CN201124092Y - A supercritical state continuous chemical reaction device - Google Patents

Abstract

The utility model relates to a supercritical state continuous chemical reaction device, which is characterized in that it comprises at least one reaction gas channel, at least one supercritical solvent channel, at least one liquid reactant channel and a set of reaction device, the gas channel includes a through tube The gas bottle, gas compressor, pressure stabilizing valve, and mass flow meter connected in sequence by the pipeline; the supercritical solvent channel includes the solvent bottle connected in sequence through the pipeline and the high-pressure pump with controllable pressure and flow; the liquid reactant channel includes the liquid reactant The container and the high-pressure liquid pump; the outlets of the reaction gas passage, the supercritical solvent passage and the liquid reactant passage are respectively connected to the high-pressure mixer of the reaction device, and are connected to the phase state observation pool, the reactor, and the other behind the high-pressure mixer through pipelines in sequence. A phase state observation cell, a back pressure valve, a product expansion separation device and a gas flow meter, and a constant temperature box with a window are arranged outside the reactor and the two phase state observation cells. The utility model can simultaneously observe and study the chemical reaction property and the phase behavior of the reaction system in the supercritical state reaction process.

Description

A supercritical state continuous chemical reaction device

technical field

The utility model relates to a chemical reaction experiment device, in particular to a supercritical state continuous chemical reaction device.

Background technique

The application of supercritical fluids in chemical reactions is one of the important directions in the field of supercritical fluids. The chemical reaction in the supercritical state has many advantages, which has attracted widespread attention at home and abroad. However, because there are still many important scientific and technical problems to be further studied and solved, the application of supercritical fluid technology in chemical reactions is far from being developed. Combining the study of complex supercritical chemical reactions with the phase state of the reaction system is an important way to further study the nature and laws of the particularity of supercritical chemical reactions and to promote the application of supercritical fluid technology in chemical reaction engineering. way.

There are many kinds of chemical reaction devices currently used. For supercritical state chemical reactions, due to the high pressure involved, autoclave batch reaction devices and tubular continuous reaction devices are mainly used. These two types of reaction devices have their own advantages and disadvantages. For example, the batch reaction device is simple, but it cannot be operated continuously; while the continuous reaction device has a complex structure, but for most supercritical reactions, the continuous reaction device is closer to the actual industrial process, and can more effectively study the effects of different factors on Influence of chemical reaction properties and catalyst properties.

With the in-depth research on the properties of supercritical fluids and chemical reactions in supercritical states, people have gradually realized that the phase state has a great influence on the conversion rate, selectivity, catalyst life and other properties of chemical reactions in supercritical fluids. The combination of property research and phase state research has become a hot spot and difficulty in supercritical state reactions. However, neither the existing technology reaction devices nor commercial reaction devices can observe the phase state of the reaction system. The research in this area is carried out using Phase state and chemical reaction are studied separately, but this method has complicated steps and cannot monitor the phase state of the reaction system on-line. In addition, the devices in the prior art are generally suitable for relatively simple reaction systems, but in practical applications often involve For complex reaction systems, with the gradual industrialization of supercritical chemical reaction technology, the research on complex systems is becoming more and more important. Therefore, it is necessary to invent and improve the test equipment used in supercritical chemical reactions.

Contents of the invention

In view of the above problems, the purpose of this utility model is to provide a supercritical state continuous chemical reaction device that can be used to study the chemical reaction properties and phase behavior of supercritical fluid complex reaction systems.

To achieve the above object, the utility model adopts the following technical solutions: a supercritical state continuous chemical reaction device, characterized in that: it includes at least one reaction gas channel, at least one supercritical solvent channel, at least one liquid reactant channel and a A set of reaction devices, the gas channel includes a gas bottle, a gas compressor, a pressure stabilizing valve, and a mass flow meter connected in sequence through a pipeline; the supercritical solvent channel includes a solvent bottle connected in sequence through a pipeline and a controllable pressure and The high-pressure pump of flow rate; Described liquid reactant passage comprises liquid reactant container and high-pressure liquid pump; The outlet of described reaction gas passage, supercritical solvent passage and liquid reactant passage connects the high-pressure mixer of described reaction device respectively, by The pipeline is sequentially connected to the phase state observation tank behind the high-pressure mixer, the reactor, another phase state observation tank, back pressure valve, product expansion separation device and gas flow meter, the reactor and two phase state observation tanks The outside of the pool is provided with a constant temperature box with a window.

The number of the reaction gas channels is two or more.

The number of the liquid reactant channel is more than one.

The number of the supercritical solvent channel is more than one.

Because the utility model adopts the above technical scheme, it has the following advantages: 1. The utility model is respectively provided with a phase state observation pool at the inlet and outlet of the reactor, so the chemical reaction properties of the supercritical state can be measured simultaneously under high temperature and high pressure. The observation and study of the phase behavior of the reaction system. 2. The utility model can input one or more gas reactants and one or more liquid reactants contained in the supercritical fluid by connecting each input port of the high-pressure mixer, which can be suitable for Simple reaction system, but also suitable for complex reaction system. 3. The utility model adopts the coupling structure of high pressure pump, compressor, back pressure valve and pressure stabilizing valve, which can stabilize the flow rate, pressure and temperature of the complex reaction system under high temperature and high pressure, and can run continuously for a long time. 4. The reactor of the present invention can be designed and processed into various sizes, and its volume can be 1, 5, 10, 20, 30, 40, 50 milliliters, etc., so as to adapt to tests with different reaction systems and conditions.

Description of drawings

Fig. 1 is a schematic diagram of the flow path of the utility model

Detailed ways

Below in conjunction with embodiment and accompanying drawing, the utility model is described in detail.

As shown in Figure 1, the utility model includes reaction gas channel, supercritical solvent channel, liquid reactant channel and reaction device. The reaction gas channel includes a gas bottle 11, a gas compressor 12, a pressure stabilizing valve 13, and a mass flow meter 14 connected in sequence through pipelines, and the outlet of the reaction gas channel is connected to a high-pressure mixer 41 in the reaction device. The supercritical solvent channel includes a solvent bottle 21 and a high-pressure pump 22 with controllable pressure and flow rate connected in sequence through pipelines, and the outlet of the supercritical solvent channel is connected to a high-pressure mixer 41 . The liquid reactant channel includes a liquid reactant container 31 and a high-pressure liquid pump 32 , and the outlet of the liquid reactant channel is connected to a high-pressure mixer 41 . The high-pressure mixer 41 is provided with a constant temperature and stirring device, and the reaction device also includes a phase state observation tank 42, a reactor 43, another phase state observation tank 44, and a back pressure valve 45 connected in sequence behind the high-pressure mixer 41 through pipelines. , product expansion separation device 46 and gas flow meter 47, gas flows out from the gas flow agent 47, and liquid flows out from the valve 48 at the bottom of the product expansion separation device 46. A constant temperature box 49 with a window is arranged outside the reactor 43 and the two phase observation pools 42 and 44 of the reaction device.

In the above-mentioned embodiment, only one reaction gas channel can be provided, that is, a reaction gas and a liquid can be mixed and reacted; two reaction gas channels can also be provided (this method is adopted in this embodiment), so that two reaction gases and one liquid can be mixed and reacted. The purpose of mixed reaction of two kinds of liquids; more than two reaction gas input channels can also be set to realize the purpose of mixed reaction of multiple reaction gases and one liquid. In the same way, the purpose of mixing more than one liquid with one or more reaction gases can also be achieved by setting multiple liquid reactant channels. It is also possible to add more than one supercritical solvent by setting more than one supercritical solvent channel.

In the above embodiments, precision pressure gauges P, safety valves 5 and temperature controllers T are also installed at different positions of the pipelines as required. Only one safety valve 5 can be set, and its setting position can be changed; the precision pressure gauge P respectively tests the pressure at the following positions; 21 and the high-pressure pump 22, between the high-pressure pump 22 and the high-pressure mixer 41, and between the phase observation pool 44 and the back pressure valve 45. Two temperature controllers T are arranged on the constant temperature stirring high-pressure mixer 41 and the thermostat box 49 with a window.

In the above-mentioned embodiment, the gas compressor 12 compresses the reaction gas to achieve the effect of pressurization; the pressure stabilizing valve 13 can adjust the pressure to make the reaction air pressure stable; the mass flow meter 14 can adjust the input reaction gas; the high-pressure mixer 41 is a belt There is a high-pressure mixer with constant temperature function and stirring function; the solvent in solvent bottle 31 can be liquid or gas, and the high-pressure pump 22 effect is to extract the solvent in solvent bottle 21; It has the function of heat preservation and has a window for easy observation; the function of the back pressure valve 45 is to reduce the pressure of the reacted mixture; the product expansion separation device 46 divides the depressurized reactant into gas and liquid, wherein the liquid flows out from the lower side, and the gas passes through the upper side. The gas flow meter 47 on the side is discharged, and the amount of discharged gas can be measured.

During the experiment, different reactants enter the reactant mixer 41 through different passages, and after being stirred and mixed by the reactant mixer 41, the operator can observe from the two phase state observation pools 42 and 44 through the window on the thermostat 49 The phase state of the mixed reaction before and after the mixture enters the reactor 43 is observed at any time whether there is phase separation under different reaction conditions and conversion rates, and then the product composition is analyzed by means of gas chromatography and mass spectrometry. During the reaction process, the flow rate and feed ratio of each reactant are controlled by the pressure and flow rate of the air compressor 12, high-pressure pump 22 and mass flow meter 14 in each channel. The product passing through the reactor 43 enters the product expansion separation device 46 for decompression separation through the back pressure valve 45 , the liquid product is discharged from the valve 48 at the bottom of the product expansion separation device 46 , and the gas product is discharged through the gas flow meter 47 .

Claims (6)

1. A supercritical state continuous chemical reaction device is characterized in that: it comprises at least one reaction gas channel, at least one supercritical solvent channel, at least one liquid reactant channel and a set of reaction device, and the gas channel includes a tube A gas bottle, a gas compressor, a pressure stabilizing valve, and a mass flow meter connected in sequence; the supercritical solvent channel includes a solvent bottle connected in sequence through a pipeline and a high-pressure pump with controllable pressure and flow rate; the liquid reactant channel Including a liquid reactant container and a high-pressure liquid pump; the outlets of the reaction gas channel, the supercritical solvent channel and the liquid reactant channel are respectively connected to the high-pressure mixer of the reaction device, and are sequentially connected behind the high-pressure mixer through pipelines A phase state observation cell, a reactor, another phase state observation cell, a back pressure valve, a product expansion separation device and a gas flow meter, the reactor and the two phase state observation cells are equipped with a constant temperature box with a window outside. 2. A supercritical state continuous chemical reaction device according to claim 1, characterized in that: the number of said reaction gas channels is two. 3. A supercritical state continuous chemical reaction device according to claim 1, characterized in that: the number of said reaction gas channels is more than two. 4. A supercritical state continuous chemical reaction device according to claim 1, 2 or 3, characterized in that the number of said liquid reactant channels is more than one. 5. A supercritical state continuous chemical reaction device according to claim 1, 2 or 3, characterized in that: the number of said supercritical solvent channels is more than one. 6. A supercritical state continuous chemical reaction device as claimed in claim 4, characterized in that: the number of said supercritical solvent channels is more than one.