Method and device for measuring calorimetry of non-isothermal reaction process

A technology of reaction process and measurement method, applied in the direction of material thermal development, etc., can solve the problem of lack of non-isothermal reaction process calorimetric methods

Pending Publication Date: 2018-09-14
SHENYANG RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem of lack of non-isothermal reaction process calorimetric methods in the prior art, the purpose of the present invention is to provide a non-isothermal reaction process calorimetric measurement method and device

Method used

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  • Method and device for measuring calorimetry of non-isothermal reaction process
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  • Method and device for measuring calorimetry of non-isothermal reaction process

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Experimental program
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Effect test

Embodiment 1

[0074] Such as figure 1 As shown, the present invention includes a control system and a reaction system module, wherein the reaction system module includes a reactor 1, a feeding system 4, a distillation system 5, a heater 9, a temperature control module, and a pressure monitoring module. The reactor 1 is equipped with a stirring system 6, the feeding system 4 is connected to the feed port of the reactor 1 through a pipeline, and the distillation and back distillation system 5 is connected to the discharge port of the reactor 1 through a pipeline. The back distillation system 5 is controlled by the control system to start and stop. One end of the heater 9 extends into the reactor 1 and heats the interior of the reactor 1, and the heater 9 transmits to the control system through the temperature control module. A signal is sent to adjust the heating temperature, and a pressure monitoring module is provided in the reactor 1.

[0075] Such as figure 1 As shown, the control system i...

Embodiment 2

[0090] Acetic anhydride hydrolysis test.

[0091] According to the above device, water was added to the reactor. After the addition, the feed port of the reactor was sealed, and then acetic anhydride was added dropwise through the liquid feeding system. The molar ratio of acetic anhydride to water was 1:22.7. Acetic anhydride was added dropwise at 30°C. , After 50min of dripping, the reaction is kept for 10min after the dropping; the temperature is raised to 40℃ at a rate of 1℃ / min, and the reaction is kept for 1h; the temperature is raised to 50℃ at a rate of 1℃ / min, and the reaction is kept for 1h, and the reaction is over.

[0092] experiment procedure:

[0093] According to the actual feeding situation, set the control program, drip temperature 30℃, stir 300rpm, run heating, calibration, dripping materials, heat preservation, heat preservation, heat preservation, heat preservation, heat preservation, calibration procedures in sequence; The material system is cleaned; the experim...

Embodiment 3

[0097] 3-cyanopyridine and phosphorus oxychloride are chlorinated to prepare 2-chloro-3-cyanopyridine.

[0098] According to the above device records, solid 3-cyanopyridine, dimethylformamide and xylene were added to the reactor. After the addition, the reactor inlet was sealed, and then phosphorus oxychloride was added dropwise through the liquid feeding system. The molar ratio of cyanopyridine (104), phosphorus oxychloride (153.3), dimethylformamide (73.1) and xylene (106.2) is 1:1.3:1.8:2. Phosphorus oxychloride is added dropwise at 90°C, After 1h of dripping, the reaction is kept for 2h after dripping; the temperature is raised to 100°C at a rate of 0.5°C / min, and the reaction is kept for 3h; the temperature is raised to 120°C at a rate of 1°C / min, and the reaction is kept for 2h, and the reaction is over.

[0099] experiment procedure:

[0100] According to the actual feeding situation, set the control program, drip temperature 90℃, stir 300rpm, run heating, calibration, drippi...

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Abstract

The invention belongs to the field of chemical safety technology and engineering, and relates to a method and a device for measuring calorimetry of a non-isothermal reaction process. Reaction temperature gradients T1, T2, T3 to Tn are set according to the non-isothermal reaction, initial acquisition temperature T0 is obtained, and generation reaction heat DELTArHm (generation) is calculated and obtained; according to the non-isothermal reaction, blank experimental reaction heat DELTArHm (blank) is obtained; according to the generation reaction heat DELTArHm (generation) and the blank experimental reaction heat DELTArHm (blank), heat effect caused by temperature rise during the reaction calorimetry process is obtained and deducted, and target reaction heat DELTArHm is obtained. The method adopts a non-isothermal heat flow mode to carry out the reaction calorimetry to realize real-time collection of various heat data in the reaction process and risk assessment on the non-isothermal reaction.

Description

Technical field [0001] The invention belongs to the field of chemical safety technology and engineering, and relates to a method and device for measuring calorimetry in a non-isothermal reaction process. Background technique [0002] To conduct thermal risk assessment for a specific chemical reaction process, it is necessary to obtain parameters such as the amount of heat released by the reaction process, the specific heat capacity of the reaction material, the rate of heat release, the rate of heat conversion, and the rate of gas release. These parameters must be obtained through the calorimetry of the reaction, with the help of different Research equipment to achieve calorimetric testing by means of isothermal calorimetry, non-isothermal calorimetry, and steam reflux heat. [0003] Patents US8815601, US12767019, CN101603935A mainly introduce the equipment structure, control principle and instrument operation method of the conventional reaction calorimeter, and do not involve non-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N25/20
CPCG01N25/20
Inventor 程春生魏振云马晓华李全国吕国锋赵闯刘玄孔蓉
Owner SHENYANG RES INST OF CHEM IND
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