Thermal safety risk assessment method for benzyl alcohol oxidation reaction

Abstract

The invention provides a benzyl alcohol oxidation reaction thermal safety risk assessment method, and relates to the technical field of thermal risk analysis. The thermal safety risk assessment method for the benzyl alcohol oxidation process comprises the following steps: step 1, testing the thermal stability of a material; step two, reaction calorimetry testing of the oxidation reaction; step 3, secondary decomposition test of oxidation reaction completion liquid; and 4, evaluating the safety risk of the oxidation reaction. Through thermal risk assessment of oxidation reaction, thermal stability of various raw materials, intermediates and products involved in the process, compatibility between TCCA and different solvents and thermodynamic characteristics in the reaction process are deeply analyzed, and a safety risk assessment model of benzyl alcohol oxidation reaction heat is established. Effective technical support and guarantee can be provided for thermal safety and production safety accident prevention in the production process of the oxidation process according to the evaluation result, and the method has very important significance for safety production in the chemical industry.

Description

Technical Field

[0001] The invention relates to the technical field of thermal risk analysis processes, and in particular to a thermal safety risk assessment method for a benzyl alcohol oxidation reaction. Background Art

[0002] my country's chemical industry is one of the pillar industries of the national economy and is at the forefront of the world. However, while it brings convenience to people, it also brings huge safety hazards. The raw materials and products involved in the production, storage, transportation, use and waste disposal are often flammable, explosive or toxic, harmful, corrosive and other characteristics. If they are misused, abused or improperly disposed, they are very likely to cause accidents such as combustion, explosion, and poisoning. There are many chemical companies, and the complex and diverse processes and production equipment involved exacerbate this risk. This will not only cause casualties and property losses, but may also have irreversible negative impacts on the environment.

[0003] Although oxidation processes have been included in high-risk processes, the current thermal hazard assessment methods for oxidation processes are slightly insufficient, and the reaction has the risk of material impact or even explosion in actual production. Due to the lack of analytical research, the reaction is likely to lose control during process production, which can easily cause heat accumulation or accidental release, and can easily lead to major production safety accidents. Therefore, it is extremely important for the chemical industry to discover and master more thermal safety risk assessment methods for oxidation reactions, and to identify and reduce risks in the materials and reaction exothermic and gas release processes involved before process production. Summary of the invention

[0004] The purpose of the present invention is to provide a method for thermal safety risk assessment of benzyl alcohol oxidation reaction, which solves the problem that there is a lack of thermal safety risk assessment methods for oxidation process reactions in China.

[0005] The technical solution adopted by the present invention to solve the above technical problems is as follows:

[0006] The present invention provides a thermal safety risk assessment method for a benzyl alcohol oxidation reaction, comprising the following steps:

[0007] S1: Material thermal stability test

[0008] A thermal stability test is performed on a benzyl alcohol oxidation reaction solution using a differential scanning calorimeter; the benzyl alcohol oxidation reaction solution comprises benzyl alcohol, an oxidant, a catalyst and a solvent;

[0009] The oxidant is selected from any one of TCCA, PCC, NaClO, MnO2, and DMSO;

[0010] The catalyst is selected from TEMPO;

[0011] The solvent is selected from any one of EA, DMF, CH3CN, Acetone, H2O or dichloromethane;

[0012] S2: Reaction calorimetry test of oxidation reaction

[0013] The test was carried out using a fully automated chemical synthesis reactor according to the following process:

[0014] a. First, add the solvent, benzyl alcohol and catalyst to feed;

[0015] b. Lower the temperature to 0 degrees Celsius;

[0016] c. Perform stable calibration;

[0017] d. adding oxidant in batches;

[0018] e. Insulation reaction;

[0019] f. Stable calibration;

[0020] g. Data calculation and analysis;

[0021] Thus, the charging curve (Mr), the heat released curve (qr_hf)1, the heat conversion rate curve (qr_hf integral 1.Conversion), the heat accumulation rate curve (Thermal Accumulation (qr_hf)1), the cooling failure curve (Tcf), the reaction temperature curve (Tr), and the jacket temperature curve (Tj) during the oxidation reaction are obtained;

[0022] S3: Secondary decomposition test of the oxidation reaction completed liquid

[0023] The oxidation reaction completion liquid was subjected to secondary decomposition test using TAC-500A adiabatic accelerating calorimeter to obtain: the time-temperature curve of the HWS mode test of the oxidation reaction completion liquid ARC, the temperature-temperature rise rate curve of the exothermic section of the HWS mode test of the oxidation reaction completion liquid ARC, the calculation of the kinetic parameters of the oxidation reaction completion liquid, and the adiabatic experiment TMR diagram;

[0024] S4: Oxidation reaction safety risk assessment

[0025] The safety risk assessment of oxidation reactions includes the following assessment contents:

[0026] Material decomposition heat assessment, severity assessment, possibility assessment, risk matrix assessment, reaction process hazard assessment.

[0027] As a preferred embodiment, the benzyl alcohol oxidation reaction solution in step S1 comprises benzyl alcohol, an oxidant, a catalyst and a solvent;

[0028] The oxidant is selected from TCCA; the catalyst is selected from TEMPO; and the solvent is selected from dichloromethane.

[0029] As a preferred embodiment, the reaction calorimetry test of the oxidation reaction in step S2 further comprises the following steps:

[0030] The test was carried out using a fully automated chemical synthesis reactor according to the following process:

[0031] a. First, add dichloromethane, benzyl alcohol and TEMPO to feed;

[0032] b. Lower the temperature to 0 degrees Celsius;

[0033] c. Perform stable calibration;

[0034] d. Join TCCA in batches;

[0035] e. Insulation reaction;

[0036] f. Stable calibration;

[0037] g. Data calculation and analysis;

[0038] Thus, the charging curve (Mr), the heat released curve (qr_hf)1, the thermal conversion rate curve (qr_hf integral 1.Conversion), the thermal accumulation rate curve (Thermal Accumulation(qr_hf)1), the cooling failure curve (Tcf), the reaction temperature curve (Tr), and the jacket temperature curve (Tj) during the oxidation reaction are obtained.

[0039] As a preferred embodiment, the process of the benzyl alcohol oxidation reaction is as follows:

[0040] Add dichloromethane, benzyl alcohol and TEMPO into the reaction kettle, stir to dissolve, then add TCCA in seven batches, with an interval of 10-20 minutes between each batch. After the addition is completed, keep the temperature for 1 hour;

[0041] The chemical reaction formula is as follows:

[0042]

[0043] As a preferred embodiment, the fully automatic chemical synthesis reactor is selected from EasyMax 402 or RC1mx.

[0044] Compared with the prior art, the present invention has the following beneficial effects:

[0045] (1) The present invention provides a method for thermal safety risk assessment of benzyl alcohol oxidation reaction, which can provide effective technical support and guarantee for thermal safety of the production process of oxidation process and prevention of production safety accidents according to the assessment results, and is of great significance to production safety and major accident prevention in the chemical industry.

[0046] (2) In common oxidation reactions, when TCCA is used as an oxidant in the reaction, most solvents react with it, which leads to a decrease in the reaction yield. More importantly, when the solvent reacts with TCCA, a large amount of heat is generated, which brings unnecessary thermal risks to the reaction. The present invention screens out the optimal reaction solvent DCM by testing solutions of different solvents mixed with TCCA, thereby effectively solving the problem of such reactions.

[0047] (3) The reaction heat of the oxidation reaction is usually large, which leads to great risks in factory production. The present invention reduces heat accumulation to a great extent and greatly improves the safety of the process by adding TCCA in batches and waiting for each batch of heat to be released before adding the next batch of materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0048] Figure 1 This is the DSC test curve of benzyl alcohol.

[0049] Figure 2 This is the DSC test curve of TCCA.

[0050] Figure 3 This is the DSC test curve of TCCAin 5V EA.

[0051] Figure 4 This is the DSC test curve of TCCA in 5V DMF.

[0052] Figure 5 This is the DSC test curve of TCCA in 5V CH3CN.

[0053] Figure 6 This is the DSC test curve of TCCA in 5V Acetone.

[0054] Figure 7 This is the DSC test curve of TCCAin 5V H2O.

[0055] Figure 8 This is the DSC test curve of TCCA in 5V DCM.

[0056] Fig. 9 This is the DSC test curve of TEMPO.

[0057] Fig.10It is a DSC test curve diagram of benzyl alcohol oxidation reaction liquid, wherein the oxidation reaction liquid includes benzyl alcohol, oxidant TCCA, catalyst TEMPO and solvent DCM.

[0058] Fig.11 They are the charging curve (Mr) of the oxidation reaction process, the heat released curve (qr_hf)1, the thermal conversion rate curve (qr_hf integral 1.Conversion), the thermal accumulation rate curve (Thermal Accumulation(qr_hf)1), the cooling failure curve (Tcf), the reaction temperature curve (Tr), and the jacket temperature curve (Tj).

[0059] Fig.12 The time-temperature curve of the ARC HWS mode test for the oxidation reaction completion liquid.

[0060] Fig.13 This is the temperature-temperature rise rate curve of the exothermic section of the ARC HWS mode test of the oxidation reaction completion liquid.

[0061] Fig.14 Complete the hydrodynamic parameter diagram for the oxidation reaction.

[0062] Fig.15 TMR diagram of the liquid adiabatic test completed for the oxidation reaction. DETAILED DESCRIPTION

[0063] The technical solution of the present invention is described in detail below in conjunction with the embodiments. The reagents and biological materials used below are all commercial products unless otherwise specified.

[0064] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0065] Embodiment 1:

[0066] This embodiment provides a method for thermal safety risk assessment of benzyl alcohol oxidation reaction, comprising the following steps:

[0067] Step 1: Material thermal stability test

[0068] An embodiment of the present invention provides a method for thermal safety risk assessment of benzyl alcohol oxidation reaction, comprising the following steps:

[0069] Step 1: Material thermal stability test

[0070] Using a differential scanning calorimeter, the thermal stability of benzyl alcohol, oxidant TCCA and catalyst TEMPO were first tested respectively; TCCA was then mixed with one of ethyl acetate (EA), dimethylformamide (DMF), acetonitrile (CH3CN), acetone (Acetone), H2O and dichloromethane (DCM) solvents, and the mixed solution was tested for thermal stability to screen out solvents suitable for the following processes; the reaction solution of benzyl alcohol oxidation was tested for thermal stability;

[0071] Figure 1 is the DSC test curve of benzyl alcohol, Figure 1 It can be seen that an exothermic peak is detected between (0-400)°C, which starts from 169.84°C and ends at 227.32°C, and the heat released is 23.45 J / g.

[0072] Figure 2 is the DSC test curve of the oxidant TCCA; Figure 2 It can be seen that two endothermic peaks and one exothermic peak are detected between (0-400)℃, the first endothermic peak starts from 132.63℃ and ends at 162.45℃, the second endothermic peak starts from 225.32℃ and ends at 250.59℃, the exothermic peak starts from 279.54℃ and ends at 400℃, and the heat released is 2092.21J / g. This compound is a high-energy compound, 1200J / g<decomposition heat<3000J / g, the decomposition heat is large, and the potential explosion hazard is high.

[0073] Figure 3 is the DSC test curve of TCCA in 5V EA; Figure 3 It can be seen that 3 exothermic peaks and 2 endothermic peaks are detected between (0-400)℃. The first exothermic peak starts from 62.88℃ and ends at 203.12℃, releasing 399.60J / g of heat. The second exothermic peak starts from 209.60℃ and ends at 246.97℃, releasing 14.93J / g of heat. The first endothermic peak starts from 350.49℃ and ends at 373.37℃. The third exothermic peak starts from 373.37℃ and ends at 377.27℃, releasing 5.62J / g of heat. The second endothermic peak starts from 377.27℃ and ends at 399.79℃. At 5V When TCCA was added to the EA solution, the temperature rose rapidly and a yellow-green gas was released, indicating that TCCA reacted with the solvent EA. The DSC spectrum also showed that the decomposition exothermic peak of TCCA disappeared, and several different peaks were generated starting from 62.88°C, which meant that when TCCA was used as an oxidant, EA as a solvent would introduce exothermic reaction and also reduce the yield of the reaction.

[0074] Figure 4 is the DSC test curve of TCCA in 5V DMF; Figure 4 It can be seen that three exothermic peaks are detected between (0-400)°C, the first exothermic peak starts from 27.23°C and ends at 166.88°C, releasing 156.99 J / g of heat, the second exothermic peak starts from 176.60°C and ends at 292.46°C, releasing 214.36 J / g of heat, and the third exothermic peak starts from 296.78°C and ends at 400°C, releasing 352.17 J / g of heat; when TCCA is added to the 5V DMF solution, the temperature rises rapidly and a yellow-green gas is released, indicating that TCCA reacts with the solvent DMF; from the DSC spectrum, it can also be seen that the decomposition exothermic peak of TCCA disappears, and several different peaks are generated starting from 27.23°C, which means that when TCCA is used as an oxidant, DMF as a solvent will introduce exothermic heat and also lead to a decrease in the yield of the reaction.

[0075] Figure 5 is the DSC test curve of TCCA in 5V CH3CN; Figure 5 It can be seen that three exothermic peaks are detected between (0-400)°C, the first exothermic peak starts from 51.46°C and ends at 208.55°C, releasing 452.48 J / g of heat, the second exothermic peak starts from 291.60°C and ends at 367.42°C, releasing 72.02 J / g of heat, and the third exothermic peak starts from 368.50°C and ends at 400°C, releasing 154.75 J / g of heat; when TCCA is added to 5V CH3CN solution, the temperature rises rapidly and a yellow-green gas is released, indicating that TCCA reacts with the solvent CH3CN; from the DSC spectrum, it can also be seen that the decomposition exothermic peak of TCCA disappears, and several different peaks are generated starting from 51.46°C, which means that when TCCA is used as an oxidant, CH3CN as a solvent will introduce exothermic heat, which will also lead to a decrease in the yield of the reaction.

[0076] Figure 6 is the DSC test curve of TCCA in 5V Acetone; Figure 6It can be seen that two exothermic peaks are detected between (0-400)℃, the first exothermic peak starts from 59.03℃ and ends at 148.52℃, releasing 435.44J / g of heat, and the second exothermic peak starts from 256.98℃ and ends at 400℃, releasing 617.47J / g of heat; when TCCA is added to the 5V Acetone solution, the temperature rises rapidly and a yellow-green gas is released, indicating that TCCA reacts with the solvent Acetone; from the DSC spectrum, it can also be seen that the decomposition exothermic peak of TCCA disappears, and several different peaks are generated starting from 59.03℃, which means that when TCCA is used as an oxidant, Acetone as a solvent will introduce exothermic heat and also lead to a decrease in the yield of the reaction.

[0077] Figure 7 is the DSC test curve of TCCA in 5V H2O; Figure 7 It can be seen that 2 exothermic peaks and 1 endothermic peak are detected between (0-400)℃, the first exothermic peak starts from 52.97℃ and ends at 252.63℃, releasing 408.30J / g of heat, the second exothermic peak starts from 258.68℃ and ends at 310.32℃, releasing 68.38J / g of heat, and the endothermic peak starts from 315.30℃ and ends at 348.23℃; when TCCA is added to 5V H2O solution, the temperature rises rapidly and a yellow-green gas is released, indicating that TCCA reacts with the solvent H2O; from the DSC spectrum, it can also be seen that the decomposition exothermic peak of TCCA disappears, and several different peaks are generated starting from 52.97℃, which means that when TCCA is used as an oxidant, H2O as a solvent will introduce exothermic heat and also lead to a decrease in the yield of the reaction.

[0078] Figure 8 is the DSC test curve of TCCA in 5V DCM; Figure 8 It can be seen that 2 endothermic peaks and 1 exothermic peak were detected between (0-400)℃. The first endothermic peak started from 129.42℃ and ended at 159.24℃. The second endothermic peak started from 190.14℃ and ended at 206.99℃. The exothermic peak started from 242.84℃ and ended at 400℃. The heat released was 1967.25J / g. When TCCA was added to the 5V DCM solution, the temperature hardly changed and no gas was generated. There was no obvious peak generated from the DSC spectrum. Therefore, when TCCA was used as an oxidant and DCM was used as a solvent, TCCA in 5V DCM had good stability.

[0079] Fig. 9 is the DSC test curve of TEMPO; Fig. 9It can be seen that one endothermic peak and one exothermic peak are detected between (0-400)℃. The endothermic peak starts from 30.88℃ and ends at 61.78℃, and the exothermic peak starts from 185.15℃ and ends at 368.56℃. The heat released is 1239.42J / g. This compound is a high-energy compound, 1200J / g<decomposition heat<3000J / g, the decomposition heat is large, and the potential explosion hazard is high.

[0080] From the DSC curves of TCCA in different solvents, it can be seen that TCCA and EA, DMF, CH3CN, Acetone, and H2O all have obvious heat release at very low temperatures and release yellow-green gas. When TCCA and DCM are mixed, there is almost no obvious heat release peak below 200°C, and it has good stability. Therefore, the present invention uses benzyl alcohol, oxidant TCCA, catalyst TEMPO and solvent DCM to form a benzyl alcohol oxidation reaction liquid.

[0081] Fig.10 The DSC test curve of the benzyl alcohol oxidation reaction solution, wherein the oxidation reaction solution includes benzyl alcohol, oxidant TCCA, catalyst TEMPO and solvent DCM. Fig.10 It can be seen that two exothermic peaks are detected between (0-400)℃. The first exothermic peak starts from 210.42℃ and ends at 232.24℃, releasing 4.83J / g of heat. The second exothermic peak starts from 339.87℃ and ends at 400℃, releasing more than 288.75J / g of heat.

[0082] Step 2: Calorimetric measurement of oxidation reaction

[0083] The reaction calorimetry of the reaction mixture was tested using the fully automatic chemical synthesis reactor EasyMax 402 according to the following process:

[0084]

[0085] Thus, the charging curve (Mr), the heat released curve (qr_hf)1, the heat conversion rate curve (qr_hf integral 1.Conversion), the heat accumulation rate curve (Thermal Accumulation(qr_hf)1), the cooling failure curve (Tcf), the reaction temperature curve (Tr), and the jacket temperature curve (Tj) in the process of benzyl alcohol oxidation reaction are obtained, such as Fig.11As shown in the figure, the qr_hf curve is the heat effect curve of the exothermic process. After integrating the time, the total heat release of the reaction is obtained. It can be calculated that during the addition process of this reaction, the temperature in the kettle increases, and during the insulation reaction process, the temperature in the kettle is stable. The total heat released is 23.25kJ, and the total mass of the materials participating in the reaction is 244.98g. Therefore, the specific heat release of this reaction is 95J / g;

[0086] ΔTad is the adiabatic temperature rise, which is the total heat released by the synthesis reaction or material decomposition, and the temperature at which the system can rise under adiabatic conditions. The ΔTad of this reaction is 85.4K;

[0087] MTSR is the highest temperature that the system can reach under adiabatic conditions when the material accumulation is maximum. Through calculation, the highest temperature MTSR corresponding to the runaway reaction in the oxidation reaction process is 39°C.

[0088] Since the oxidation reaction of benzyl alcohol is a normal pressure reaction, the technical maximum temperature MTT is the boiling point of the largest material in the reaction system under normal pressure, that is, the boiling point of dichloromethane: 39.75°C;

[0089] Step 3: Secondary decomposition test of the oxidation reaction completed liquid

[0090] The secondary decomposition test of the oxidation reaction completion liquid was carried out using a TAC-500A adiabatic accelerating calorimeter to obtain the following time-temperature curve of the oxidation reaction completion liquid ARC HWS mode test ( Fig.12 , the curves are sample temperature, upper cover temperature, instrument environment temperature, bottom temperature), temperature-temperature rise rate curve of the exothermic section of the oxidation reaction completion liquid ARC HWS mode test ( Fig.13 ); after that, the oxidation reaction completed liquid was subjected to kinetic parameter calculation and adiabatic test TMR calculation, and the calculation result graphs correspond to Fig.14 , Fig.15 .

[0091] Depend on Figure 12-14 It can be seen that the initial decomposition temperature of the oxidation reaction completion liquid is 230.43℃, the decomposition reaction does not stop at 500.02℃ (reaching the upper limit of the instrument), the heat release is 1396.94J / g, and the adiabatic temperature rise ΔTad of the secondary reaction process of the oxidation reaction completion liquid is 504.41℃ (after correction). Fig.15 Calculation shows that Td24 is 154.50℃, and when the process temperature is 0℃, the maximum reaction rate of the runaway reaction reaches TMRad>24h, and when the temperature reaches the maximum temperature of the system (MTSR), the maximum reaction rate of the runaway reaction reaches TMRad>24h;

[0092] Step 4: Oxidation reaction safety risk assessment

[0093] The safety risk assessment for oxidation reactions includes the following:

[0094] Material decomposition heat assessment, severity assessment, possibility assessment, risk matrix assessment, reaction process hazard assessment;

[0095] Material decomposition heat assessment: According to the adiabatic calorimetry test results of the oxidation reaction completed liquid, the decomposition heat of the oxidation reaction completed liquid is 1200J / g<1396.94J / g<3000J / g, which is assessed as Level 3. The material decomposition heat is large and the potential explosion hazard is high;

[0096] Severity assessment: According to the reaction calorimetry test results of the oxidation reaction, the adiabatic temperature rise ΔTad = 504.41K, ΔTad ≥ 400K, and the severity of the runaway oxidation reaction is assessed as Level 4. The runaway reaction may cause devastating losses to the factory;

[0097] Possibility assessment: According to the adiabatic calorimetry test results of the oxidation reaction completion liquid, the Td24 of the completion reaction liquid is 154.50°C. When the system process temperature is 0°C, the maximum reaction rate of the runaway reaction reaches TMRad>24h. When the temperature reaches the system maximum temperature (MTSR), the maximum reaction rate of the runaway reaction reaches TMRad>24h. The possibility of the runaway reaction is assessed to be level 1, and the runaway reaction is less likely to occur.

[0098] Risk matrix assessment: Based on the results of severity assessment and possibility assessment, the risk matrix assessment is Level II, and Level II risk is conditionally acceptable risk: Under the condition that control measures are implemented, the risk level can be reduced through process optimization, engineering, and management control measures;

[0099] Reaction process hazard assessment: According to the reaction calorimetry test results of the oxidation reaction, the process temperature Tp = 0°C, the highest temperature that the synthesis reaction may reach at the actual feeding rate under adiabatic conditions MTSR = 39°C, the technical maximum temperature MTT = 39.75°C, and according to the secondary decomposition test of the oxidation reaction completed liquid Td24 = 154.50°C, it is obtained that Tp < MTSR < MTT < Td24 (0°C < 39°C < 39.75°C < 154.50°C), that is, the reaction process hazard assessment at the actual feeding rate is level 1.

[0100] The process of benzyl alcohol oxidation reaction is as follows:

[0101] Add dichloromethane, benzyl alcohol and TEMPO into the reaction kettle, stir and dissolve, then add TCCA in batches, add in seven batches, each batch is added with an interval of 10-20min, and keep warm for 1h after adding. The chemical reaction formula is as follows:

[0102]

[0103] After the target reaction of this process gets out of control, if the temperature does not reach the technical limit (i.e., MTSR < MTT), and since MTSR is lower than Td24, then the decomposition reaction will not be triggered. The reaction risk of this process is relatively low, but since MTSR is close to MTT, a conventional automatic control system should be configured to centrally monitor and automatically adjust the main reaction parameters (DCS or PLC). Alarm and interlock controls for deviations from normal values should be set. Once the reaction deviates from the normal value, the heat source supply should be cut off, and the reaction materials should not stay in the accumulation state for a long time.

[0104] The above are only some preferred embodiments of the present invention, and the present invention is not limited to the content of the embodiments. For those skilled in the art, various changes and modifications can be made within the scope of the concept of the technical solution of the present invention, and any changes and modifications made are within the protection scope of the present invention.

Claims

1. A method for thermal safety risk assessment of benzyl alcohol oxidation reaction, characterized in that: The following steps are involved: S1: Material thermal stability test A thermal stability test is performed on a benzyl alcohol oxidation reaction solution using a differential scanning calorimeter; the benzyl alcohol oxidation reaction solution comprises benzyl alcohol, an oxidant, a catalyst and a solvent; The oxidant is selected from any one of TCCA, PCC, NaClO, MnO2, and DMSO; The catalyst is selected from TEMPO; The solvent is selected from any one of EA, DMF, CH3CN, Acetone, H2O or dichloromethane; S2: Reaction calorimetry test of oxidation reaction The test was carried out using a fully automated chemical synthesis reactor according to the following process: a. First, add the solvent, benzyl alcohol and catalyst to feed; b. Lower the temperature to 0 degrees Celsius; c. Perform stable calibration; d. adding oxidant in batches; e. Insulation reaction; f. Stable calibration; g. Data calculation and analysis; Thus, the charging curve (Mr), the heat released curve (qr_hf)1, the heat conversion rate curve (qr_hf integral 1.Conversion), the heat accumulation rate curve (Thermal Accumulation (qr_hf)1), the cooling failure curve (Tcf), the reaction temperature curve (Tr), and the jacket temperature curve (Tj) during the oxidation reaction are obtained; S3: Secondary decomposition test of the oxidation reaction completed liquid The oxidation reaction completion liquid was subjected to secondary decomposition test using TAC-500A adiabatic accelerating calorimeter to obtain: the time-temperature curve of the oxidation reaction completion liquid ARC HWS mode test, the temperature-temperature rise rate curve of the exothermic section of the oxidation reaction completion liquid ARC HWS mode test, the calculation of the kinetic parameters of the oxidation reaction completion liquid and the adiabatic experiment TMR diagram; S4: Oxidation reaction safety risk assessment The safety risk assessment of oxidation reactions includes the following assessment contents: Material decomposition heat assessment, severity assessment, possibility assessment, risk matrix assessment, reaction process hazard assessment.

2. The method for safety risk assessment of benzyl alcohol oxidation reaction heat according to claim 1, characterized in that: The benzyl alcohol oxidation reaction solution in step S1 comprises benzyl alcohol, an oxidant, a catalyst and a solvent; The oxidant is selected from TCCA; the catalyst is selected from TEMPO; and the solvent is selected from dichloromethane.

3. The method for safety risk assessment of benzyl alcohol oxidation reaction heat according to claim 1, characterized in that: The reaction calorimetric test of the oxidation reaction in step S2 further comprises the following steps: The test was carried out using a fully automated chemical synthesis reactor according to the following process: a. First, add dichloromethane, benzyl alcohol and TEMPO to feed; b. Lower the temperature to 0 degrees Celsius; c. Perform stable calibration; d. Join TCCA in batches; e. Insulation reaction; f. Stable calibration; g. Data calculation and analysis; Thus, the charging curve (Mr), the heat released curve (qr_hf)1, the thermal conversion rate curve (qr_hf integral 1.Conversion), the thermal accumulation rate curve (Thermal Accumulation(qr_hf)1), the cooling failure curve (Tcf), the reaction temperature curve (Tr), and the jacket temperature curve (Tj) during the oxidation reaction are obtained.

4. The thermal safety risk assessment method for the benzyl alcohol oxidation reaction according to claim 1, characterized in that: The process of the benzyl alcohol oxidation reaction is as follows: Add dichloromethane, benzyl alcohol and TEMPO into the reaction kettle, stir to dissolve, then add TCCA in seven batches, with an interval of 10-20 minutes between each batch. After the addition is completed, keep the temperature for 1 hour; The chemical reaction formula is as follows:

5. The thermal safety risk assessment method for the benzyl alcohol oxidation reaction according to claim 1, characterized in that: The fully automatic chemical synthesis reactor is selected from EasyMax 402 or RC1mx.

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