in the preparation at this time was obtained as α (b) × β (b).
6. The method for controlling the heat in the reaction vessel according to claim 1, wherein the final determined value T "(b) of the vessel temperature in the b-th control interval is solved as follows:
T”(b)＝T(b)-ΔT”(b)
wherein, the delta T' (b) is a corrected value of the container temperature in the b-th control interval;
t (b) is the initial determined value of the container temperature in the b-th control interval;
theta is the air-fuel ratio;
gamma is the ratio of oil fume generated by fuel combustion;
C’ o under the preparation condition, the monitoring part in the b-th control interval monitors the specific heat of the oil smoke matched with the temperature;
and q is the fuel calorific value.
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