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Calorimetric testing method and device of continuous flow gas-phase reaction technology

The technology of a testing device and a testing method, which is applied in the field of calorimetric testing of a continuous flow gas phase reaction process, can solve problems such as the lack of calorimetric testing of a continuous flow chemical process, improve collection sensitivity, meet measurement accuracy requirements, and solve temperature measurement problems Effect

Pending Publication Date: 2018-09-04
SHENYANG RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problem of lack of calorimetric testing of continuous flow chemical process in the prior art, the present invention provides a calorimetric testing method and device for continuous flow gas phase reaction process

Method used

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Embodiment 1

[0042] Such as figure 1 As shown, the present invention includes a reactor 22, a control unit 19, a central control system 20 and a plurality of sensors, wherein the reactor 22 is provided with a reaction test pool 21, and the reactor 22 and the reaction test pool 21 are both airtight , the reactor 22 provides a sealed reaction environment for the reaction test pool 21, and the multiple sensors include sensors for monitoring the internal temperature and pressure of the reactor 22 and sensors for monitoring the reaction test pool. 21 internal temperature and pressure sensors, each sensor is connected to the control unit 19, the control unit 19 is connected to the central control system 20, and the reaction test pool 21 is provided with independent feed channels and outlets. The feed channel, and both the feed channel and the discharge channel extend to the outside of the reactor 22, and the feed channel is connected with the feed system. Both the reactor 22 and the reaction te...

Embodiment 2

[0062] In this example, the process of trichlorethylene and hydrogen fluoride to generate 1,1,1-trifluoro-2-chloroethane through addition and substitution reaction is taken as an example, and the solid catalyst is CrO-Y 2 o 3 . The invented calorimetric test method will be described. The feed molar ratio of chloroalkene and hydrogen fluoride is 1:3.05, the reaction temperature range is 220-300°C, the material residence time is 30-90s, and the reaction pressure is 0.8-1.05Mpa.

[0063] experiment procedure:

[0064]1) Air tightness test of the reaction system. Connect the reaction system to the nitrogen cylinder, feed nitrogen into the system through the pressure reducing valve, the nitrogen pressure reaches 2.0MPa, keep the pressure for 1 hour, during the pressure keeping process, the pressure drop of the reactor system is less than 0.01bar / min, it is considered that there is no leakage in the reaction system , the end of holding pressure;

[0065] 2) Pressure relief. Af...

Embodiment 3

[0082] This embodiment takes 1,1,2-trifluoro-1,2,2-trichloroethane and hydrogen as an example to generate chlorotrifluoroethylene through catalytic reaction, and selects copper, lanthanum and activated carbon supported solid catalyst (copper is the main active component, lanthanum is the modifier component, and activated carbon is the carrier). The invented calorimetric test method will be described. The feed molar ratio of 1,1,2-trifluoro-1,2,2-trichloroethane and hydrogen is 1:3, the reaction temperature range is 130-180°C, and the material residence time is 30-40s. The pressure is 0.1-0.15Mpa.

[0083] Adopt the device described in embodiment 1 to carry out the measurement that above-mentioned reaction is carried out calorimetry, test procedure is identical, derives experimental data through IQ, analysis experimental result is as follows Figure 4 According to the data analysis, 1,1,2-trifluoro-1,2,2-trichloroethane reacts with hydrogen to generate chlorotrifluoroethylene...

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Abstract

The invention relates to testing of substance reaction heat, in particular to a calorimetric testing method and device of a continuous flow gas-phase reaction technology. By adopting a continuous flowgas-phase calorimetric method, calorimetric testing is conducted on an adiabatic calorimetry testing device according to an adiabatic mode and a gradient scanning mode, precise control can be conducted on the reaction process, and meanwhile, data can be collected and analyzed in real time. The device comprises a reactor system, a central control system, a temperature control unit and a reaction testing pool unit. The problem can be well solved through testing, and the device can be used for calorimetric testing of gas-phase continuous flow reaction technology.

Description

technical field [0001] The invention relates to the measurement of heat of reaction of substances, in particular to a calorimetric test method and device for a continuous flow gas phase reaction process. Background technique [0002] To evaluate the thermal risk of a specific process, it is necessary to obtain parameters such as heat release rate, heat release, adiabatic temperature rise, and pressure rise. The methods for obtaining these parameters must pass calorimetric tests, adopt different calorimetric equipment, and use constant temperature heat flow, Power compensation and energy balance are used to realize calorimetric testing. Calorimetric testing equipment mainly includes reaction calorimeter (RC1 / Simular), accelerating calorimeter (ARC), differential scanning calorimeter (DSC) and so on. [0003] Among the existing calorimeters, RC1 / Simular can realize gas-liquid, liquid-liquid and liquid-solid homogeneous or heterogeneous reactions under normal pressure / high pre...

Claims

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Application Information

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IPC IPC(8): G01N25/20
CPCG01N25/20
Inventor 程春生李全国马晓华魏振云李子亮刘玄孔蓉赵闯
Owner SHENYANG RES INST OF CHEM IND
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