CN115101139B - 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 30
- 238000000034 method Methods 0.000 title claims abstract description 23
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 22
- 230000008569 process Effects 0.000 title claims abstract description 11
- 229930002330 retinoic acid Natural products 0.000 title abstract description 10
- 229960001727 tretinoin Drugs 0.000 title abstract description 10
- -1 hydroxy pinacolone retinoic acid ester Chemical class 0.000 title abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 121
- 239000000446 fuel Substances 0.000 claims abstract description 112
- 238000002360 preparation method Methods 0.000 claims abstract description 61
- 239000002994 raw material Substances 0.000 claims abstract description 58
- 230000003245 working effect Effects 0.000 claims abstract description 6
- 238000012937 correction Methods 0.000 claims description 44
- 239000000243 solution Substances 0.000 claims description 44
- 238000012544 monitoring process Methods 0.000 claims description 19
- 230000008859 change Effects 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000779 smoke Substances 0.000 claims description 7
- 238000004088 simulation Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 238000009472 formulation Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000011550 stock solution Substances 0.000 claims description 3
- 230000005856 abnormality Effects 0.000 abstract description 2
- 230000035772 mutation Effects 0.000 abstract description 2
- 230000001276 controlling effect Effects 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 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
- 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 2
- 210000002615 epidermis Anatomy 0.000 description 2
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- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 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
- 230000002194 synthesizing effect Effects 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 206010039792 Seborrhoea Diseases 0.000 description 1
- 238000004458 analytical method Methods 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
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
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- 230000006872 improvement Effects 0.000 description 1
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- 230000004060 metabolic process Effects 0.000 description 1
- 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
- 208000008742 seborrheic dermatitis Diseases 0.000 description 1
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- 210000000434 stratum corneum Anatomy 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
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- G—PHYSICS
- G16—INFORMATION AND COMMUNICATION TECHNOLOGY [ICT] SPECIALLY ADAPTED FOR SPECIFIC APPLICATION FIELDS
- G16C—COMPUTATIONAL CHEMISTRY; CHEMOINFORMATICS; COMPUTATIONAL MATERIALS SCIENCE
- G16C20/00—Chemoinformatics, i.e. ICT specially adapted for the handling of physicochemical or structural data of chemical particles, elements, compounds or mixtures
- G16C20/10—Analysis or design of chemical reactions, syntheses or processes
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C403/00—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
- 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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- G—PHYSICS
- G16—INFORMATION AND COMMUNICATION TECHNOLOGY [ICT] SPECIALLY ADAPTED FOR SPECIFIC APPLICATION FIELDS
- G16C—COMPUTATIONAL CHEMISTRY; CHEMOINFORMATICS; COMPUTATIONAL MATERIALS SCIENCE
- G16C10/00—Computational theoretical chemistry, i.e. ICT specially adapted for theoretical aspects of quantum chemistry, molecular mechanics, molecular dynamics or the like
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- G—PHYSICS
- G16—INFORMATION AND COMMUNICATION TECHNOLOGY [ICT] SPECIALLY ADAPTED FOR SPECIFIC APPLICATION FIELDS
- G16C—COMPUTATIONAL CHEMISTRY; CHEMOINFORMATICS; COMPUTATIONAL MATERIALS SCIENCE
- G16C60/00—Computational materials science, i.e. ICT specially adapted for investigating the physical or chemical properties of materials or phenomena associated with their design, synthesis, processing, characterisation or utilisation
Abstract
The application relates to the technical field of organic synthesis, in particular to a synthesis process of hydroxy pinacolone retinoic acid ester, which takes data in the synthesis preparation process as a reference, sets up overall data of fuels required by synthesis reaction of raw materials with different contents in a reaction vessel, and matches the overall data of the raw materials with the overall data of the fuels to realize the optimal working effect of the reaction vessel in the synthesis preparation process. According to the application, through a reasonable temperature control mode in the reaction vessel and then linking the temperature data in the reaction vessel with the data of the fuel, the reaction abnormality of the raw materials in the reaction vessel caused by the mutation of the temperature of the reaction vessel due to the influence of other factors in the reaction vessel can be effectively prevented, and resources can be saved to a certain extent.
Description
Technical Field
The application relates to the technical field of organic synthesis, in particular to a synthesis process of hydroxy pinacolone retinoic acid ester.
Background
The hydroxy pinacolone retinoic acid ester with 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, resisting aging, reducing seborrhea, fading epidermis pigment, preventing skin aging, treating acne, whitening and fading spots, and the like. The powerful effect of retinoic acid is ensured, and the irritation is greatly reduced, so that the retinoic acid is mainly used for resisting aging, removing wrinkles and preventing acne recurrence.
Along with the development of the cosmetic field, the usage amount of hydroxy pinacolone retinoic acid ester is continuously improved, but the source of the material is mainly imported abroad, the domestic yield is extremely low, the market demand is difficult to meet, no method which is very effective and easy for industrial operation exists in the currently disclosed literature for synthesizing HPR, in the prior art, hydroxy pinacolone retinoic acid ester is synthesized by utilizing the catalytic reaction of biological enzyme in a reaction container at a proper temperature, the conversion rate is higher, the conversion rate is inevitably related to the temperature control in the reaction container, different amounts of raw materials need to be added in 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 control the raw materials with different addition amounts, and the conversion rate of synthesis is improved. The control of the heat in the reaction vessel is simply based on the temperature of the raw materials in the vessel to deduce the temperature of the vessel, and the control of the temperature in the reaction vessel, the conversion rate of product synthesis and the fuel saving problem are affected by the data of burning the raw materials.
Disclosure of Invention
In view of the above-mentioned shortcomings, the present application aims to provide a process for synthesizing hydroxy pinacolone retinoic acid ester.
The application provides the following technical scheme:
a control mode of heat of a reaction vessel comprises the following steps:
firstly, setting overall data of fuels required by the synthesis reaction of raw materials with different contents in a reaction container by taking data in the synthesis preparation process as a reference, and matching the raw material category and the overall data of the fuels to obtain 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 actual monitoring of the temperature in the container of each control interval in the reaction container; at the site for preparing the product, according to the volume of the solution in the container, a finite element difference method is utilized to solve a heat conduction simulation equation;
thirdly, the temperature monitoring data in the container are connected, and the fuel flow standard value and the fuel flow solving value in the state of each control interval in the reaction container are solved;
fourth, comparing the standard value of the fuel flow and the solving 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 by the comparison between the data of the standard value and the solving value of the fuel flow, thereby realizing the differential correction of the fuel flow to the temperature of the reaction container under different conditions;
and fifthly, carrying the temperature correction value of the container in the control interval through the temperature correction coefficient and other influence coefficients in the container into a solution equation, and then carrying the temperature correction value back to the initial determination value of the container temperature.
As a preferred technical scheme of a control mode of the heat of the reaction vessel, setting up overall data of fuels required by the synthesis reaction of raw materials with different contents in the reaction vessel based on data in the synthesis preparation process, and matching the raw material category and the overall data of the fuels with the optimal working effect of the reaction vessel in the synthesis preparation process; the specific conditions are that the solution in the container is a, the control interval b of the reaction container, the synthesized product quantity O (a), the index temperature T (a, b) of the tail section of the control interval, and the flow rate Q of the fuel required by the control interval 1 (a, b) controlling the actual flow rate Q of the fuel in the interval 2 (a, b) controlling the use ratio u (a, b) of the interval fuel; the raw materials in the reaction container are the same in formula and content, the solution in the container is a, and when the reaction rate in the reaction container is stable, the formula and content of the raw materials are matched with the corresponding raw material a;
under the condition of stable reaction rate, the raw material with the category T (a, b) being a raw material, wherein the index temperature of the liquid raw material in the container at the end of the b-th control interval section 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 zone, i.e., the amount of fuel required to increase the amount of heat ingested by the temperature, under conditions of stable reaction rate for a feedstock of category a;
wherein ,b controlling the average specific heat between the temperature of the feeding nozzle and the index temperature of the discharging nozzle in the interval under the condition of stable reaction rate of the raw materials with the category a;
ΔT a,b b controlling the temperature difference between the non-index temperature of the interval section and the temperature of the feeding nozzle of the control section under the condition of stable reaction rate for the raw material with category a;
q is the heating value of the fuel.
3. The method for controlling heat of a reaction vessel according to claim 2, wherein O (a) is a preparation amount of a raw material of category a in each of the control intervals for 60 minutes under the condition of a stable reaction rate, a preparation amount of a raw material in each of the control intervals for 60 minutes under the condition of a stable reaction rate is equal,wherein m (b) is the mass 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 product flow rate;
u (a, b) is the fuel usage rate of the feedstock of category a in the b-th control zone under conditions of stable reaction rate; u (a, b) =q 1 (a,b)/Q 2 (a,b)，
in the formula ,Q2 (a, b) is the actual flow rate of the feedstock of category a at the b-th control zone under conditions of stable reaction rate.
As a preferred technical scheme of a control mode of the heat of the reaction vessel, the mass O (a, b) of the solution in the vessel in 60 minutes in the b-th control interval of the solution category a,wherein m (a, b) is the quality of the synthesized product in the b-th mastering interval of the solution with category a in the state of being prepared in the process; solving, in the preparation state, the flow standard value Q of the fuel required by the b control interval 3 (b)＝∑Q 3 (a, b) and the situation of preparation at the moment, the b-th control interval requires a fuel flow solving value
wherein ,Q3 (a, b) in the case of the preparation at this time, the preparation amount of the solution of category a in the b-th control interval for 60 minutes requires a fuel flow specification value;
Q 2 (a, b) the same raw material formulation as category a, and the same content of the solution is used for actually monitoring the fuel flow in the b control interval under the stable reaction rate;
wherein: o (a, b) in the case of this preparation, the yield of the synthesis product of 60 minutes in the b-th control zone of the stock solution category a;
the average specific heat between the temperature of the input nozzle and the index temperature of the output nozzle in the b control interval under the condition of stable reaction rate for the solution in the container with the category a;
ΔT’ a,b in the case of the preparation at this time, the difference between the index temperature of the solution in the container of category a at the tail section of the control section b and the temperature of the input nozzle of the control section b;
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 specific steps of realizing the differential correction of the flow rate of the fuel to the temperature of the reaction vessel under different conditions are as follows: 1. establishing a flow correction coefficient alpha (b) and a flow change trend correction coefficient beta (b) of a b-th control interval, wherein alpha (b) is between 0.1 and 0.7, and beta (b) is between 0.2 and 0.5; prescribed fuel flow deviation Δq (b) =q 5 (b)-Q 3 (b) Solving for fuel flow deviation value DeltaQ 1 (b)＝Q 5 (b)-Q 4 (b)，ΔQ 2 (b)＝Q 5 (b)-Q 5 Old one (b)，Q 5 (b) In the case of the preparation for this purpose,b, actual monitoring fuel flow value in the control interval; q (Q) 5 Old one (b) In the preparation case, the b-th control section monitors the fuel flow value monitored last time; 2. by DeltaQ (b), deltaQ 1 (b) Δq 2 (b) According to experience, selecting proper flow correction coefficient alpha (b) and flow change trend correction coefficient beta (b); 3. the temperature correction coefficient Φ (b) =α (b) ×β (b) of the b-th control section in the production case at this time is obtained.
As a preferred technical solution of a control mode of the heat of the reaction vessel, the b-th control interval vessel temperature final determination value T "(b), the specific solving process is as follows:
T”(b)＝T(b)-ΔT”(b)
wherein ΔT "(b) is the correction 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;
θ is the air-fuel ratio;
in the case of this time preparation, the b-th control section removes the loss of other heat than the heat absorbed by the prepared product;
gamma is the ratio of oil smoke generated by burning fuel;
C’ o in the preparation case, the monitoring part in the b-th control interval monitors the specific heat of the oil smoke with the matched temperature;
q is the fuel heating value.
The beneficial effects of the application are as follows: according to the application, through a reasonable temperature control mode in the reaction vessel, the temperature data in the reaction vessel and the data of the fuel are linked, so that the reaction abnormality of raw materials in the reaction vessel caused by mutation of the temperature of the reaction vessel due to the influence of other factors in the reaction vessel can be effectively prevented, and resources can be saved to a certain extent; the control mode of the application is particularly suitable for the reaction vessels with high reaction speed and different raw materials.
Detailed Description
The conception, specific structure, and technical effects produced by the present application will be clearly and completely described in connection with the embodiments below to fully understand the objects, aspects, and effects of the present application.
A control mode of heat of a reaction vessel comprises the following steps:
firstly, setting overall data of fuels required by the synthesis reaction of raw materials with different contents in a reaction container by taking data in the synthesis preparation process as a reference, and matching the raw material category and the overall data of the fuels to obtain the optimal working effect of the reaction container in the synthesis preparation process; the specific conditions are as follows:
the raw materials in the reaction container are the same in formula and content, the solution in the container is a, and when the reaction rate in the reaction container is stable, the formula and content of the raw materials are matched with the corresponding raw material a;
under the condition of stable reaction rate, the raw material with the category T (a, b) being a raw material, wherein the index temperature of the liquid raw material in the container at the end of the b-th control interval section 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 zone, i.e., the amount of fuel required to increase the amount of heat ingested by the temperature, under conditions of stable reaction rate for a feedstock of category a;
wherein ,b controls the reaction rate of the raw material of category a under the condition of stable reaction rateAverage specific heat between the temperature of the feeding nozzle and the index temperature of the discharging nozzle in the interval;
ΔT a,b b controlling the temperature difference between the non-index temperature of the interval section and the temperature of the feeding nozzle of the control section under the condition of stable reaction rate for the raw material with category a; q is the heating value of the fuel;
o (a) is the preparation amount of the raw material with the category a in 60 minutes in each control interval under the condition of stable reaction rate, the preparation amount of the raw material in 60 minutes in each control interval is equal under the condition of stable reaction rate,wherein m (b) is the mass 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 product flow rate;
u (a, b) is the fuel usage rate of the feedstock of category a in the b-th control zone under conditions of stable reaction rate;
u(a,b)＝Q 1 (a,b)/Q 2 (a, b) wherein Q 2 (a, b) is the actual flow rate of the feedstock of category a at the b-th control zone under conditions of stable reaction rate.
Secondly, setting up container temperature change data in the length direction of the reaction container based on actual monitoring of the temperature in the container of each control interval in the reaction container; at the site where the product is prepared, the heat conduction simulation equation is solved by utilizing a finite element differential method according to the volume of the solution in the container. The distribution condition of each component in the reaction vessel is connected, and the real vessel temperature of each control interval in the reaction vessel is taken as the root, so that vessel temperature change data in the length direction of the reaction vessel is set up; according to the theory of the heat conduction simulation equation, the temperature in the container is monitored in real time by utilizing a finite element difference method, and the starting determination value T (b) of the container temperature in the b-th control interval is obtained by solving the necessary temperature of the solution in the control interval through the terminal of the large-scale analysis force.
Thirdly, the temperature monitoring data in the container are connected, and the fuel flow standard value in the state of each control interval in the reaction container at the moment is solvedSolving a fuel flow rate; solving the mass O (a, b) of the solution in the container for 60 minutes in the b-th control interval,wherein m (a, b) is the quality of the synthesized product in the b-th mastering interval of the solution with category a in the state of being prepared in the process; solving, in the preparation state, the flow standard value Q of the fuel required by the b control interval 3 (b)＝∑Q 3 (a, b) and the situation of preparation at the moment, the b-th control interval requires a fuel flow solving value Q 4 (b)＝∑ 4 Q (a, b); finally, the utilization ratio u (b) and +.of the b-th control zone in the preparation situation at this time are solved>
wherein ,Q3 (a, b) in the case of the preparation at this time, the preparation amount of the solution of category a in the b-th control interval for 60 minutes requires a fuel flow specification value;
Q 2 (a, b) the same raw material formulation as category a, and the same content of the solution is used for actually monitoring the fuel flow in the b control interval under the stable reaction rate;
wherein: o (a, b) in the case of this preparation, the yield of the synthesis product of 60 minutes in the b-th control zone of the stock solution category a;
the temperature of the inlet nozzle and the outlet nozzle in the b-th control zone under the condition of stable reaction rate for the solution in the container of category aMean specific heat between index temperatures;
ΔT’ a,b in the case of the preparation at this time, the difference between the index temperature of the solution in the container of category a at the tail section of the control section b and the temperature of the input nozzle of the control section b;
q is the heating value of the fuel;
fourth, comparing the standard value of the fuel flow and the solving 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 by the comparison between the data of the standard value and the solving value of the fuel flow, thereby realizing the differential correction of the fuel flow to the temperature of the reaction container under different conditions; 1. establishing a flow correction coefficient alpha (b) and a flow change trend correction coefficient beta (b) of a b-th control interval, wherein alpha (b) is between 0.1 and 0.7, and beta (b) is between 0.2 and 0.5; prescribed fuel flow deviation Δq (b) =q 5 (b)-Q 3 (b) Solving for fuel flow deviation value DeltaQ 1 (b)＝Q 5 (b)-Q 4 (b)，ΔQ 2 (b)＝Q 5 (b)-Q 5 Old one (b)，Q 5 (b) In the preparation case of the time, the b-th control interval actually monitors the fuel flow value; q (Q) 5 Old one (b) In the preparation case, the b-th control section monitors the fuel flow value monitored last time; 2. by DeltaQ (b), deltaQ 1 (b) Δq 2 (b) According to experience, selecting proper flow correction coefficient alpha (b) and flow change trend correction coefficient beta (b); 3. the temperature correction coefficient Φ (b) =α (b) ×β (b) of the b-th control section in the production case at this time is obtained.
If DeltaQ (b) and DeltaQ 1 (b) When the flow correction coefficient alpha (b) is positive or negative, the actual conditions of the container reflected by the prepared solution product temperature monitoring data and the fuel flow data can be confirmed to be similar, and meanwhile, the flow correction coefficient alpha (b) can be used for selecting the maximum terminal value in the range; in the opposite case, the terminal minimum may be chosen.
Determining Δq (b) and Δq 2 (b) The relation between the flow change trend correction coefficient values is selected in the established interval;
| ΔQ (b) is 0 or more | ΔQ (b) is less than 0 | |
| ΔQ 2 (b) Greater than or equal to 0 | E | F |
| ΔQ 2 (b) Less than 0 | G | H |
E, monitoring that the fuel flow value is higher at the moment, wherein the monitored fuel flow is changed in an increased way, and the flow change trend is towards the rightmost value in the correction coefficient value range;
f: at the moment, the monitored fuel flow is smaller in value, the monitored fuel flow is changed in an increasing way, and the flow change trend is towards the leftmost value in the correction coefficient value range;
g: at the moment, the monitored fuel flow is higher in value, the monitored fuel flow is changed in a reduced mode, and the value of the flow change trend correction coefficient is the leftmost value in the range;
h: at the moment, the monitored fuel flow is smaller in value, the monitored fuel flow is changed in a reduced mode, and the value of the flow change trend correction coefficient is the rightmost value in the range;
fifthly, carrying the temperature correction value of the container in the control interval into a solving equation through the temperature correction coefficient and other influence coefficients in the container, and then carrying the temperature correction value back to the initial determination value T (b) of the container temperature, wherein the final determination value T "(b) of the container temperature in the control interval is carried out, and the specific solving process is as follows:
T”(b)＝T(b)-ΔT”(b)
wherein ΔT "(b) is the correction 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;
θ is the air-fuel ratio;
in the case of this time preparation, the b-th control section removes the loss of other heat than the heat absorbed by the prepared product;
gamma is the ratio of oil smoke generated by burning fuel;
C’ o in the preparation case, the monitoring part in the b-th control interval monitors the specific heat of the oil smoke with the matched temperature;
q is the fuel calorific value;
the synthetic product is prepared by using a reaction vessel of the company as a specific embodiment, wherein the reaction vessel is formed in a cuboid shape, the total length is about 4.6 meters, the reaction vessel 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 b, and the b value is 1/2/3/4; natural gas with heat value of 5646kcal/m is used as fuel 3 The air-fuel ratio thereof is 10; the ratio of the oil smoke generated by burning the fuel is 0.856; the raw materials fed into the reaction vessel were 1 and 2 in terms of type and the product flow rate s was 16m/h.
In the case of this preparation, the flow rate values of the monitored fuels in each control zone are shown in table 1:
TABLE 1
| Control section | 1 | 2 | 3 | 4 |
| Q 5 (m 3 /h) | 17 | 18 | 15.88 | 14.88 |
| Q Old one 5 (m 3 /h) | 14.26 | 13.50 | 14.20 | 17.80 |
Under the preparation condition, according to the temperature monitoring of the solution in the reaction vessel, the temperatures of the input nozzles of different types of target products in each control interval are shown in table 2:
TABLE 2
A temperature start determination value T (b) in each control section container is set as shown in table 3 below:
TABLE 3 Table 3
| Each control section b | 1 | 2 | 3 | 4 |
| Determined container temperature T (b) | 50℃ | 55℃ | 62℃ | 65℃ |
Under the stable reaction speed in the container, the corresponding hour preparation yield of the raw material solution with the categories of 1 and 2 is 20Kg and 25Kg, the matched product flow rates are 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 are shown in table 4;
TABLE 4 Table 4
Wherein category a solutions of raw materials under stable reaction rates, b governs the flow rate of fuel required in the interval:
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
under the preparation state of the reaction vessel at the moment, solving the flow standard value Q of the fuel flow required by each control interval 3 (b) And the solution 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 20Kg;
TABLE 5
In the preparation state of the reaction vessel at this time, the standard value of the fuel flow required by the preparation amount of the raw material with category a in the b-th control interval matching hour 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 case of preparation at this time, the solution of the fuel usage rate in the b-th control section 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 section b | u(b) |
| 1 | 0.6945 |
| 2 | 0.6421 |
| 3 | 0.6023 |
| 4 | 0.4561 |
The temperature difference between the tail section of each control section and the temperature of the input nozzle of each control section can be used to obtain the temperature difference delta T 'of the solution in the container a in the control section b' a,b ；
In the case of this preparation, the solution raw materials in the container of category a are in the control section b, and the fuel flow required for the preparation of the synthesis amount for 60 minutes is solved:
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 at this time, the b-th control interval needs fuel flow solving values;
the condition judgment determines the temperature correction coefficient phi (b) of the b-th control section through the calculation given below in combination with the above principle.
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 |
Obtaining the temperature correction value of the reaction vessel in the control zone through solving the temperature correction coefficient and other parameters in the reaction vessel
After solving the deltat "(b) of the reaction vessel, solving the deltat" (b) =t (b) -deltat "(b) of the control interval to obtain the corrected determined temperature;
| control section b | 1 | 2 | 3 | 4 |
| Start to determine temperature | 50℃ | 55℃ | 62℃ | 65℃ |
| Final determination of temperature | 48℃ | 55℃ | 62℃ | 62℃ |
The foregoing description is only a preferred embodiment of the present application, and the present application is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present application has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (6)
1. A method for controlling heat of a reaction vessel, comprising the steps of:
firstly, setting overall data of fuels required by the synthesis reaction of raw materials with different contents in a reaction container by taking data in the synthesis preparation process as a reference, and matching the raw material category and the overall data of the fuels to obtain 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 actual monitoring of the temperature in the container of each control interval in the reaction container; at the site for preparing the product, according to the volume of the solution in the container, a finite element difference method is utilized to solve a heat conduction simulation equation;
thirdly, the temperature monitoring data in the container are connected, and the fuel flow standard value and the fuel flow solving value in the state of each control interval in the reaction container are solved;
fourth, comparing the standard value of the fuel flow and the solving 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 by the comparison between the data of the standard value and the solving value of the fuel flow, thereby realizing the differential correction of the fuel flow to the temperature of the reaction container under different conditions;
and fifthly, carrying the temperature correction value of the container in the control interval through the temperature correction coefficient and other influence coefficients in the container into a solution equation, and then carrying the temperature correction value back to the initial determination value of the container temperature.
2. The method for controlling heat of a reaction vessel according to claim 1, wherein the overall data of fuels required by the synthesis reaction of different contents of raw materials in the reaction vessel are established based on the data in the synthesis preparation process, and the raw material category and the overall data of fuels are matched to obtain the optimal working effect of the reaction vessel in the synthesis preparation process; the specific conditions are that the solution in the container is a, the control interval b of the reaction container, the synthesized product quantity O (a), the index temperature T (a, b) of the tail section of the control interval, and the flow rate Q of the fuel required by the control interval 1 (a, b) controlling the actual flow rate Q of the fuel in the interval 2 (a, b) controlling the use ratio u (a, b) of the interval fuel; the raw materials in the reaction container are the same in formula and content, the solution in the container is a, and when the reaction rate in the reaction container is stable, the formula and content of the raw materials are matched with the corresponding raw material a;
under the condition of stable reaction rate, the raw material with the category T (a, b) being a raw material, wherein the index temperature of the liquid raw material in the container at the end of the b-th control interval section 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 zone, i.e., the amount of fuel required to increase the amount of heat ingested by the temperature, under conditions of stable reaction rate for a feedstock of category a;
wherein ,b controlling the average specific heat between the temperature of the feeding nozzle and the index temperature of the discharging nozzle in the interval under the condition of stable reaction rate of the raw materials with the category a;
ΔT a,b b controlling the temperature difference between the non-index temperature of the interval section and the temperature of the feeding nozzle of the control section under the condition of stable reaction rate for the raw material with category a;
q is the heating value of the fuel.
3. The method for controlling heat of a reaction vessel according to claim 2, wherein O (a) is a preparation amount of a raw material of category a in each of the control intervals for 60 minutes under the condition of a stable reaction rate, a preparation amount of a raw material in each of the control intervals for 60 minutes under the condition of a stable reaction rate is equal,wherein m (b) is the mass 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 product flow rate;
u (a, b) is the fuel usage rate of the feedstock of category a in the b-th control zone under conditions of stable reaction rate; u (a, b) =q 1 (a,b)/Q 2 (a,b)，
in the formula ,Q2 (a, b) is the actual flow rate of the feedstock of category a at the b-th control zone under conditions of stable reaction rate.
4. The method for controlling heat of a reaction vessel according to claim 1, wherein the mass O (a, b) of the solution in the vessel for 60 minutes is the mass O (a, b) of the solution in the control section b,wherein m (a, b) is the quality of the synthesized product in the b-th mastering interval of the solution with category a in the state of being prepared in the process; solving, in the preparation state, the flow standard value Q of the fuel required by the b control interval 3 (b)＝∑Q 3 (a, b) and the situation of preparation at the moment, the b-th control interval requires a fuel flow solving value Q 4 (b)＝∑ 4 Q (a, b); finally, solving the utilization rate of the b-th control zone in the preparation situation at the moment>
wherein ,Q3 (a, b) in the case of the preparation at this time, the preparation amount of the solution of category a in the b-th control interval for 60 minutes requires a fuel flow specification value;
Q 2 (a, b) the same raw material formulation as category a, and the same content of the solution is used for actually monitoring the fuel flow in the b control interval under the stable reaction rate;
wherein: o (a, b) in the case of this preparation, the yield of the synthesis product of 60 minutes in the b-th control zone of the stock solution category a;
the average specific heat between the temperature of the input nozzle and the index temperature of the output nozzle in the b control interval under the condition of stable reaction rate for the solution in the container with the category a;
ΔT’ a,b in the case of the preparation at this time, the difference between the index temperature of the solution in the container of category a at the tail section of the control section b and the temperature of the input nozzle of the control section b;
q is the heating value of the fuel.
5. The method for controlling heat of a reaction vessel according to claim 1, wherein the specific step of correcting the difference in the flow rate of the fuel to the temperature of the reaction vessel under different conditions is realized: 1. establishing a flow correction coefficient alpha (b) and a flow change trend correction coefficient beta (b) of a b-th control interval, wherein alpha (b) is between 0.1 and 0.7, and beta (b) is between 0.2 and 0.5; prescribed fuel flow deviation Δq (b) =q 5 (b)-Q 3 (b) Solving for fuel flow deviation value DeltaQ 1 (b)＝Q 5 (b)-Q 4 (b)，ΔQ 2 (b)＝Q 5 (b)-Q 5 Old one (b)，Q 5 (b) In the preparation case of the time, the b-th control interval actually monitors the fuel flow value; q (Q) 5 Old one (b) In the preparation case, the b-th control section monitors the fuel flow value monitored last time; 2. by DeltaQ (b), deltaQ 1 (b) Δq 2 (b) According to experience, selecting proper flow correction coefficient alpha (b) and flow change trend correction coefficient beta (b); 3. the temperature correction coefficient Φ (b) =α (b) ×β (b) of the b-th control section in the production case at this time is obtained.
6. The method for controlling the heat of a reaction vessel according to claim 1, wherein the final determination value T "(b) of the vessel temperature in the control interval is calculated by the following specific solving process:
T”(b)＝T(b)-ΔT”(b)
wherein ΔT "(b) is the correction 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;
θ is the air-fuel ratio;
in the case of this time preparation, the b-th control section removes the loss of other heat than the heat absorbed by the prepared product;
gamma is the ratio of oil smoke generated by burning fuel;
C’ o in the preparation case, the monitoring part in the b-th control interval monitors the specific heat of the oil smoke with the matched temperature;
q is the fuel heating value.
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